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*1): PRESSURE MAX LIMIT ERROR also appears when the

pressure exceeds the internal pressure limit.
The limit is changed automatically related to the flow rate.
The internal pressure limit is 60 MPa for 0.000 to 2.500
mL/min, and 30 MPa for 2.501 to 5.000 mL/min.

4.3.2 Troubleshooting

Table 4-3 offers a guideline for the troubleshooting of the pump.
Refer to this table first, if a problem occurs.

Table 4-3 The Chromaster 5160 Pump Troubleshooting

No. Symptom

Cause

Measure

1

Even if the PROG key is
pressed, setting of input mode is
failed.

The program mode is not displayed. Set the program mode by

pressing the INITIAL key.

2

The pump does not start when
pressing the PUMP ON/OFF
key.

Flow rate is set at 0.

Set the flow rate by pressing the

MANUAL key of the MANUAL

function.

3

Gradient delivery does not start
when pressing the START key.

1) The monitor screen is not

displayed.

2) The program mode is not

displayed.

1) Display the monitor screen

by pressing the ESC key.

2) Set the program mode by

pressing the INITIAL key.

4

Purging can’t be set or cancelled
by pressing the PURGE key.

1) monitor screen is not

displayed.

2) Waiting for numerical input.

Display the monitor screen by
pressing the ESC key.

5

A monitor lamp for the
degassing unit doesn’t light up.

1) The power supply of the pump

or the system unit is turned off.

2) The power supply cable is

unconnected.

1) Turn on the power supply

for the pump or the system
unit.

2) Connect the power supply

cable.

6

Air bubbles are coming out from
the exit of the degassing unit.

1) Rapid

suction

2)  Looseness of the piping joint.
3)  Clogging of the solvent filter
4)  Negative pressure depending on

the position of the solvent bottle.

5) Incomplete replacement of

solvent

1) Set suction velocity as:

5 mL/min and below for
replacement of the solvent.
3 mL/min and below for an
analysis.

2)  Tighten the joint manually.
3)  Wash the solvent filter.
4)  Place the solvent bottle in

the same height as the
instrument.

5) Replace the solvent

completely.

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Summary of Contents for CHROMASTER 5160

Page 1: ...ions and precautions carefully Be sure to observe the safety instructions in this manual and the WARNING CAUTION labels on the instrument Keep this manual in a safe place nearby so it can be referred to whenever needed 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 3rd Edition August 2014 Copyright C Hitachi High Tech Science Corporation 2013 1st Edition 2012 All rights reserved Printed in Ja...

Page 2: ... party in any form or by any means without the express written permission of Hitachi High Tech Science Corporation 3 Hitachi High Tech Science Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 3: ...ety Note that it is allowed only for persons having a basic knowledge of chemical analysis procedures to use this instrument Carefully read this instruction manual before attempting operation For proper use of the software please acquaint yourself with it The liquid chromatograph system comprises a pump unit for delivering mobile phases a sample introduction unit for injecting samples autosampler ...

Page 4: ...adient System Section 2 FUNCTIONS Name and Function of Each Part on Pump Specifications Section 3 OPERATION Basic Operation UTLTY Setting GLP and Preparation Section 4 MAINTENANCE INSPECTION Performance and Specifications Check Section 5 PARTS REPLACEMENT Consumables and Spare Parts Section 6 INDEX APPENDIX1INSTRATTION APPENDIX2Description on Contact Signal Communication APPENDIX3Terminology First...

Page 5: ... Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be available in original ve...

Page 6: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 7: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Tech Science does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Tech Science or its related companies or application of said instrument Installation Re...

Page 8: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 9: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 10: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 11: ...affected by electromagnetic noise within the permissible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power devi...

Page 12: ...d NOTICE or NOTE is used to indicate precautionary instructions concerning possible property damage NOTICE Used to indicate a potentially hazardous situation which if not avoided will or can result in damage to user s property serious damage to the instrument damage to data or environmental pollution though personal injury may not be incurred NOTE Used to indicate explanatory information for ensur...

Page 13: ...tric shock or fire Radiation from the Laser Light Source WARNING The internal CD ROM or CD R W drive of the PC is provided with a laser beam source In normal operation of the PC containing the laser beam source no laser beam harmful to human health will be emitted outside Note however that if a laser beam leaking out of the PC accidentally gets into the eye eye injury could occur When using the PC...

Page 14: ...r waste solution Leakage of solvent inside the instrument Section 3 4 3 6 When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution employ and provide proper grounding connection to it Section 3 4 3 6 Explosion of Vapor from Flammable Chemicals If a flammable chemical such ...

Page 15: ...n an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet b If a grounded 3P power outlet is not available use a grounded 3P table tap or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 mm APPEN...

Page 16: ...ent from tipping over accidentally APPENDIX 1 Fatigue due to Long Hour Operation If you keep working with the display monitor and keyboard for long hours your eyes and body will be fatigued to jeopardize your health When working with the display monitor for a long time take a break for 10 to 15 minutes per hour for health of your eyes and body Chapter 3 Injury of Hand by Seal remover PV When remov...

Page 17: ...ck the appearances of these warning labels to see if they are clean to allow easy reading over a safe distance If any one of the warning labels becomes illegible due to deterioration contact your local Hitachi High Technologies Corporation sales representative or service office of Hitachi High Technologies Corporation sales representative for replacement with a new one 1 Ignition of Flammable Chem...

Page 18: ...ll Furthermore leakage of a highly volatile solvent may not be detected Be sure to check for liquid leakage regularly to prevent a possible serious accident regardless of whether the leak sensor is activated or not a In routine inspection of the instrument visually check for liquid leakage before attempting measurements b In periodic inspection of the instrument check that the leak sensor works no...

Page 19: ...TY SUMMARY NOTICE Precaution Continued Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally If necessary conduct measurement on a control sample ...

Page 20: ...UMMARY SAFETY 1 General Safety Precautions SAFETY 2 WARNING Precautions in the Manual SAFETY 3 CAUTION Precautions in the Manual SAFETY 5 WARNING and CAUTION Labels on Instrument SAFETY 6 NOTICE Precautions SAFETY 7 1 OUTLINE 1 1 1 1 Isocratic System 1 1 1 2 Low pressure Gradient System 1 2 2 FUNCTIONS 2 1 2 1 Name and Function of Each Part on Pump 2 1 2 2 Name and Function of Each Part on UI Pad ...

Page 21: ...itor 3 46 3 3 7 Key Lock 3 47 3 4 Analysis Operation 3 48 3 4 1 Operation Procedure 3 50 3 4 2 Analyzing Operation 3 50 3 5 Setup 3 61 3 5 1 Pump Mode Setting 3 61 3 5 2 LCD Contrast Setting 3 63 3 6 Before Performing Analysis 3 64 3 6 1 Selection of Mobile Phase and Cautions on Handling 3 66 3 6 2 Characteristics of Organic Solvents 3 69 3 6 3 Cautions on Static Electricity 3 74 3 7 Preparation 3...

Page 22: ... 5 17 5 9 Parts Replacement for the Plunger Wash Mechanism 5 20 5 10 Parts Replacement for the Auto Purge Valve 5 24 INDEX INDEX 1 APPENDIX APPENDIX 1 1 APPENDIX 1 INSTALLATION APPENDIX 1 1 1 Unpacking APPENDIX 1 1 2 Place for Installation APPENDIX 1 2 3 Items to be Prepared by Customer APPENDIX 1 3 3 1 Power Supply Arrangement APPENDIX 1 3 3 2 Installation Space APPENDIX 1 7 4 Check against Packi...

Page 23: ... sample In addition a degassing unit for deaerating a mobile phase a gradient device for varying a mixing ratio of mobile phases with time and other optional devices are incorporated in the system 1 1 Isocratic System The isocratic system has a simple configuration in which single solvent analysis is performed Fig 1 1 Isocratic System Chromaster 5110 5160 pump Chromaster 5310 column oven Chromaste...

Page 24: ...nt System In the low pressure gradient system two or more solvents are mixed in its low pressure section from which a liquid feed is performed by a single pump The composition of a mobile phase is made to vary with time in chromatographic separation Fig 1 2 Low Gradient System Mobile phase Chromaster organizer Chromaster 5410 5420 5430 detector Chromaster 5310 column oven Wash pump Injection valve...

Page 25: ...are mixed at a pre specified ratio 3 Through the mixer the mixture mobile phase is delivered 4 A sample is injected by the autosampler 5 The injected sample is separated through the column which is maintained at a constant temperature by the column oven 6 Each component separated from the sample is detected as a signal by the detector ...

Page 26: ...p Fig 2 1 Front Panel Fig 2 2 Front View LED Left door Right door Power switch UI pad option Pump head 2 Purge valve Flow path filter Pressure sensor Pump head 1 Plunger wash mechanism Check valve Intake side Check valve Discharge side Leak sensor Drain tray ...

Page 27: ... Purge Valve Auto purge valve Flow path filter Pressure sensor Pump head 1 Pump head 2 Plunger wash mechanism Check valve Intake side Check valve Discharge side Leak sensor Drain tray Port 1 Flow path for the system Port Flow path for waste fluid ...

Page 28: ...n PUMP1 and PUMP2 is used Name color LED status 1 blue orange Blue Pump1 is running Orange Pump1 error 2 blue orange Blue Pump2 is running Orange Pump2 error FLOW blue Blue When the pump is ON it lights up PROG RUN blue Blue Under the time program running 2 When PUMP3 is used Name color LED status 1 blue orange Blue Pump3 is running Orange Pump3 error 2 blue orange Blue Pump3 is running Orange Pum...

Page 29: ...und terminals Three terminals for grounding the instrument e Line connector A connector for e Line connection between instrument units in the Chromaster series ポンプは外部 EVENT LIMIT OUT PUMP ON IN PUMP OFF IN PRESS OUT 1 2 3 4 Pressure value is output to the exterior Approx 70 MPa 1 V Ground terminals Wiring covers An external signal stops the pump An external signal starts the pump ...

Page 30: ...rogram EVENT No and Event code EVENT No Signal Pulse OFF ON 1 10 11 12 2 20 21 22 3 30 31 32 4 40 41 42 Specifying 00 as an EVENT code stops a pump and EVENT code 92 rings buzzer 1 Becomes OFF when the pulse is output in the ON status 2 OFF has priority over ON 3 Contact output specification of each terminal Voltage 30 V DC max Current 100 mA max PRESS OUT Pressure value is output to the exterior ...

Page 31: ...is section describes how to use the UI pad for operations The UI pad is provided with common control keys available for different modules and unique control keys for particular modules The functions of the common control keys are described below Fig 2 5 Control Panel of UI pad for Pump NOTE If a mistake has been made during operation click the ESC key In most cases the initial status will return u...

Page 32: ...Low pressure gradient 2 Sets LCD contrast of UI Pad option Press this key together with the Power key to display the Setup screen Keep the keys pressed down until the Setup screen appears 4 Displays and sets the contents of the auxiliary function UTILITY 1 Correction of zero pressure 2 Setting the motor control method 3 Setting purge flow rate time 4 Setting low pressure gradient mode LFM HFM 5 Sp...

Page 33: ...ing are held until the parameter setting is finished 13 LOCK OFF 1 Returns the screen to Monitor from Numerical value input mode for inputting each mode 2 Releases key lock 14 15 16 17 A B C D Press the A key in Manual status to obtain A 100 in one touch B C or D has a similar function This key can be used depending on the gradient conditions Low pressure gradient A B C D key 18 Inputs a decimal p...

Page 34: ...gisters inputted numerical values It is quite necessary to press ENT key at the end of inputting a numerical value 23 P WASH Starts Stops the plunger wash pump The plunger wash pump delivers wash fluid to the plunger wash mechanism automatically according to the setting time Press the key once again during washing to suspend plunger wash The key is enabled only when the optional wash pump is mount...

Page 35: ...sure limit range 0 60 0 MPa f Delivery volume of No 1 plunger stroke 100 µL stroke g Flow rate accuracy constant room temperature 20 C distilled water delivering pressure 30 MPa 2 L min 0 01 0 1 mL min 1 0 101 2 5 mL min h Flow rate precision 0 075 RSD or 0 02 min SD whichever is greater Retention time flow rate 1 mL min constant room temperature 20 C distilled water i Solvent compression rate cal...

Page 36: ... Ceramics PTFE Carbon containing PTFE VespelⓇ Pump with auto purge valve q Communication e Line OUTPUT BUSY INPUT 1 GRADIENT START IN 2 ERROR IN r GLP corresponding function Total flow rate display Double speed error Changeover number of times of the proportioning valve Running time of the dynamic mixer Changeover number of times of the auto purge valve Operating time of the plunger wash pump s Di...

Page 37: ...n condensing x Humidity 25 to 85 RH y Option Chromaster GUI controller UI pad Low gradient unit Dynamic mixer Semi micro mixer Auto purge valve when a pump with auto purge valve is selected Plunger wash pump 6 channel degassing unit ...

Page 38: ... the display monitor for a long time take a break for 10 to 15 minutes per hour for health of your eyes and body 3 1 Basic Operation 3 1 1 Power Supply The power activation operation of pump is described here Fig 3 1 Front Panel NOTE If the monitor display screen does not appear on the LCD within 3 minutes after turning on the power or if an error message appears on the LCD refer to 4 3 1 Error Me...

Page 39: ...ing is completed normally Press key to indicate from the second to the fifth monitor screen Press ESC key to return to the first monitor screen b 1 st Monitor Screen Table 3 1 1 st Monitor Screen Indication Description TIME Program precessing time A A fluid mixture ratio B B fluid mixture ratio C C fluid mixture ratio D D fluid mixture ratio FLOW Pump flow rate PRESS Pump pressure C or O Auto purg...

Page 40: ...urge is in execution LK Keyboard on operating panel is locked FL Column flush is in execution LC Conditioning of a link program is in execution Table 3 2 Status Indication State Input Key Pump ON OFF GRADIENT START GR STOP IN MANUAL SET MN MN PURGE PG KEY LOCK LK LK COLUMN FLUSH FL LINK CONDITIONING LC The key is disabled when status indication is LC or FL c 2 nd Monitor Screen P UNIT P MAX P MIN ...

Page 41: ...atically D MIX Dynamic mixer USE No USE P WASH Wash pump ON Running OFF Suspended NOTE For Chromaster 5160 Pump an internal maximum operating pressure will be set up according to the flow rate setting Pressure limit range 0 to 2 500 mL min 60 0 MPa 2 501 to 5 000 mL min 30 0 MPa d 3 rd Monitor Screen Table 3 4 3 rd Monitor Screen Indication Description LOW GR Low pressure gradient unit connection ...

Page 42: ...e PUMP Low pressure gradient setup state LFM Low Frequency Mode HFM High Frequency Mode FLUSH Column flush setup ON OFF f 5 th Monitor Screen When the link program function is in the OFF state the screen won t be displayed Table 3 6 5 th Monitor Screen Indication Description LINK PROG ON when the link program function is used STEP Step No in execution CYCLE Execution cycle number of times EVENT 1 ...

Page 43: ...OW PRESS 0 0 100 0 0 0 0 000 0 0 C 1 1 st Monitor Screen P UNIT P MAX P MIN D MIX P WASH MPa 20 0 0 0 USE ON 1 2 nd Monitor Screen OPTION LOW GR P WASH A VALVE D MIX YES YES YES YES 1 3 nd Monitor Screen EVENT 1 2 3 4 PUMP FLUSH OFF OFF OFF OFF LFM ON 1 4 th Monitor Screen LINK PROG STEP CYCLE ON 1 1 99 1 5 th Monitor Screen or ESC ...

Page 44: ...eric c Numerical selection d Program setup screen SET PROGRAM NO 1 9 1 Parameter name Input range Input field PUMP SEAL CHANGE MM DD YYYY 2000 2100 9 1 2010 Parameter name Input range Input Item Input field TIME B C D FLOW EVENT 0 0 0 0 0 1 000 1 Input Item Input field PUMP 1 1 2 2 3 3 1 Parameter name Selection item Input field ...

Page 45: ...ply default numbers are indicated in the selection item When the CL key is pressed in the input field indication in the field is deleted and the cursor returns to the first character in the input field When the DEL key is pressed in the input field items are deleted while editing the program When the ESC key is pressed during the plural parameter setup operation it is reflected to the items that t...

Page 46: ...a spectrum output is started during an acquisition of chromato data it will be output to an integrator The UI pad operation will be disabled when a Chromaster GUI controller and CDS are connected 3 1 3 Operational State The pump operational state is indicated below Press the key to operate Fig 3 2 Pump State INITIAL Waiting for start in the programming mode MANUAL Running state under the constant ...

Page 47: ...re When carrying out purge operation make sure a purge valve is in the open state When the purge valve is closed a pressure limiter stops the pump An auto purge valve opens closes a valve automatically in conjunction with the PURGE key operation 1 Press the key to start the pump 2 Press the key to start purging 3 Re press the key to stop purging The auto purge valve closes a valve automatically in...

Page 48: ...nual operation settings will be deleted when the power supply is turned off Conditions must be set up each time when turning on the power supply NOTE The pump noise will be changed with the operating condition such as the flow rate and the pressure Monitor screen MANUAL 0 MANUAL FLOW 1 PRESS 2 1 CONSTANT FLOW FLOW MAX MIN 1 000 20 0 0 0 Select Isocratic mode FLOW 1 ENT CONSTANT FLOW FLOW PRESS MN ...

Page 49: ...pump noise will be changed with the operating condition such as the flow rate and the pressure NOTE When liquid delivering is started during column packing in constant pressure mode the liquid delivering flow rate or the pressure may increase rapidly When packing a column start liquid delivering in isocratic mode confirm that it increased to the target pressure and then switch to constant pressure...

Page 50: ...sure limit at 0 MPa and flow rate is1 0 ml min at 0 minute of analysis time Output pulse signals by Event 1 to 4 Change the flow rate to 0 5 ml min by 10 minutes of analysis time The parameters in the table below are an example of input PROGRAM N0 1 PRESSURE VALUE MAX MIN MPa 20 0 0 0 TIME FLOW EVENT min ml min 1 2 3 4 0 0 1 000 12 22 32 42 10 0 0 500 ...

Page 51: ... PROG TIME FLOW EVENT 0 0 1 000 12 22 32 42 1 TIME FLOW EVENT 10 0 0 500 1 Input TIME FLOW rate and EVENT Up to 4 entries can be made per step for event Refer to 3 2 8 for details of EVENT ENT TIME FLOW EVENT 1 A new input screen will be appeared Input TIME FLOW rate and EVENT ENT Enter MAX and MIN pressure limit ENT A new input screen will be appeared Press the ESC key to close the input screen a...

Page 52: ...ter Operation When buffer solution example salt solution is used it causes a wear of a plunger The whole flow path system must wash with distilled water after the analysis Distilled water must be used in a plunger wash system to prevent from a salt induced precipitation for a plunger and plunger seal when using the mobile phase which is salt induced precipitation type Additionally pour distilled w...

Page 53: ...h fluid distilled water by a syringe of an accessory 3 Connect the syringe to a joint of an inlet tube and the wash fluid distilled water is injected 4 Wash fluid is injected until a flow path of the wash system is filled with it 5 Detach the syringe from the joint of the inlet tube and stop up quickly 6 The waste solution bottle is emptied and rearranged Waste solution bottle beaker Syringe Inlet...

Page 54: ...3 17 Fig 3 3b Connecting with the Chromaster 5260 Autosampler Injection valve Syringe valve Port4 ...

Page 55: ...in valve Refer to the following operation for calibration Monitor screen PRESS is displayed as 0 and the zero pressure calibration is completed UTLITY CONDITION 1 UNIT 2 FLUSH 3 1 EVENT 4 LINK 5 P WASH 6 OTHERS 7 CONDITION SET Z ADJ 1 MOTOR CTRL 2 1 PURGE 3 CALIBRATION 4 LPGR 5 Select CONDITION 1 ENT PRESSURE ZERO ADJUT YES 1 NO 0 1 NOTE OPEN DRAIN VLAVE Select Z ADJ ZERO ADJUST 1 ENT Select YES 1...

Page 56: ...DITION 1 UNIT 2 FLUSH 3 1 EVENT 4 LINK 5 P WASH 6 OTHERS 7 CONDITION SET Z ADJ 1 MOTOR CTRL 2 2 PURGE 3 CALIBRATION 4 LPGR 5 Select CONDITION 1 ENT MOTOR CONTROL STANDARD 1 FIX 2 1 Select MOTOR CTRL 2 ENT SET UP UTLTY Select STANDARD 1 ENT Select FIX 2 ENT The motor control method is set as STANDARD FIX STEP AREA 0 30 300 100 Enter FIX STEP AREA Input range is from 0 or 30 to 300 ENT Monitor scree...

Page 57: ...RATION 4 LPGR 5 Select CONDITION 1 ENT PURGE SET MANUAL 1 A PURGE 2 0 Select PURGE 3 ENT Monitor screen SET UP UTLTY Monitor screen Select MANUAL 0 ENT Select A PURGE When auto purge is connected only 1 ENT A PURGE FLOW 0 001 9 999 5 000 Enter purging flow rate ENT Monitor screen PURGE FLOW 0 001 9 999 5 000 Enter purging flow rate ENT A PURGE TIME 1 30 min 5 Enter purging time ENT ...

Page 58: ...t 0 MPa 3 2 4 Flow Rate Calibration Setting Set up a calibration coefficient for the flow rate UTLITY CONDITION 1 UNIT 2 FLUSH 3 1 EVENT 4 LINK 5 P WASH 6 OTHERS 7 CONDITION SET Z ADJ 1 MOTOR CTRL 2 4 PURGE 3 CALIBRATION 4 LPGR 5 Select CONDITION 1 ENT CALIBRATION FLOW 1 PRESS 2 1 Select CALIBRATION 4 ENT SET UP UTLTY Monitor screen Select FLOW 1 ENT FLOW CALIB 0 970 1 030 1 000 Monitor screen Ent...

Page 59: ...2 FLUSH 3 1 EVENT 4 LINK 5 P WASH 6 OTHERS 7 CONDITION SET Z ADJ 1 MOTOR CTRL 2 4 PURGE 3 CALIBRATION 4 LPGR 5 Select CONDITION 1 ENT CALIBRATION FLOW 1 PRESS 2 2 Select CALIBRATION 4 ENT SET UP UTLTY Monitor screen Select PRESS 2 ENT PRESSURE CALIB 0 900 1 100 1 000 Monitor screen Enter calibration coefficient ENT ...

Page 60: ...r supply is turned on Table 3 7 Pressure unit Pressure Unit MPa bar psi Kgf cm 2 Corresponding value 1 00 10 0 145 10 2 UI pad display 1 0 10 145 10 Select a unit ENT UTLITY CONDITION 1 UNIT 2 FLUSH 3 2 EVENT 4 LINK 5 P WASH 6 OTHERS 7 PRESSURE UNIT MPa 1 bar 2 psi 3 1 kgf cm 2 4 Select UNIT 2 ENT SET UP UTLTY Monitor screen Monitor screen ...

Page 61: ...nction or the column flushing function were set up after 15 minutes of the analysis and the column flushing time is set up as 30 minutes to be continued UTLITY CONDITION 1 UNIT 2 FLUSH 3 3 EVENT 4 LINK 5 P WASH 6 OTHERS 7 AUTO PUMP OFF YES 1 NO 0 1 Select FLUSH 3 ENT SET DELAY TIME 1 0 600 0 min 15 0 Select YES 1 ENT SET UP UTLTY Monitor screen Enter DELAY TIME for execution of the pump auto stop ...

Page 62: ...ogram when the column flush is set up However the link program uses program No 9 The pump will be automatically stopped after the completion of program No 9 Select PARAM 1 ENT Monitor screen COLUMN FLUSH FLOW 1 000 Enter column flash time from 1 0 to 600 min 3 0 ENT Select PROGRAM No 9 2 ENT Monitor screen FLUSHING TIME 1 0 600 0 min 30 0 Enter column flash condition ENT ...

Page 63: ...ump stop Stabilization time Analysis 1 COLUMN FLUSH Delay time Analysis n Analysis 3 Analysis 2 Pump stop Stabilization time Analysis 1 Delay time n is the number of analyses specified for the autosampler Stabilization time is the time from the completion of an analysis to the starting of the next analysis Analysis n Analysis 3 Analysis 2 Stabilization time Analysis 1 Pump is delivering liquid n i...

Page 64: ...e limiter error is detected UTLITY CONDITION 1 UNIT 2 FLUSH 3 1 EVENT 4 LINK 5 P WASH 6 OTHERS 7 EVENT SET PRESS LIMIT 1 EVENT CODE 2 1 Select EVENT 4 ENT SET UP UTLTY Monitor screen Select PRESS LIMIT 1 ENT Select EVENT CODE 2 ENT SET EVENT CODE 00 92 00 Select a code ENT Monitor screen PRESS LIMIT NONE 0 PULSE 1 LEVEL 2 0 NOTE EVENT NO 4 Select a code An event will be output to EVENT No 4 when a...

Page 65: ... digit Behavior class Behavior Contact point for one sec CLOSE Pump 00 Pump has stopped Buzzer 92 Buzzer sounds for 5 sec NOTE The setting for EVENT No 4 of the gradient program will be disabled when the pressure limiter error is set Contact point OPEN Signal OFF Start point Signal ON Contact point CLOSE Start point Close marker OPEN 1 s ...

Page 66: ... program by a few steps execution of the next steps will be avoided and the link program will return to the first step and will be executed again Assume that a 5 step link program is set If you set link restart after the 2nd step in this case the 3rd step will not be executed and execution will restart from the 1st step Also when plural cycles of the same step are set the link program will return ...

Page 67: ...ge from 1 to 9 CYCLE Input the number of program repetitions Input is valid within a range from 1 to 99 COND TIME Input a conditioning time for an execution step Input is valid within a range from 0 0 to 600 0 min During the conditioning time liquid is delivered under the initial condition TIME 0 0 of the execution step When the start signal is input after the conditioning time program execution s...

Page 68: ...tions a Programs PROGRAM No 1 PRESSURE VALUE MAX MIN MPa 19 6 1 0 TIME CONCENTRATION FLOW EVENT min A B C D mL min 1 2 3 4 0 0 10 90 0 0 1 000 5 0 10 90 0 0 10 0 20 80 0 0 15 0 20 80 0 0 20 0 10 90 0 0 PROGRAM No 2 PRESSURE VALUE MAX MIN MPa 19 6 1 0 TIME CONCENTRATION FLOW EVENT min A B C D mL min 1 2 3 4 0 0 30 70 0 0 1 000 5 0 40 60 0 0 10 0 40 60 0 0 15 0 30 70 0 0 ...

Page 69: ... 10 B 90 C 0 D 0 FLOW 6 00 mL min TIME 10 0 min c Link program conditions STEP PROG No CYCLE COND TIME min 1 1 1 10 0 2 2 1 10 0 i Upon start after gradient elution Screen transition in the above example is explained The encircled numerals in this execution example correspond to the step numbers of screen display ...

Page 70: ...ample Gradient When start is input in the initial status the program at execution step program No 2 in this example will start Conditioning time After completion of the final step of link program the system returns to the first step program No 1 in this example and conditioning is carried out TIME A B C D FLOW PRESS IN 0 0 10 90 0 0 1 000 5 5 C 1 TIME A B C D FLOW PRESS GR 10 0 20 80 0 0 1 000 5 5...

Page 71: ...ime column flushing in will begin When start is input during the delay time the system returns to action in Column flushing ii Without start input after gradient elution The encircled numerals in this execution example correspond to the step numbers of screen display TIME A B C D FLOW PRESS IN 0 0 10 90 0 0 1 000 5 5 C 1 TIME A B C D FLOW PRESS FL 0 0 10 90 0 0 1 000 5 5 C 1 ...

Page 72: ... program No 2 in this example Delay time Liquid is delivered in the initial status initial condition of program No 2 in this example When start is not input during the delay time column flushing in will begin Column flushing TIME A B C D FLOW PRESS IN 0 0 10 90 0 0 1 000 5 5 C 1 TIME A B C D FLOW PRESS GR 10 0 20 80 0 0 1 000 5 5 C 1 TIME A B C D FLOW PRESS LC 0 0 30 70 0 0 1 000 5 5 C 2 TIME A B ...

Page 73: ... delivered in the initial status initial condition of program No 1 in this example Gradient Gradient elution is carried out program No 1 is executed in this example In this case the step stopped halfway will be carried out TIME A B C D FLOW PRESS IN 0 0 10 90 0 0 1 000 5 5 C 1 TIME A B C D FLOW PRESS GR 10 0 20 80 0 0 1 000 5 5 C 1 TIME A B C D FLOW PRESS LC 0 0 10 90 0 0 1 000 5 5 C 2 TIME A B C ...

Page 74: ...rogram No 1 in this example and conditioning is carried out Delay time initial Liquid is delivered in the initial status initial condition of program No 1 in this example When start is not input during the delay time column flushing in will begin When start is input during the delay time the system returns to action in Column flushing TIME A B C D FLOW PRESS LC 0 0 30 70 0 0 1 000 5 5 C 2 TIME A B...

Page 75: ... detected Enter wash time ENT UTLITY CONDITION 1 UNIT 2 FLUSH 3 6 EVENT 4 LINK 5 P WASH 6 OTHERS 7 WASH TIME 0 300 sec 0 Select P WASH 6 ENT SET UP UTLTY Monitor screen Monitor screen UTLITY CONDITION 1 UNIT 2 FLUSH 3 7 EVENT 4 LINK 5 P WASH 6 OTHERS 7 OTHERS ERROR OUT 1 LEAK SENSOR 2 1 Select OTHERS 7 ENT ERROR OUT SIGNAL DISABLE 0 ENABLE 1 1 Select ERROR OUT 1 ENT Monitor screen SET UP UTLTY Mon...

Page 76: ...or is in the OFF state it returns in the ON state when power is resupplied UTLITY CONDITION 1 UNIT 2 FLUSH 3 7 EVENT 4 LINK 5 P WASH 6 OTHERS 7 OTHERS ERROR OUT 1 LEAK SENSOR 2 2 Select OTHERS 7 ENT LEAK SENSOR OFF 0 ON 1 1 Monitor screen SET UP UTLTY Monitor screen Select LEAK SENSOR 2 ENT 0 The leak sensor is disabled 1 The leak sensor is enabled ENT ...

Page 77: ...OGBOOK REPORT 1 RESET 2 1 Select PUMP SEAL 1 ENT Monitor screen GLP Monitor screen Select REPORT 1 ENT Select RESET 2 ENT PUMP SEAL CHANGE MM DD YYYY 2000 2100 9 1 2010 Reset logbook NOTE Enter the pump seal replacing date Enter Month Date Year And press ENT In other words it can t be reset without pressing the ENT key Even if the previous data is still indicated reenter a desired date and then pr...

Page 78: ...1 Select P WASH 2 ENT Monitor screen GLP Monitor screen Select REPORT 1 ENT Select RESET 2 ENT P WASH PUMP CHANGE MM DD YYYY 2000 2100 9 1 2010 Reset logbook NOTE Enter the plunger wash pump replacing date Enter Month Date Year And press ENT In other words it can t be reset without pressing the ENT key Even if the previous data is still indicated reenter a desired date and press ENT The total runn...

Page 79: ...een GLP Monitor screen Select RESET 2 ENT A V SEAL CHANGE MM DD YYYY 2000 2100 9 1 2010 Reset logbook NOTE Enter the maintenance part for the auto purge valve replacing date Enter Month Date Year And press ENT In other words it can t be reset without pressing the ENT key Even if the previous data is still indicated reenter a desired date and press ENT The total number of times of the changeover wi...

Page 80: ...r screen GLP Monitor screen Select RESET 2 ENT D MIX STIRRERCHANGE MM DD YYYY 2000 2100 9 1 2010 Reset logbook NOTE Enter the maintenance part for the dynamic mixer replacing date Enter Month Date Year And press ENT In other words it can t be reset without pressing the ENT key Even if the previous data is still indicated reenter a desired date and press ENT The total running time will be indicated...

Page 81: ... unit to be continued GLP LOGBOOK 1 PRESSURE M 2 KEY LOCK 3 1 LOGBOOK PUMP SEAL 1 P WASH 2 5 A VALVE 3 D MIX 4 P VALVE 5 Select LOGBOOK 1 ENT LOGBOOK REPORT 1 RESET 2 1 Select P VALVE 5 ENT GLP Monitor screen P VALVE A LAST CHANGED DATE 10000000 09 01 2010 The total number of times of the changeover after replacement of a maintenance part for the proportioning valve is indicated ENT or ESC 1 Displ...

Page 82: ... ENT NOTE Enter the maintenance part for the dynamic mixer replacing date Enter Month Date Year And press ENT In other words it can t be reset without pressing the ENT key Even if the previous data is still indicated reenter a desired date and press ENT The total number of times of the changeover will be indicated as zero and integration will be started ...

Page 83: ...sate for decreased pressure Air bubbles in the flow path may cause the error The pressure monitor will be reset in the following cases Input of PUMP ON or PUMP OFF Activation of contact Start of gradient elution Receiving of start signal from integrator in e line configuration External start of pump Input of PURGE ON or PURGE OFF GLP LOGBOOK 1 PRESSURE M 2 KEY LOCK 3 2 PRESSURE MONITOR 9999 TIMES ...

Page 84: ...anel NOTE The UI pad operation will be disabled when the Chromaster GUI controller and CDS are connected GLP LOGBOOK 1 PRESSURE M 2 KEY LOCK 3 3 KEY LOCK YES 1 NO 0 1 Select KEY LOCK 3 ENT Monitor screen GLP Monitor screen The operating panel is key locked to prevent incorrect input Select YES 1 or ENT Press ESC to release the key lock ...

Page 85: ...r waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemicals If a flammable chemical such as organic solvent leaks from t...

Page 86: ...injury For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper protective clothes e g safety goggles so that a solvent will not come into direct contact with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor ...

Page 87: ...led with mobile phase so that air won t enter the column NOTE The whirring sound of the pump during operation varies depending on such operating conditions as flow rate and pressure Although the whirring sound may become larger anywhere in the high pressure range it is not a symptom of abnormality 3 4 2 Analyzing Operation 1 SET PROGRAM allows the generation of a maximum of 9 programs You can exec...

Page 88: ...internal action such as a pump stop and the ringing of a buzzer Example EVENT 1 1 ENT 2 1 ENT b In case that an event setting is desired independent of FLOW only the event code showed be entered Press ENT to skip all the entries you do not want until you reach event column In the SET PROGRAM mode the interpolation of mixing ratio flow rate etc that occurs in a time program is as follows Parameter ...

Page 89: ...DIFY 0 NEW 1 1 ENT MAX Upper limit pressure level ENT MIN Lower limit pressure level ENT TIME Set time Ti ENT FLOW Set flow rate Fi ENT EVENT Event code E1i ENT Event code E2i ENT Event code E3i ENT Event code E4i ENT 8 Repeat steps to until you define all programs lines 9 To terminate the program generation press ESC 4 1 2 3 5 6 7 7 7 7 7 5 ...

Page 90: ...MPa 5 The set time can be from 0 0 to 600 0 6 Flow rate valid entries are from 0 00 to 5 000 7 Input the event code At the set time point you can stop the pump generate an audible signal markers timers etc When properly interfaced these signals can be output to an external system No display will show on the screen unless an event is set When an event is not set press only the ENT key 8 Repeat step...

Page 91: ... next PROG SET PROG No No of program to be deleted m ENT MODIFY 0 NEW 1 1 ENT ESC 1 Program number can be from 1 to 9 2 Input 1 to generate a new program The contents of the existing program will be deleted 3 Press the ESC key and Monitor screen reappears 1 2 3 ...

Page 92: ...gram input 1 3 If pump pressure rises beyond the level set here the pump automatically stops Set pressure is from 0 1 to 60 0 MPa 4 If pump pressure falls below the level set here the pump automatically stops Set pressure is from 0 0 to 60 0 MPa 5 Press the key until the step you want to delete appears on the screen If display advances beyond that step press the key 6 Press the DEL key when the cu...

Page 93: ...tep m ENT MODIFY 0 NEW 1 0 ENT MAX Upper limit pressure level ENT MIN Lower limit pressure level ENT TIME Time point of step added Ti ENT FLOW Set flow rate Fi ENT EVENT Event code E1i ENT Event code E2i ENT Event code E3i ENT Event code E4i ENT ESC 1 2 4 3 5 6 7 7 7 7 8 ...

Page 94: ...ues that can be inputted are 0 0 to 60 0 MPa 5 Input the time point of the step you want to add 6 Flow rate valid entries are from 0 00 to 5 000 7 Input the event code At the set time point you can stop the pump generate an audible signal markers times etc When properly interfaced these signals can be output to an external system No display will show on the screen unless an event is set When an ev...

Page 95: ...ontaining step to be corrected m ENT MODIFY 0 NEW 1 0 ENT MAX Upper limit pressure level ENT MIN Lower limit pressure level ENT TIME Time point of step added Ti ENT FLOW Set flow rate Fi ENT EVENT Event code E1i ENT Event code E2i ENT Event code E3i ENT Event code E4i ENT ESC 1 2 3 4 5 6 7 8 8 8 8 9 ...

Page 96: ...ops Values that can be inputted are 0 0 to 60 0 MPa 5 Press the key until the step to be corrected appears on the screen If the display advances beyond that step press the key 6 When a correction is unnecessary press the ENT key only The allowable input range is 0 to 600 0 7 When a correction is unnecessary press the ENT key Valid flow is from 0 00 to 5 000 8 Enter the event code When a correction...

Page 97: ... the level set here the pump automatically stops Values that can be inputted are 0 1 to 60 0 MPa 4 If pump pressure falls below the level set here the pump automatically stops Values that can be inputted are 0 0 to 60 0 MPa 5 Press the key until the step to be corrected appears on the screen If display advances beyond that step press the key 6 Move the cursor to the parameter to be deleted while h...

Page 98: ...NTRAST 2 D MIX 3 1 ENT PUMP 1 1 2 2 3 3 1 Select PUMP 1 ENT SET UP UTLTY POWER ON Select PUMP number 3 ENT GR MODE LOW 1 FLOW 2 2 Select FLOW isocratic mode 2 ENT LOW Low gradient mode FLOW Isocratic mode Press the POWER and SET UP UTLTY keys simultaneously The Pump mode setting screen will be displayed Continue pressing SET UP UTLTY until the setting screen appears SETUP PUMP MODE CONTRAST S NO 3...

Page 99: ...SETUP PUMP MODE CONTRAST S NO 1 FLOW 4 02AB 111 Turn off the power supply once TIME FLOW PRESS 0 0 0 00 0 0 1 A monitor screen of the isocratic mode will be indicated Turn on the power supply again Self diagnosis is performed ...

Page 100: ...2 D MIX 3 2 ENT LCD CONTRAST 1 7 4 Select CONTRAST 2 ENT SET UP UTLTY POWER ON Enter contrast intensity 4 ENT Press the POWER and SET UP UTLTY keys simultaneously LCD contrast setting screen will be displayed Continue pressing SET UP UTLTY until the setting screen appears POWER OFF POWER ON SETUP PUMP MODE CONTRAST S NO 1 FLOW 4 02AB 111 Instrument starts with the set contents ...

Page 101: ...top operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemicals If a flammable...

Page 102: ...injury For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper protective clothes e g safety goggles so that a solvent will not come into direct contact with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor ...

Page 103: ...have a specially high content of air and the baselines may be fluctuated by bubbles Malfunction of check valve and loss of column efficiency may also be caused Degassing unit is especially required for mixing solvents for gradient use Degas the solvents before use seeing 3 7 2 Degassing Mobile Phase b When performing analysis with a UV detector in the short wavelength range or highly sensitive ana...

Page 104: ...pump head to wash it out Plunger Cleaning Mechanism option is separately prepared It is recommended to use this option Refer to 3 1 9 Wash after operation for details NOTE When the suction valve and the discharge valve on the pump head side are dried mobile phase suctioning may not be performed in early stage of the pump starting In such case suck the mobile phase using an attached syringe and dis...

Page 105: ...carbonate Sodium carbonate Ammonium chloride Potassium chloride Sodium chloride Tolufluoroacetic acid Note 1 Max concentration of above reagents should be 5 to 6 Note 2 When the above reagents have been used necessarily wash all the flow paths with distilled water completely without fail Do not use reagents that corrode SUS316 though they are not shown in the table above High viscosity solvent won...

Page 106: ...an abnormality is found stop operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable...

Page 107: ... WARNING Ignition of Flammable Chemicals This instrument is not explosion proof In unattended operation do not use organic solvents having a flash point below 70 C Be aware of ignition hazard when using flammable chemicals such as organic solvents a Do not bring a heat or flame source near the instrument b Well ventilate the laboratory room where the instrument is used c Always check the following...

Page 108: ...e the laboratory room adequately WARNING Inflammation or Injury due to Toxic Corrosive or Stimulative Solvent When using a toxic corrosive or stimulative solvent be careful not to incur a physical inflammation or injury For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper prot...

Page 109: ... 1 368 1 378 1 496 1 389 1 525 1 501 1 424 1 353 1 442 1 443 1 424 1 394 1 408 1 445 1 381 1 400 1 359 1 422 1 370 1 362 1 410 1 586 1 387 1 394 1 344 1 510 1 38 1 361 1 329 1 427 1 372 1 333 210 210 210 210 210 210 210 380 265 225 220 290 220 225 285 225 280 220 290 245 245 330 220 230 330 380 220 260 260 210 275 380 210 305 220 210 210 210 210 40 21 7 46 1 20 17 8 30 12 8 9 4 o 17 2 m 25 p 25 27...

Page 110: ...f low boiling point are not only dangerous but also generate bubbles when sucked by pump so that normal pumping will be impossible 3 When performing high sensitivity analysis with UV detector use solvents which absorb especially small amount of UV light Since special grade reagents such as methanol and acetonitrile generally used absorb the shorter wavelengths a lot use reagents for liquid chromat...

Page 111: ...conductive container for waste solution and provide proper grounding connection to it Since flammable organic solvents are used for the High Speed Liquid Chromatograph be careful about heat and fire Since thin tubings are used for the liquid chromatograph static electricity is easily generated If charged liquid is collected into an insulated waste container for example and an electric discharge oc...

Page 112: ...bbles d Variation of pump pressure e Reduced precision of gradient mixing ratio 2 For degassing mobile phase two methods are available Degassing unit and Manual Degassing method is explained in 3 7 2 3 Use mobile phase without dust Dust in mobile phase causes trouble in pumping and the pressure may vary 3 7 2 Degassing Mobile Phase There are various ways of degassing Perform degassing suitable for...

Page 113: ... degassing small bubbles are generated first then gradually larger bubbles are generated Continue degassing until bubbles are not generated anymore It takes 5 to 10 minutes to finish d When bubble generation finishes turn off the power of ultrasonic cleaner e Take out mobile phase container from ultrasonic cleanser wipe the water from the container and set the container to liquid chromatograph 2 E...

Page 114: ...y be caused NOTE Degas mobile phase of aqueous solution by using both ultrasonic cleaner with water and aspirator to decrease pressure Fix the degassing time b Insert rubber tube of aspirator into mouth of reagent bottle c Turn on the power of ultrasonic cleaner d Open the faucet of city water for aspirator to decrease pressure e When degassing small bubbles are generated first then gradually larg...

Page 115: ...ause constitution ratio of mobile phase may be varied by the degassing time boiling point of mobile phase would vary with a reduced pressure 3 7 3 Removing Dust from Mobile Phase There are various ways to remove dust from mobile phase Remove dust in the way suitable for the purpose of use 1 Example of Filtering of Mobile Phase by Using Membrane Filter Removing dust and degassing can be performed s...

Page 116: ...g sample Filter the sample in the way suitable for the sample amount b Example of Removing Foreign Matter from Sample For example when analysis is performed with a reversed phase column e g ODS column foreign matter can be removed as follows Take sample into a syringe attach a normal phase cartridge and perform filtering See the figure at left NOTE There are various ways of removing foreign matter...

Page 117: ...260 or equivalent Detector Chromaster 5410 or equivalent Data processing unit Waste solution bottle NOTE If deaeration of detergent is inadequate full performance may not be provided In this case deaerate the detergent sufficiently or connect it through a degassing unit 2 Items for Performance Check Prepare the following items for performance check Load resistance coil A coiled stainless tube or t...

Page 118: ...e autosampler and pump detector is properly connected Fig 4 1 Flow Path Diagram 2 Connect the e Line cable among the autosampler detector and pump 3 Check if the drain tube is properly connected to the waste solution bottle The waste solution bottle must be at a lower position than the autosampler Detector Load resistance coil Injection valve Syringe valve Autosampler Pump Mobile phase Waste bottl...

Page 119: ...utosampler with fluid 8 After the mobile phase has reached the injection valve of autosampler turn on the autosampler power supply If the injection valve is switched over when no fluid is INITIAL the valve seal may be damaged To prevent this be sure to start the pump earlier The autosampler will go through the initialization sequence and then the INITIAL screen will appear 9 Press the WASH key of ...

Page 120: ...EAD VOLUME 10 0 REAR VOLUME 50 0 ASP SYRINGE SPEED 2 DSP SYRINGE SPEED 2 NEEDLE DOWN SPEED 1 AIR VOLUME 2 0 NEEDLE WASH TIME SOLVENT1 15 RINSE PORT WASH TIME 1 SYRINGE VOL 2 175 µL 11 Set the pump flow rate to 0 1 mL min 12 Set the detector wavelength to 265 nm Set the detector time constant to 0 5 s 13 Set the following conditions in the data processing unit SAMPLE PERIOD 100 ms STOP TIME 3 min ...

Page 121: ...on port and fill the flow path of the syringe system with the cleaning agent 4 Place a vial containing at least 1 mL of standard sample in rack position No 1 and set the rack in the autosampler 5 Press the START key of autosampler to start analysis The analysis is carried out 6 times The operating conditions during analysis are indicated on the display Ensure beforehand that the room temperature w...

Page 122: ... standard deviation RSD 100 x SD xi Retention time due to each injection n Number of injections Make sure the RSD value is 0 075 or less However this value represents the precision of not the pump alone but the entire chromatographic system Therefore the value varies with each stability of the autosampler and detector accuracy of the data processing unit and its processing parameters ...

Page 123: ...s instructed below 1 Operation check Put 0 5 mL of water on the liquid leak sensor And confirm the leak error Fig 4 2 Leak Sensor Position NOTES 1 When a solvent is used turn on the liquid leak sensor function 2 The liquid leak sensor may not detect a drop of leakage or high volatile solvents Always check the leakage even while the liquid leak sensor is turned ON 3 Visual confirmation of a liquid ...

Page 124: ...the liquid leak sensor and the drain tray And reinstall the liquid leak sensor on the drain tray NOTE When reinstalling the liquid leak sensor after removing and cleaning bring a tip of the sensor into contact with the drain tray Fig 4 3 Leak Sensor Fixation Screw NOTE Please install the liquid leak sensor in the correct position Otherwise it may cause malfunction of the sensor and an error Leak s...

Page 125: ...ple is apt to remain in the column This not only causes poor stability or drift but also shortens the column life Particles present in the sample plug the column filters Pressure will increases abnormally Impurities in the sample also contaminate the column Impurities cause erroneous data Occasionally clean the column by injecting a large amount 1 to 3 mL of solvent The injection of the solvent wi...

Page 126: ... air bubbles of wash fluid in the wash mechanism every day Depends on the state of the wash fluid it causes deterioration of the pump seal and the plunger Leaks lead to poor baseline stability and data reproducibility The net result of leaks is degradation of reliability in measurement ...

Page 127: ...d from the receptacle 1 If an abnormality occurs on the Model Chromaster 5160 pump an error message appears on the LCD Liquid Crystal Display Error displays result from either the detection of a fault during the self diagnostics at power up upon Initialization or from a problem which occurs during operation Fig 4 4 shows error detecting functions and the error messages Operation Function Error mes...

Page 128: ...t service office of Hitachi High Technologies Corporation sales representative 4 PARAMETER ERROR PARAMETERS ARE SET TO DEFAULT VALUE PARAMETER error 5 LOG INFORMATION ERROR LOG INFORMATION IS INITIALIZED LOG INFORMATION error 6 PRESSURE MAX LIMIT ERROR PRESS CL KEY TO CLEAR MESSAGE The upper pressure limit is exceeded 1 Check the flow for leaks or clogging 7 PRESSURE MIN LIMIT ERROR PRESS CL KEY T...

Page 129: ...program mode is not displayed 1 Display the monitor screen by pressing the ESC key 2 Set the program mode by pressing the INITIAL key 4 Purging can t be set or cancelled by pressing the PURGE key 1 monitor screen is not displayed 2 Waiting for numerical input Display the monitor screen by pressing the ESC key 5 A monitor lamp for the degassing unit doesn t light up 1 The power supply of the pump o...

Page 130: ...ipitation type wash with distilled water enough and replace with the target solvent completely 8 A leak error occurs 1 The liquid leaked 2 Dirt attached to the leak sensor 1 Clean up the leaked liquid in the drain tray Wipe the liquid attached to the leak sensor off Readjust the height of the leak sensor refer to 4 2 1 2 Wipe the liquid attached to the leak sensor off Readjust the height of the le...

Page 131: ...n the pushing screws Disassemble the Cell and clean See the instruction manual for the detector See 4 4 2 Abnormal Pressure Replace the Drain tube Inside diameter 0 33 mm length 2 m Valve etc Flow path system of Pump Drain tube Inside diameter of Length of Drain tube Vibration Environment Is there abnormal high pressure or abnormal fluctuation Is the tube a specified one No vibration from other in...

Page 132: ...iping from the inside of the Ferrule part and use it again 3 After using a salt solvent substitute distilled water for the inside of the Flow path system Check valve Bubbles are generated in Check valve Foreign matters in Check valve Open the Drain valve fully pump liquid for 3 5 minutes with the maximum flow rate This should be performed when bubbles are generated in the Pump after leaving the Pu...

Page 133: ... in Cell Leakage from Cell Detector Autosampler See 4 4 1 Cell Flow path system Leakage from piping connection Check leak visually Column Flow path system Deterioration of Column Leakage from piping connection Check leak visually Check Cell visually Tighten OK See 4 4 1 Cell Tighten OK Large variation of pressure See 4 4 2 Abnormal pressure Environment Influence to Column If Column oven is not use...

Page 134: ...uble vitamine analysis 2 Column Storage If the column is not used for a long time fill the column with a solvent seal the inlet outlet of the column and store it a Continue to make the solvent flow Flow rate 0 2 ml min 0 02 ml min with a semi micro column b Remove the piping from the outlet Connect a stopcock manually c Stop the Pump d Remove the piping from the inlet Connect a stopcock manually e...

Page 135: ...ics wavelength of the solvent that is a wavelength with less absorption Use a solvent for high speed liquid chromatography if possible b When using organic solvent be sure to degas it before using Fig 4 7 Solvetn Selection Stopcock Pump Outlet Inlet 0 2 ml min 0 02 ml min Absorbance Ultrasonic cleaner Aspirator Wavelength ...

Page 136: ...re increases abnormally When tightening a Teflon tube or a SUS pipe see the following a Push screw resin screw Tighten it fully with your fingers using no tools b Push screw SUS screw Tighten it fully with your fingers using no tools then re tighten with a wrench with a tightening torque of 4 N m to secure firmly Refer to the table shown below about an angle of re tightening Table 4 4 Angle of Re ...

Page 137: ...long time clean the detector then short the inlet and the outlet to seal the liquid so that the inside of the detector will not dry 7 Replacing Consumables A replacing period of consumables depends on the frequency in use However early replacing is recommended SUS ferrule SUS pipe SUS push crew ...

Page 138: ...he conditions solvent flow rate pressure prepare enough quantity of each part considering the actual conditions of use 5 1 Pump Main Unit Part No Name Shape and Specifications Position Used Normal Life 891 1213 Plunger seal Pump seal Color Black Pump head for Chromaster 5160 4 months 640 h 885 1884 Wash mechanism seal Wash mechanism plunger guide 4 month 640 h 810 1163 Plunger Pump head for Chroma...

Page 139: ...sn t work properly clean If this doesn t solve the problem replace the valve 1 3 year 893 0801 Check valve OUT 1 3 year 893 0903 Auto purge valve valve stator Auto purge valve Option 40000 times Filter 638 1423 Packing 638 1422 Packing B 891 1364 Check valve 810 1325 Packing A 810 1345 Packing A 810 1345 Check valve 810 1325 Valve holder IN 893 1248 IN OUT Valve holder OUT 893 1249 ...

Page 140: ...OD SUS pipe Rheodyne injector 655 1459 SUS push screw M 1 16 inch 1 57 mm OD SUS pipe Rheodyne injector 810 1310 PCTFE push screw 3 2 ID 3 mm OD PTFE tube Example of use Piping for solvent suction with Pump 810 1311 PCTFE push screw 2 2 ID 2 mm OD PTFE tube 810 1312 PCTFE push screw 2 1 ID 2 mm OD PTFE tube Example of use Piping from Low pressure gradient solenoid valve to pump 638 1099 SUS ferrul...

Page 141: ...gradient solenoid valve to pump 638 1140 PTFE tube 1 5 mm ID 3 0 mm OD 10 m Example of use Piping for suction of Pump Low pressure gradient unit 634 1976 Stainless steel pipe 0 25 mm ID 1 57 mm OD 5 m Example of use Internal piping of a Pump Standard piping of a Cell 633 1263 SUS Nipple 1 16 OD SUS pipe for connection 885 1601 SUS Nipple 1 16 OD SUS pipe for connection 885 1602 SUS Nipple 1 16 OD ...

Page 142: ...nnect the inlet tube and outlet pipes 1 2 from the pump heads using a 1 4 inch double end wrench of workshop tools 2 Loosen the hexagon screws alternately with a hex wrench and remove them 3 Carefully pull out the pump head toward you with both hands NOTE Take care not to damage the plunger Pump head Outlet pipe 1 Outlet pipe 2 Pump head Spring washer Hexagon screws Hex wrench Plunger wash mechani...

Page 143: ...en the pump seal remains in the plunger start the pump and as soon as the plunger has come out stop the pump and pull out the pump seal Wipe the surface of the plunger with gauze or any other soft cloth 6 Wash the pump head Wash the pump head thoroughly with distilled water or organic solvent Depending on the circumstances use a neutral detergent and or ultrasonic cleaner Guide Seal removing rod P...

Page 144: ...he plunger wash mechanism into the plunger while rotating it to the left and right gently The direction of the flow path of a plunger is shown in the figure 9 Next install the pump head on the main body of the pump as guided by the guide pin 10 Fix the pump head Two hexagonal screws are tightened up lightly with the hex wrench Next tighten alternately two hexagon screws little by little about 30 e...

Page 145: ...r bubbles from the flow path to the drain valve Then fill it with the mobile phase 13 Fill the plunger wash mechanism with deionized water When a new seal is used fastening loosens and leakage may occur In that case tighten up again with a hex wrench as indicated in this procedure Pump head Spring washer Hexagon screws Plunger wash mechanism Guide ...

Page 146: ...eal P N 885 2920 NOTE Recap after use the seal remover PV Keep the seal remover PV in an accessory box of Chromaster 5160 Pump 1 Loosen the purge valve knob in Open direction and pull it out 2 Screw the seal remover PV into a packing of a valve as the figure below indicates Pull down the seal remover PV and then pull up the packing to take it out 3 Attach a new valve seal at the end of drain knob ...

Page 147: ...w path filters Filter P N 638 1423 Seal P N 638 1422 for filters 1 Using the wrench 21 loosen and remove the flow path filter from the drain valve 2 Align the wash bottle nozzle with the filter outlet Wash away foreign matter from the filter surface 3 Use an ultrasonic cleaner if the contamination is excessive Flow path filter Receiving tray Flow path filter Ultrasonic cleaner Beaker Flow path fil...

Page 148: ...y push and mount the new filter into the flow path filter 6 Before attaching the flow path filter to the drain valve clean the flow path by running the pump 7 Attach the flow path filter to the lower right canted part of the drain valve Align the flow path filter with the drain valve and tighten it securely with the wrench 21 NOTE Poor tightening may cause leaks Flow path filter Freezer 10 C about...

Page 149: ... 5 1 Front Face of Chromaster 5160 Pump 1 Loosen the cap of the mobile phase bottle 2 Pull out the inlet tube from the mobile phase bottle 3 Remove the solvent filter from the inlet tube Inlet tube Cap Extract Mobile phase bottle Solvent filter Inlet tube Column Sample bottle Purge valve Inlet tube ...

Page 150: ...s 5 Replace the wash fluid with distilled water Run the ultrasonic cleaner for an additional 5 to 6 minutes Repeat this operation three or more times to eliminate the wash fluid 6 After removing the moisture from the filter mount on the inlet tube again Solvent filter Beaker Wash fluid Distilled water Ultrasonic cleaner Inlet tube Insert Solvent filter ...

Page 151: ...llowing the procedure Required Articles Workshop tools P N 810 1353 Wash fluid Neutral detergent Ultrasonic cleaner Beaker Make sure the pump head lock nuts are securely tightened 1 Remove the inlet tube and the outlet pipe 1 from the check valve suction and discharge side 2 Loosen the check valve suction and discharge side Remove them along with the valve holder using the M10 wrench Check valve D...

Page 152: ... packings B are disengaged and the inner parts come loose when washing reassemble them using the illustration as a guide Position the check valve so liquid enters from the valve seat side One side of the check valve seat is glossy while the other side is not When assembling the valve seat set it so that the glossy side will be oriented to the ball contacting direction Valve holder assembly Beaker ...

Page 153: ...y tool after loosening Attach the valve again as in 6 above 8 After 12 hours or more from attaching the valve tighten the valve with the wrench 10 by about 30 degrees 9 Install the inlet tube and outlet pipe 1 in the reverse order of their removal With the drain valve open start the pump to fill the pump head and tube with the mobile phase and to expel bubbles from the lines and the pump head 10 C...

Page 154: ...valve 1 Remove the check valve suction and discharge side referring to 1 and 2 in 5 7 2 Place a rather large piece of paper on a table Remove the packing B refer to 3 Position the valve holder slightly aslant Gently tap the valve holder against the table and take out the check valves and packings from the inside 3 Fill the beakers with the wash fluid distilled water Combine the new packings valve ...

Page 155: ...k valve using the correct procedure NOTE When assembling do not make a mistake in the check valve orientation and placement of the valve seat faces The glossy side of the valve seat should face the ball NOTE The valve seat and ball are used as a pair Be sure to assemble the same pair together Valve holder Packing A Check valve Packing A Check valve Packing B Packing A Check valve Packing A Check v...

Page 156: ...of the liquid supply is correct Refer to 6 through 8 in 6 7 NOTE When assembling do not exchange the suction and discharge sides Direction of liquid flow Glossy side Top Valve chest Ball Valve seat Filter paper Direction of liquid flow Check valve Discharge side Packing B 891 1364 Check valve 810 1325 Packing A 810 1345 Check valve 810 1325 Packing A 810 1345 Holder IN 893 1248 Check valve Suction...

Page 157: ... Disconnect the inlet tube and outlet pipes 1 2 from the pump heads Refer to 5 3 Replacement of Pump Seal 2 Loosen the hexagon screws alternately with a hex wrench and remove them 3 Carefully pull out the pump head toward you with both hands When the plunger seal remains in the pump head replace it if needed Refer to 5 3 Replacement of Pump Seal When the plunger seal remains in the plunger replace...

Page 158: ... Remove the wash mechanism seal placed between the bearing and the seal holder When the wash mechanism seal remains pull out it by screwing the exclusive seal removing rod into it 7 Wash the pump head Wash the pump head thoroughly with distilled water or organic solvent Depending on the circumstances use a neutral detergent and or ultrasonic cleaner 8 Wipe the surface of the plunger with gauze or ...

Page 159: ...tly The direction of the flow path of a plunger is shown in the figure 12 Next install the pump head on the main body of the pump as guided by the guide pin 13 Fix the pump head Two hexagonal screws are tightened up lightly with the hex wrench Next tighten alternately two hexagon screws little by little about 30 each 4 to 5 times with the hex wrench to secure the pump head NOTE Tighten two hexagon...

Page 160: ...r bubbles from the flow path to the drain valve Then fill it with the mobile phase 16 Fill the plunger wash mechanism with deionized water When a new seal is used fastening loosens and leakage may occur In that case tighten up again with a hex wrench as indicated in this procedure Pump head Spring washer Hexagon screws Plunger wash mechanism Guide ...

Page 161: ...seal P N 893 0902 Auto purge valve stator P N 893 0903 1 Remove tubes a tube for the autosampler a drain tube tube from the pressure sensor connected to the injection valve with the double end wrench 1 4 inch NOTE Avoid loosing the screw cap It may cause performance degradation or a short duration of life 2 Remove stator lock nuts 3 pcs with the hexagon wrench And remove the injection valve stator...

Page 162: ...rews equally to prevent failure operation of a valve wear of a rotor seal and damage 6 Connect each tube to the auto purge valve in the reverse order of their removal 7 Start delivering liquid of the pump via the auto purge valve 8 Make sure that there is no leakage after the seal replacing NOTE Avoid moving a valve when the inside of the valve is dried A seal wears away abnormally NOTE Decrease o...

Page 163: ...X 2 1 ENT 2 9 ERROR OUT 3 38 ESC 2 8 EVENT 2 5 Event code 3 27 F Ferrule 5 3 Flow path filter 5 10 Flow rate accuracy 2 10 Flow rate calibration 3 21 Flow rate precision 2 10 Frequency APPENDIX 1 2 G GLP 2 7 Grounding APPENDIX 1 4 I INSERT 2 8 Installation APPENDIX 1 1 Isocratic system APPENDIX 1 9 APPENDIX 1 10 APPENDIX 3 1 ...

Page 164: ...acking 5 1 5 11 Parts replacement 5 1 Plunger 5 1 Power connector APPENDIX 1 8 APPENDIX 1 9 APPENDIX 1 10 Power supply 2 11 Pressure calibration 3 22 Pressure monitor 3 46 Pressure unit 3 23 PROG 2 7 Programming 3 13 Pump mode 2 7 3 61 Pump seal 5 5 PURGE 2 7 3 3 Purge valve 2 1 5 9 Push screw 5 3 R Removing dust 3 75 3 78 S Seal 5 1 Specifications 2 10 Static electricity 3 48 3 64 3 70 3 74 ...

Page 165: ...INDEX 3 U UI Pad 2 6 UTLTY 2 7 3 18 W Wiring covers 2 4 APPENDIX 1 19 Z Zero pressure calibration 3 18 ...

Page 166: ...h NOTE It is not permitted for the user to carry out installation at the time of delivery For ensuring safety and high accuracy in operation of the instrument installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its authorized service agent Before installation however the user shall make adequate preparations for installi...

Page 167: ...t be filled with gas of an organic solvent particularly benzine and paint thinner which dissolves coating 4 Other general precautions on instrument a Shall not be exposed to direct sunlight Otherwise performance degradation or coating discoloration might be caused Avoid a place near windows as far as possible b Shall not be exposed to draft c Shall be free from strong vibration or shock which can ...

Page 168: ...n shall be 0 5 Hz of the rated frequency 3 Power Capacity 100 VA or more for a single unit and 600 VA or more for the total system The total system shown comprises an organizer Chromaster 5110 5160 pump Chromaster 5210 5260 autosampler Chromaster 5310 column oven Chromaster 5410 5420 5430 5450 detector Confirm the necessary power capacity taking actual system configuration and OA equipment in the ...

Page 169: ...ument The use of a different type of power cable may result in an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet as a rule b If a grounded 3P power outlet is not available use a 3P table tap with a grounding wire or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or larger and a...

Page 170: ...more below ground Copper plate Example of grounding electrode Grounded 3P power outlet 15 A Ground resistance 100 or less Grounding electrode underground section Grounding construction for 100 or less Grounded 3P table tap Chromaster 5110 5160 pump Connector Rear panel 300 mm 2 mm 10 mm Organizer or AC adapter option ...

Page 171: ...n for 100 or less 3P table tap with grounding wire Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Chromaster 5110 5160 pump Connector Rear panel Organizer or AC adapter option 10 mm 2 mm 300 mm b 2 With 2P power outlet having a grounding terminal Power outlet with grounding terminal Grounding terminal 2P 3P adapter Grounding wire green Screw diameter M...

Page 172: ...ecessary For installation prepare a level and sturdy bench which withstands a load of 150 kg or more The system conceived here is an example in which Chromaster organizer Chromaster 5110 5160 pump Chromaster 5210 5260 autosampler Chromaster 5310 column oven and Chromaster 5410 5420 5430 5450 detector are stacked Confirm the necessary space taking the actual system configuration and OA equipment in...

Page 173: ...e organizer unit has been prepared To the organizer available at option one pump one autosampler and one detector can be connected For the column oven the power cord needs to be connected to the column oven unit If a single organizer is inadequate due to use of 2 detectors for example an AC adapter option that matches the instrument concerned needs to be used Connect the power cable from the organ...

Page 174: ... N 892 6912 attached to organizer AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 5160 pump Chromaster 5210 5260 autosampler and Chromaster 5410 5420 5430 5450 detector plug the connector cable from the organizer into the power connector of each unit Chromaster 5410 5420 5430 5450...

Page 175: ...tely available AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 5160 pump Chromaster 5210 5260 autosampler and Chromaster 5410 5420 5430 5450 detector plug the connector cable from the organizer into the power connector of each unit Chromaster 5410 5420 5430 5450 detector Chromaste...

Page 176: ...Connection Appended Table 1 3 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampler and interface control board Rear panel of module unit e Line connector Power connector Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 5260 autosampler Interface control board Chrom...

Page 177: ... cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampler fluorescence detector and interface control board Chromaster 5410 5420 5430 detector Chromaster 5440 fluorescence detector Chromaster 5310 column oven Chromaster 5210 5260 autosampler Interface control board e Line cable 1 e Line cable 2 Chromaster organizer Chromaster 5110 5160 pump ...

Page 178: ...r column and detector through the central hole of the drain tray 1 Isocratic System Appended Fig 1 8 Tubing Diagram of Isocratic System stacked in one block Drain receiver Detergent Mobile phase liquid Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 5260 autosampler Wash pump Chromaster 5110 5160 pump Degassing unit Drain Syringe valve Injec...

Page 179: ...ection valve in the autosampler Connect port 5 of the injection valve to the inlet of column To the outlet of column connect the inlet tube of detector cell Connect the detergent container to the wash pump of autosampler through the degassing unit Chromaster 5440 fluorescence detector Detector cell Chromaster 5310 column oven Column Injection valve Chromaster 5210 5260 autosampler Wash pump Drain ...

Page 180: ...stem stacked in one block Detergent Mobile phase liquid Chromaster organizer Chromaster 5410 5420 5430 detector Chromaster 5310 column oven Chromaster 5210 5260 autosampler Wash pump Low pressure gradient unit proportioning valve Chromaster 5110 5160 pump Drain Degassing unit Syringe valve Injection valve ...

Page 181: ...t the purge valve of pump to port 4 of the injection valve in the autosampler Also connect port 5 of the injection valve to the inlet of column To the outlet of column connect the inlet tube of detector cell Connect the detergent container to the wash pump of autosampler through the degassing unit Chromaster 5440 fluorescence detector Detector cell Chromaster 5310 column oven Column Injection valv...

Page 182: ...hed to organizer Drain tube 4 P N 893 2873 attached to organizer Drain tube P N 080 3090 attached to autosampler T joint P N 810 1362 attached to organizer T joint N1 P N 890 3493 attached to autosampler L joint P N L369125 attached to organizer Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 5260 autosampler Chromaster 5110 5160 pump Drain ...

Page 183: ...nizer T joint N1 P N 890 3493 attached to autosampler I joint P N 893 2876 attached to autosampler L joint P N L369125 attached to organizer 5 4 GUI Controller The GUI controller is a touch panel type operation panel This operation panel alone enables the user to control the respective modules For operation refer to the instruction manual of the GUI controller Chromaster organizer Drain tube A1 3 ...

Page 184: ...installing the instrument provide a proper means for preventing the instrument from tipping over accidentally On the rear of each module unit a cabling cover is attached The adjacent models are fastened with each other by attaching the fastening plate between the wiring covers Appended Fig 1 14 Fastening between Component Units Fastening plate Fastening screw ...

Page 185: ...are contact signals that are input and output via 3 pin connector Their names and functions vary with the unit A name that indicates the function is given at each connector Example of output contact signal EVENT of pump Example of input contact signal LAMP OFF IN of detector 2 Contact Signals Entering the e Line Connector Each unit has two e Line connectors for connection at the rear of the main u...

Page 186: ...ection Connect the START L and G terminals of the e DIO cable 890 6146 to the EXTERNAL COM terminal of the Model D 2500 To L 2000 series instrument To Chromaster series instrument e Line connector 3 pin connector BUSY ERROR STOP START e Line connector e DIO cable 890 6145 e DIO cable 890 6145 D 2500 START COM EXTERNAL H L BUSY H L G START BUSY e Line connector To Chromaster series instrument ...

Page 187: ...al Output Terminals These are contact signal input terminals for control using contact signals of an external unit The output circuit is shown in Appended Fig 2 4 The rating of contacts used is 12 V 0 1 A Make sure the load connected does not exceed this rating Appended Fig 2 1 e Line Cable Connection Appended Fig 2 2 e Line Contact Circuit Configuration e Line cable Other unit Chromaster series u...

Page 188: ...ontacts of external unit Appended Fig 2 3 Contact Signal Input Circuit Appended Fig 2 4 Contact Signal Output Circuit 5 V 320 Chromaster series unit External unit Max 10 mA 0 1 A max 30 V max 1 2 3 Chromaster series unit External unit 1 2 3 ...

Page 189: ...f two to four mobile phases is varied with time for analytical operation Liquid leak sensor A sensor to detect liquid leakage in a column oven It detects fluid in a drain tray Initialize To reset the instrument in the initial status Initial screen After power on the initial screen appears upon completion of initialization Warming up To warm the instrument for stable analysis Error message A messag...

Page 190: ...APPENDIX 3 2 Log book Means the information containing records of instrument operating conditions ...

Page 191: ...ctions in this manual and the WARNING CAUTION labels on the instrument Keep this manual in a safe place nearby so it can be referred to whenever needed 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 3rd Edition June 2011 Copyright C Hitachi High Technologies Corporation 2011 1st Edition 2011 All rights reserved Printed in Japan Part No 892 9805 2 HH M RT HMS ...

Page 192: ... party in any form or by any means without the express written permission of Hitachi High Technologies Corporation 3 Hitachi High Technologies Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 193: ...al data but also in consequences adverse to safety Note that it is allowed only for persons having a basic knowledge of chemical analysis procedures to use this instrument Carefully read this instruction manual before attempting operation For proper use of the software please acquaint yourself with it The liquid chromatograph system comprises a pump unit for delivering mobile phases a sample intro...

Page 194: ... SAFETY SUMMARY collected and summarized Section 1 GENERAL Outline of Chromaster Organizer Section 2 FUNCTIONS Name and Function of Each Part on Pump Specifications Section 3 REPLACEMENT PARTS Replacement Procedure Section 4 TROUBLESHOOTING Section 5 INDEX APPENDIX1INSTRATTION APPENDIX2TERMINOLOGY First of all read IMPORTANT and SAFETY SUMMARY at the beginning of this manual for ensuring safety in...

Page 195: ... Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be available in original ve...

Page 196: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 197: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Technologies does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Technologies or its related companies or application of said instrument Installation Re...

Page 198: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 199: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 200: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 201: ...affected by electromagnetic noise within the permissible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power devi...

Page 202: ...d NOTICE or NOTE is used to indicate precautionary instructions concerning possible property damage NOTICE Used to indicate a potentially hazardous situation which if not avoided will or can result in damage to user s property serious damage to the instrument damage to data or environmental pollution though personal injury may not be incurred NOTE Used to indicate explanatory information for ensur...

Page 203: ...tric shock or fire Radiation from the Laser Light Source WARNING The internal CD ROM or CD R W drive of the PC is provided with a laser beam source In normal operation of the PC containing the laser beam source no laser beam harmful to human health will be emitted outside Note however that if a laser beam leaking out of the PC accidentally gets into the eye eye injury could occur When using the PC...

Page 204: ...vent or waste solution Leakage of solvent inside the instrument Section 1 When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution employ and provide proper grounding connection to it Section 1 Explosion of Vapor from Flammable Chemicals If a flammable chemical such as org...

Page 205: ...n electric shock hazard Connect the 3P power cable to a grounded 3P power outlet b If a grounded 3P power outlet is not available use a grounded 3P table tap or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 mm APPENDIX...

Page 206: ...s in the Manual CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over When installing the instrument provide a proper means for preventing the instrument from tipping over accidentally APPENDIX 1 ...

Page 207: ...odically check the appearances of these warning labels to see if they are clean to allow easy reading over a safe distance If any one of the warning labels becomes illegible due to deterioration contact your local Hitachi High Technologies Corporation sales representative or service office of Hitachi High Technologies Corporation sales representative for replacement with a new one 1 Electric Shock...

Page 208: ...evant laws and regulations regarding water pollution control and sewage treatment Improper treatment of waste solution may result in environmental pollution and could also lead to a penalty Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally If necessary conduct measurement on a control sample ...

Page 209: ...Countries IMPORTANT 6 Other Precautions IMPORTANT 6 SAFETY SUMMARY SAFETY 1 General Safety Precautions SAFETY 2 WARNING Precautions in the Manual SAFETY 3 CAUTION Precautions in the Manual SAFETY 5 WARNING and CAUTION Labels on Instrument SAFETY 6 NOTICE Precautions SAFETY 7 1 GENERAL 1 1 1 1 Outline of Chromaster Organizer 1 3 1 2 Configuration of Liquid Chromatograph System 1 3 1 2 1 Isocratic S...

Page 210: ...ENDIX 1 3 3 1 Power Supply Arrangement APPENDIX 1 3 3 2 Installation Space APPENDIX 1 7 4 Check against Packing List APPENDIX 1 7 5 Assembling APPENDIX 1 8 5 1 System Power Supply APPENDIX 1 8 5 2 System Cabling APPENDIX 1 11 5 3 System Tubing APPENDIX 1 13 5 4 Fastening between Component Units APPENDIX 1 19 APPENDIX 2 TERMINOLOGY APPENDIX 2 1 ii ...

Page 211: ...urce near the instrument b Well ventilate the laboratory room where the instrument is used c Always check the following conditions If an abnormality is found stop operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity...

Page 212: ...ilate the laboratory room adequately WARNING Inflammation or Injury due to Toxic Corrosive or Stimulative Solvent When using a toxic corrosive or stimulative solvent be careful not to incur a physical inflammation or injury For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper ...

Page 213: ...ystem The liquid chromatograph system consists of a pump for feeding an eluent a sample introducing section autosampler manual injector for injecting a sample a column for chromatographic separation of the injected sample a column oven for maintaining the column at a constant temperature and a detector section for detecting a signal of a separated component of the sample In addition a degassing un...

Page 214: ...ted from the autosampler 3 The injected sample is separated through the column which is maintained at a constant temperature by the column oven 4 Each component separated from the sample is then detected as a signal by the detector Chromaster 5110 pump Chromaster 5310 column oven Chromaster 5210 autosampler Chromaster 5410 5420 5430 5440 detector Mobile phase Column Wash fluid Degassing unit Injec...

Page 215: ... pressure gradient unit proportioning valve Mobile phase Chromaster 5110 pump Chromaster 5310 column oven Chromaster 5210 autosampler Chromaster 5410 5420 5430 detector Injection valve Wash pump Drain Degassing unit Syringe valve Fig 1 2 Low Pressure Gradient System 1 Each of plural eluents is fed from the degassing unit to the low pressure unit 2 In the low pressure unit the eluents are mixed at ...

Page 216: ...d Chromatograph System 5 The injected sample is separated through the column which is maintained at a constant temperature by the column oven 6 Each component separated from the sample is detected as a signal by the detector 1 6 ...

Page 217: ...power is turned on Front bar The front bar is lowered before the reagent bottle is set up It is locked in the upper position after setup AC inlet Ground terminals Fig 2 2 Rear side View Wiring covers The power connector to be connected to Chromaster Series unit appears when the left wiring cover viewed from the front is removed 2 1 ...

Page 218: ...r button Turn on and off the power Power connector for pump Power connector for AS Power connector for detector Power connector for IFC Fig 2 4 Left side View Power connector for pump Connect the dc power cord for pump Power connector for AS Connect the dc power cord for AS Power connector for IFC Connect the dc power cord for Interface control board IFC Power connector for Detector Connect the dc...

Page 219: ... pump 1 unit Chromaster 5210 autosampler 1 unit Chromaster 5410 5420 5430 5450 detector 1 unit Interface Control Board 1 unit 3 Operating Temperature Range 4 to 35 C without dew condensation 4 Operating Humidity Range 25 to 85 RH 5 Dimensions 340 width 420 depth 200 height mm 6 Weight Approx 9 kg 7 Reagent Bottles Mountable 1000 mL bottle 6 pieces 500 mL bottle 3 pieces 2 3 ...

Page 220: ...eplacement 1 Item to be Prepared New fuse Part No J821337 Be sure to use a time lag fuse having the specified rating T6 3AL for 250 V 2 Pre check Condition Make sure that the power switch of the instrument is turned off and that the power cord is disconnected from the instrument 3 How to Replace the Fuse a Remove the fuse holder by hooking a tool having a thin and flat tip such as blade edge screw...

Page 221: ...3 1 Replacement Procedure b Replace the fuse with a new one and then attach the fuse holder by pressing it 3 2 ...

Page 222: ...ied to organizer main unit 2 Check that power connector for the organizer and instrument is connected securely 3 If power is still not supplied despite taking the above steps 1 and 2 contact our service office of Hitachi High Technologies Corporation sales representative 2 LED does not light up 1 Power is not supplied to organizer main unit 1 Check that power is supplied to organizer main unit 2 I...

Page 223: ... SAFETY 4 SAFETY 6 3 1 Explosion of Vapor from Flammable Chemicals SAFETY 3 F Fuse 3 1 G Grounding terminal APPENDIX1 4 H How to replace the fuse 3 1 I Ignition of flammable chemicals SAFETY 3 Instrument tipover SAFETY 5 Isocratic system 1 4 L LED 2 1 Low pressure gradient system 1 5 O Outline organizer 1 3 5 1 ...

Page 224: ...ector APPENDIX1 8 Power switch 3 1 Precautions on CE conformity marking IMPORTANT 4 S Specifications 2 3 T Troubleshooting 4 1 W Warning and caution labels on instrument SAFETY 6 Warranty on Product IMPORTANT 1 5 2 ...

Page 225: ...not permitted for the user to carry out installation at the time of delivery For ensuring safety and high accuracy in operation of the instrument installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its authorized service agent Before installation however the user shall make adequate preparations for installing the instru...

Page 226: ...ith gas of an organic solvent particularly benzine and paint thinner which dissolves coating 4 Other general precautions on instrument a Shall not be exposed to direct sunlight Otherwise performance degradation or coating discoloration might be caused Avoid a place near windows as far as possible b Shall not be exposed to draft c Shall be free from strong vibration or shock which can be felt by yo...

Page 227: ...t 1 Power supply voltage 100 to 115 V AC 220 to 240 V AC Fluctuation shall be 10 of the rated voltage 2 Frequency 50 or 60 Hz Fluctuation shall be 0 5 Hz of the rated frequency 3 Power Capacity 450 W Confirm the necessary power capacity taking actual system configuration and OA equipment in the installation room into account and prepare a power supply having an adequate power capacity 4 Power outl...

Page 228: ...of a different type of power cable may result in an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet as a rule b If a grounded 3P power outlet is not available use a 3P table tap with a grounding wire or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or larger and a turn count of...

Page 229: ...cord attached to instrument Chromaster Organizer Ground resistance 100 Ω or less 750 mm or more below ground Connector Rear panel Copper plate Grounding electrode underground section 300 mm Grounding construction f 100 Ω or less or 2 mm 10 mm Example of grounding electrode Appended Fig 1 1 Grounding Method APPENDIX 1 5 ...

Page 230: ...pended Fig 1 2 Connection when Only 2P Power Outlet is Available b 1 With 2P power outlet Copper plate Grounding electrode underground section Turn count 3 or more Wire thickness 1 25 mm Grounding construction for 100 Ω or less Power outlet with grounding terminal Grounding terminal 2P 3P adapter Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Chromaste...

Page 231: ...cks becomes 100 mm If the clearance between the blocks is wider than 100 mm the length of DC power cable may become inadequate For installation prepare a level and sturdy bench which withstands a load of 150 kg or more The system conceived here is an example in which Chromaster organizer Chromaster 5110 pump Chromaster 5210 autosampler Chromaster 5310 column oven and Chromaster 5410 5420 5430 5450...

Page 232: ...tosampler one Chromaster 5410 5420 5430 5450 detector and one IFC board can be connected For the Chromaster 5310 column oven and Chromaster 5440 fluorescence detector the power cord needs to be connected to the column oven unit If a single organizer is inadequate due to use of 2 detectors for example an AC adapter that matches the instrument concerned needs to be used Connect the power cable from ...

Page 233: ...le 1 P N 892 6909 attached to organizer Connector cable 2 P N 892 6910 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 4 P N 892 6912 attached to organizer AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster 5210 autosampler a...

Page 234: ...e Used Connector cable 1 P N 892 6909 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 5 P N 892 6914 separately available Connector cable 6 P N 892 6913 separately available AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster ...

Page 235: ...ure Gradient System Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump e Line cable 1 e Line cable 2 Appended Fig 1 6 e Line Cable Connection Appended Table 1 3 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosamp...

Page 236: ...Chromaster 5210 autosampler Interface control board e Line cable 1 e Line cable 2 Chromaster organizer Chromaster 5110 pump Appended Fig 1 7 e Line Cable Connection Appended Table 1 4 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampler fluorescence detector and interface control board APPENDIX 1 12 ...

Page 237: ...sampler column and detector through the central hole of each module unit 1 Isocratic System Detergent Mobile phase liquid Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Chromaster 5110 pump Degassing unit Drain Injection valve Column Syringe valve Appended Fig 1 8 Tubing Diagram of Isocratic System stacked in one block...

Page 238: ...m stacked in two blocks Connect the inlet tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the inlet of pump Connect the purge valve of pump to port 4 of the injection valve in the autosampler Connect port 5 of the injection valve to the inlet of column To the outlet of column connect the inlet tube of detector cell Connect the deterg...

Page 239: ...420 5430 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Low pressure gradient unit proportioning valve Chromaster 5110 pump Drain Degassing unit Syringe valve Injection valve Appended Fig 1 10 Tubing Diagram of Low Pressure Gradient System stacked in one block APPENDIX 1 15 ...

Page 240: ...et tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the IN port of proportioning valve Connect the OUT port of the proportioning valve in the low pressure gradient unit to the 4 way joint Then connect the purge valve of pump to port 4 of the injection valve in the autosampler Also connect port 5 of the injection valve to the inlet of ...

Page 241: ...for Drain when stacking module units in one block Appended Table 1 5 Drain Tubes to be Used Drain tube A2 P N 893 2874 attached to organizer Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 P N 893 2872 attached to organizer Drain tube 4 P N 893 2873 attached to organizer Drain tube P N 080 3090 attached to autosampler T joint P N 810 1362 attached to organizer T joint N1 P N 890 349...

Page 242: ...ed to autosampler Drain tube 2 P N 080 3090 separately available T joint P N 810 1362 attached to organizer T joint N1 P N 890 3493 attached to autosampler I joint P N 893 2876 attached to autosampler L joint P N L369125 attached to organizer Chromaster organizer Drain tube A1 3 Drain tube B1 T joint L joint Chromaster 5110 pump Chromaster 5440 fluorescence detector Chromaster 5310 column oven T j...

Page 243: ... instrument provide a proper means for preventing the instrument from tipping over accidentally On the rear of each module unit a cabling cover is attached The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers Fastening plate Fastening screw Appended Fig 1 14 Fastening between Component Units APPENDIX 1 19 ...

Page 244: ......

Page 245: ...l network IFC Interface control board to control the chromaster series instrument by PC One IFC for every one system is required Isocratic system A single liquid is fed using one pump Low pressure gradient system Using one pump a mixing ratio of two to four mobile phases is varied with time for analytical operation APPENDIX 2 1 ...

Page 246: ...ing labels Keep this manual in a safe place nearby so it can be referred to whenever needed Copyright Hitachi High Technologies Corporation 2011 All rights reserved Printed in Japan Part No 892 9520 1 HH M SG LT 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 3rd Edition June 2011 Copyright C Hitachi High Technologies Corporation 2011 1st Edition 2011 All rights reserved Printed in Japan Part ...

Page 247: ... party in any form or by any means without the express written permission of Hitachi High Technologies Corporation 3 Hitachi High Technologies Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 248: ...es adverse to safety Note that it is allowed only for persons having a basic knowledge of chemical analysis procedures to use this instrument Carefully read this instruction manual before attempting operation For proper use of the software please acquaint yourself with it The liquid chromatograph system comprises a pump unit for delivering mobile phases a sample introduction unit for injecting sam...

Page 249: ...stem Low Pressure Gradient System Section 2 FUNCTIONS Explanation of Power Switch and Others on Front Panel Section 3 OPERATION Basic Operations Utility Setting Section 4 MAINTENANCE CHECKUP Confirmation of Basic Actions Section 5 REPLACEMENT PARTS Replacement Parts and Consumables Section 6 INDEX APPENDIX1INSTRATTION APPENDIX2EXPLANATION OF CONTACT SIGNALS APPENDIX3TERMINOLOGY First of all read I...

Page 250: ...ope of Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be available in origi...

Page 251: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 252: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Technologies does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Technologies or its related companies or application of said instrument Installation Re...

Page 253: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 254: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 255: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 256: ...affected by electromagnetic noise within the permissible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power devi...

Page 257: ...l word NOTICE or NOTE is used to indicate precautionary instructions concerning possible property damage NOTICE Used to indicate a potentially hazardous situation which if not avoided will or can result in damage to user s property serious damage to the instrument damage to data or environmental pollution though personal injury may not be incurred NOTE Used to indicate explanatory information for ...

Page 258: ...tric shock or fire Radiation from the Laser Light Source WARNING The internal CD ROM or CD R W drive of the PC is provided with a laser beam source In normal operation of the PC containing the laser beam source no laser beam harmful to human health will be emitted outside Note however that if a laser beam leaking out of the PC accidentally gets into the eye eye injury could occur When using the PC...

Page 259: ...r waste solution Leakage of solvent inside the instrument Section 3 6 4 4 When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution employ and provide proper grounding connection to it Section 3 6 4 4 Explosion of Vapor from Flammable Chemicals If a flammable chemical such ...

Page 260: ...zard Connect the 3P power cable to a grounded 3P power outlet b If a grounded 3P power outlet is not available use a grounded 3P table tap or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 mm APPENDIX 1 Inflammation or ...

Page 261: ...ufficiently Section 5 2 Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over When installing the instrument provide a proper means for preventing the instrument from tipping over accidentally APPENDIX 1 Fatigue due to Long Hour Operation If you keep working with the display monitor and keyboard for long hours your eyes and body will be fatigued to jeopardi...

Page 262: ...y check the appearances of these warning labels to see if they are clean to allow easy reading over a safe distance If any one of the warning labels becomes illegible due to deterioration contact your local Hitachi High Technologies Corporation sales representative or service office of Hitachi High Technologies Corporation sales representative for replacement with a new one 1 Ignition of Flammable...

Page 263: ...SAFETY 7 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument 4 Burns due to Contact with Hot Parts 3 Electric Shock due to Contact with Power Supply to Light Source Front View ...

Page 264: ...urthermore leakage of a highly volatile solvent may not be detected Be sure to check for liquid leakage regularly to prevent a possible serious accident regardless of whether the leak sensor is activated or not a In routine inspection of the instrument visually check for liquid leakage before attempting measurements b In periodic inspection of the instrument check that the leak sensor works normal...

Page 265: ...surement on a control sample Possible Carryover When examining the results of measurements take account of the possibility of occurrence of a carryover Otherwise a correct judgment may not be formed Since fluorocarbon resin quartz and SUS 316 materials are used for the wetted parts of piping particular attention should be paid when analyzing samples that are likely to be adsorbed by these material...

Page 266: ...TY SUMMARY SAFETY 1 General Safety Precautions SAFETY 2 WARNING Precautions in the Manual SAFETY 3 WARNING SAFETY 3 CAUTION Precautions in the Manual SAFETY 5 CAUTION SAFETY 5 WARNING and CAUTION Labels on Instrument SAFETY 6 NOTICE Precautions SAFETY 8 1 OVERVIEW 1 1 1 1 Isocratic System 1 1 1 2 Low Pressure Gradient System 1 3 2 FUNCTIONS 2 1 2 1 Explanation of Power Switch and Others on Front P...

Page 267: ...am 3 40 3 4 7 Example of Time Program Operation 3 40 3 5 Setups 3 44 3 5 1 Selection of Communication Channel 3 45 3 5 2 Setting of Thermostatic Flow Cell 3 46 3 5 3 Setting of LCD Contrast 3 47 3 6 Before Analysis 3 48 3 6 1 Precautions on Selection and Handling of Mobile Phase 3 49 3 6 2 Characteristics of Organic Solvents 3 53 3 6 3 Caution on Static Electricity 3 57 3 7 Preparatory Operation 3...

Page 268: ...TALLATION APPENDIX 1 1 1 Unpacking APPENDIX 1 1 2 Place for Installation APPENDIX 1 1 3 Items to be Prepared by Customer APPENDIX 1 3 3 1 Power Supply Arrangement APPENDIX 1 3 3 2 Installation Space APPENDIX 1 7 4 Check against Packing List APPENDIX 1 8 5 Assembling APPENDIX 1 8 5 1 Removal of Transport Screws APPENDIX 1 8 5 2 System Power Supply APPENDIX 1 10 5 3 System Cabling APPENDIX 1 13 5 4 ...

Page 269: ...as analytical signals Also a degassing unit for degassing mobile phase liquid a gradient elution unit for changing the mixing ratio of eluents with time and other options may be added to the system as required 1 1 Isocratic System This is a simple system for analysis with a single mobile liquid phase Detergent Mobile phase Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 531...

Page 270: ...assing unit 2 A sample is injected with the autosampler 3 The injected sample is separated into its constituents with the column maintained at a constant temperature by means of the column oven 4 The separated sample constituents are taken out as analytical signals with the detector 1 2 ...

Page 271: ...zer Chromaster 5410 5420 5430 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Low pressure gradient unit proportioning valve Chromaster 5110 pump Drain Degassing unit Syringe valve Injection valve Fig 1 2 Low Pressure Gradient System 1 Mobile phase liquid is sucked into the low pressure gradient unit from the degassing unit 2 In the low pressure gradient unit plural elue...

Page 272: ...m 4 The injected sample is separated into its constituents with the column maintained at a constant temperature by means of the column oven 5 The separated sample constituents are taken out as analytical signals with the detector 1 4 ...

Page 273: ...ED Four kinds of LEDs are mounted and indicate the respective statuses LED Name color LED Status CH1 blue orange Blue Use in CH1 Orange Occurrence of error during use in CH1 CH2 blue orange Blue Use in CH2 Orange Occurrence of error during use in CH2 D2 LAMP blue 1 Lights in blue while D2 lamp is lit 2 Does not light while D2 lamp is put out W LAMP blue 1 Lights in blue while W lamp is lit 2 Does ...

Page 274: ... UI pad or operations from the chromato data station The functions of respective keys are listed in the table below For details of operation keys refer to Chapter 3 No Indication Function Refer to 1 A Z Auto Zero Calibrates to zero the ABS indication and output at the measuring wavelength 3 1 3 2 WL Wavelength Sets the measuring wavelength 3 1 4 3 SET UP Utility setup 1 Sets offset value time cons...

Page 275: ...utput of stored spectral data 3 4 6 10 RECORD 4 Record Used to specify the recorder full scale range recorder output speed and output data 3 4 2 11 SPECT 5 Spectrum Used to scan the specified wavelength range and store the spectral data in memory 3 4 1 12 MARKER 1 Marker Outputs a marker on recorder output 3 4 3 13 CL Clear 1 Clears an input value before pressing the ENT key e g for canceling a wr...

Page 276: ...tion of error condition d Indication of operating status 2 LAMP OFF IN The light source lamp is turned off in response to contact signal input 3 AUTO ZERO IN Auto zero operation is executed in response to contact signal input 4 PROCESSOR option Analog output for data processor integrator 1 Absorbance value at each time point 2 Stored spectral data Absorbance value is output 5 RECORDER option Analo...

Page 277: ... mirror HM1 One half beam passes through the flow cell and arrives at detector S The other half beam arrives at detector R The latter beam is used as a reference signal to compensate for variations in the light source The beams arriving at detectors S and R are converted into electrical signals and the S R value undergoes logarithmic conversion The result is output as an absorbance linear signal t...

Page 278: ...erted in the optical path within 601 to 900 nm in order to cut off the second order diffraction light About 2 wavelength Measurement Mode Aberration free concave grating G1 is reciprocated at a high speed between any 2 wavelength positions Signals at the two wavelengths after beam dispersion are detected alternately and data is processed at each wavelength 2 6 ...

Page 279: ...2 W mode 190 to 600 nm D2 mode 380 to 900 nm W mode b 2 wavelength measurement 2 wavelengths in wavelength regions 190 to 350 nm 351 to 400 nm 401 to 600 nm and 601 to 900 nm D2 W mode 2 wavelengths in wavelength regions 190 to 350 nm and 351 to 600 nm D2 mode 2 wavelengths in wavelength regions 380 to 600 nm and 601 to 900 nm W mode Minimum wavelength interval 5 nm max wavelength interval 160 nm ...

Page 280: ...t temperature time constant 2 0 sec 9 Auto zero Zero adjusting range 0 2 to 2 AU 10 Offset 0 to 2 AU settable in 0 001 steps 11 Flow cell Quartz SUS Fluororesin optical path length 10 mm cell capacity 13 μL 12 Withstand pressure of flow cell 1 0 MPa 13 Controllable flow cell temperature option 40 C environmental temperature range 4 to 30 C 14 Time program No of programs 9 Settable time Up to 600 m...

Page 281: ...ored contents Absorption spectrum energy spectrum b No of storable spectra Absorption energy spectrum 3 Background spectrum 1 17 GLP related function a Switching time and lighting time D2 lamp W lamp Hg lamp b Key lock c D2 lamp energy check and D2 lamp wavelength check d W lamp energy check e Hg lamp wavelength check 18 Communication function e Line 19 Wavelength setting method Setting by communi...

Page 282: ...25 0 5 1 or 2 AU output as 1 V according to setting 23 Recorder output option 10 mV full scale Full scale range 0 001 to 2 500 AU settable in 0 001 steps 24 Other function Liquid leak detection 25 Operating temperature range 4 to 35 C condensation unallowable 26 Operating humidity range 25 to 85 condensation unallowable 27 Power supply 24 V DC 28 Power consumption 85 VA 29 Dimensions 340 W 440 D 1...

Page 283: ... long hour operation If you keep working with the display monitor and keyboard for long hours your eyes and body will be fatigued to jeopardize your health When working with the display monitor for a long time take a break for 10 to 15 minutes per hour for the health of your eyes and body 3 1 Basic Operations 3 1 1 Turning on Power Supply Turn on the power switch of this detector Power switch Liqu...

Page 284: ...a few seconds the next screen appears and self diagnostic test initialization is carried out WL DRIVE LAMP INITIALIZING When initialization has been normally terminated the next screen or monitor screen appears NOTE If the monitor screen does not appear on the LCD of UI pad beyond 3 minutes after turning on power supply or if an error message appears on the LCD refer to 4 5 Troubleshooting or 4 6 ...

Page 285: ...s the lit or extinguished status of each lamp Display changeover D2 W D2 lit W lit or D2 D2 lit W extinguished W D2 extinguished W lit OFF D2 extinguished W extinguished c Possible status indications are as follows Initialize status I Run time program operating status R Busy status B Key locked status L Monitor screen 2 energy indication WL SAMP REF CELL I 250 191000 202000 ON Wave length Sample e...

Page 286: ... busy status and L for the key locked status Monitor screen 2 energy indication Display changeover or 220 211000 292000 280 121000 144000 Sample energy at wavelength 2 Reference energy at wavelength 2 Wave length 2 Reference energy at wavelength 1 Sample energy at wavelength 1 Wave length 1 WL1 SAMP REF WL2 SAMP REF Monitor Screen Changeover Timing in 2 wavelength Measurement The monitor screen in...

Page 287: ... accordance with measuring conditions reference about 30 minutes 3 1 2 Parameter Input Method 1 Display Contents of Screen Explained here are display contents of the parameter input screen and program setup screen a Input of a single numeral PROGRAM NO 1 9 1 Parameter name Input range Input part b Input of plural numerals LAMP CHANGE MM DD YYYY 1 12 _ Parameter name Input item Input range Input pa...

Page 288: ...e cursor is returned to the head of character input part with the input numeral indicated thus awaiting reentry Pressing the ESC key calls back the initial screen monitor screen If the ESC key is pressed during the course of numerical input the parameter whose input is yet to be completed will not be updated previously set value remains set NOTE In item selection processing the default item select...

Page 289: ...ms before pressing the ESC key will be accepted 2 For canceling the set conditions use the ESC key The first monitor screen appears to allow re setting 3 When you don t want to change or input a setting advance to the next screen by the ENT or key display can be advanced and reversed by the and keys 4 When the time program is not used spectrum output is allowed at any time Therefore if spectrum ou...

Page 290: ...message appears PRESS CL KEY TO CLEAR MESSAGE A Z OVER RANGE NOTE Auto zero function is unusable during 2 wavelength measurement 3 1 4 Setting of Measuring Wavelength A measuring wavelength is settable WL Wavelength The measuring wavelength setting screen appears 250 D2 MODE 190 600 W MODE 380 900 WAVELENGTH 190 900 nm Press numerical keys within 1 9 0 to 9 0 0 and then the ENT key Settable wavele...

Page 291: ...ory Therefore when turning on power supply again the set conditions before turning off power supply are called out to allow measurement under the conditions 3 1 6 Washing after Use After using a buffer solution be sure to wash the flow cell with distilled water If this washing step is neglected salt will precipitate so that the flow cell might be clogged and damaged 3 9 ...

Page 292: ...rogram 4 POLARITY Select either polarity 5 OTHERS Other setting than above 3 2 1 Setting the Offset The offset is a set input signal value that is added to the actually measured value for output SET UP 1 Press key UTLTY 2 The utility setup screen appears Utility Setup Screen 1 USE PROG 3 POLARITY 4 OTHERS 5 UTILITY OFFSET 1 TIME CONSTANT 2 Select OFFSET Press numerical key 1 and then the ENT key 3...

Page 293: ...gram peaks Fig 3 2 a In this case the offset function adjusts the baseline which is shifted to the negative side to a signal level within the input range of the data processor Fig 3 2 b b Offset Used a Offset Not Used 10 corresponding to 10 mV Fig 3 2 Example of Offset Usage 4 Upon completion of offset setting the first monitor screen reappears Although the input numeral is not indicated at ABS wi...

Page 294: ... 5 UTILITY OFFSET 1 TIME CONSTANT 2 Select TIME CONSTANT Press numerical key 2 and then the ENT key 3 The time constant setup screen appears Time Constant Setup Screen 6 0 5s 5 1 0s 6 2 0s 7 TIME CONSTANT 0 01s 1 0 02s 2 0 05s 3 0 1s 4 Set a time constant Press numerical key within 1 to 7 and then the ENT key Default value 6 4 Upon completion of time constant setting the first monitor screen reapp...

Page 295: ... key 3 and then the ENT key 3 The time program setup screen appears Time Program Setup Screen 1 USE TIME PROGRAM YES 1 NO 0 Set use 1 or non use 0 of the time program Press numerical key 1 or 0 and then the ENT key 1 Time program starts in response to start input 0 Time program does not start irrespective of start input Default value 1 4 Upon completion of time program selection or avoidance the f...

Page 296: ...STANT 2 Select POLARITY Press numerical key 4 and then the ENT key 3 The polarity setup screen appears Polarity Setup Screen 1 POLARITY POSITIVE 1 NEGATIVE 2 Press numerical key 1 or 2 Usually input 1 and then the ENT key Default value 1 4 Upon completion of polarity setting the first monitor screen reappears When NEGATIVE is selected absorbance value becomes negative and ABS appears on the monito...

Page 297: ...cell to be used a Setting the Full Scale of Processor Output SET UP 1 Press key UTLTY 2 The utility setup screen appears Utility Setup Screen 1 USE PROG 3 POLARITY 4 OTHERS 5 UTILITY OFFSET 1 TIME CONSTANT 2 Select OTHERS Press numerical key 5 and then the ENT key 3 The OTHERS setup screen appears 1 LEAK SENSOR 3 LAMP 4 GAIN 5 OTHERS PROCESSOR 1 ERROR OUT 2 Select PROCESSOR Press numerical key 1 a...

Page 298: ...een 1 USE PROG 3 POLARITY 4 OTHERS 5 UTILITY OFFSET 1 TIME CONSTANT 2 Select OTHERS Press numerical key 5 and then the ENT key 3 The OTHERS setup screen appears 1 LEAK SENSOR 3 LAMP 4 GAIN 5 OTHERS PROCESSOR 1 ERROR OUT 2 Select ERROR OUT Press numerical key 2 and then the ENT key 4 The ERROR OUT setup screen appears 1 ERROR OUT SIGNAL DISABLE 0 ENABLE 1 Set the ENABLE or DISABLE status of ERROR O...

Page 299: ...E CONSTANT 2 1 USE PROG 3 POLARITY 4 OTHERS 5 Select LEAK SENSOR Press numerical key 3 and then the ENT key 4 The LEAK SENSOR setup screen appears 1 LEAK SENSOR OFF 0 ON 1 Set the use ON or non use OFF status of LEAK SENSOR Press numerical key 1 or 0 and then the ENT key Default value 1 5 Upon completion of LEAK SENSOR setting the first monitor screen reappears NOTE If power supply is turned off w...

Page 300: ...D2 1 W 2 D2 W 3 1 OTHERS PROCESSOR 1 ERROR OUT 2 1 LEAK SENSOR 3 LAMP 4 GAIN 5 UTILITY OFFSET 1 TIME CONSTANT 2 1 USE PROG 3 POLARITY 4 OTHERS 5 Set the ON or OFF status of each lamp Press numerical key within 0 to 3 and then the ENT key Default value 3 For selection of D2 lamp Press numerical key 1 and then the ENT key For selection of W lamp Press numerical key 2 and then the ENT key For selecti...

Page 301: ...USE PROG 3 POLARITY 4 OTHERS 5 Select OTHERS Press numerical key 5 and then the ENT key 3 The OTHERS setup screen appears OTHERS PROCESSOR 1 ERROR OUT 2 1 LEAK SENSOR 3 LAMP 4 GAIN 5 Select GAIN Press numerical key 3 and then the ENT key 4 The GAIN setup screen appears GAIN NORMAL 0 MICRO 1 0 Set the NORMAL or MICRO status of GAIN Press numerical key 0 or 1 and then the ENT key Default value 1 5 U...

Page 302: ... may reach the upper limit of measurement or A Z OVER RANGE may be caused when auto zero is executed For a wavelength where light quantity is large or when a difference in light quantity is large between sample and reference sides you should set NORMAL for GAIN 3 20 ...

Page 303: ... screen GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 Input Numeral Function 1 LOGBOOK Displays and resets the logbook of each lamp 2 KEY LOCK Disables acceptance of keyboard operation 3 D2 CHECK Checks energy of the D2 lamp at 250 nm and wavelength accuracy using the bright lines at 486 and 656 nm of this lamp 4 W CHECK Checks energy of the W lamp at 600 nm 5 Hg CHECK Checks waveleng...

Page 304: ...he GLP setup screen appears GLP Setup Screen GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 Select LOGBOOK Press numerical key 1 and then the ENT key 3 The lamp selection screen appears LAMP SELECT D2 1 W 2 Hg 3 1 For selection of D2 lamp Press numerical key 1 and then the ENT key For selection of W lamp Press numerical key 2 and then the ENT key For selection of Hg lamp Press numerica...

Page 305: ...ogbook Hg LAMP SWITCHING LAST CHANGED DATE 123 h 23 times 2 25 2010 b Resetting of D2 W Hg Lamp Logbook at Lamp Exchange The cumulative lamp on time referential lifetime lamp on count and lamp exchange date can be displayed for each of D2 W and Hg lamps 1 Press key GLP 2 The GLP setup screen appears GLP Setup Screen GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 Select LOGBOOK Press nu...

Page 306: ...ESET Press numerical key 2 and then the ENT key NOTE For logbook resetting input a numeral for YYYY followed by pressing the ENT key Even when the same year as desired is indicated be sure to input the same value again For resetting of D2 lamp D2 LAMP CHANGE MM DD YYYY 1 12 _9 15 2010 Press numerical month key 1 to 1 2 and then the ENT key Press numerical day key 1 to 3 1 and then the ENT key Pres...

Page 307: ...y Press numerical year keys 2 0 0 0 to 2 1 0 0 and then the ENT key For resetting of Hg lamp Hg LAMP CHANGE MM DD YYYY 1 12 _9 15 2010 Press numerical month key 1 to 1 2 and then the ENT key Press numerical day key 1 to 3 1 and then the ENT key Press numerical year keys 2 0 0 0 to 2 1 0 0 and then the ENT key 3 25 ...

Page 308: ...etup screen appears GLP Setup Screen Select KEY LOCK Press numerical key 2 and then the ENT key 3 The KEY LOCK setup screen appears GLP KEY LOCK YES 1 NO 0 0 GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 For validating keyboard operation Press numerical key 0 and then the ENT key For invalidating keyboard operation Press numerical key 1 and then the ENT key Key lock is released in the...

Page 309: ...lay is presented CHECKING LAMP ENERGY AND WL ACCURACY D2 4 After check its results are indicated D2 ENERGY ACCURACY 486 nm 656 nm 192000 GOOD 0 nm GOOD 1 nm An indicated energy value corresponds to the reference side at 250 nm Wavelength accuracy is checked utilizing the bright lines of the D2 lamp at 486 and 656 nm When deviation is within 1 nm GOOD will be indicated If deviation exceeds 1 nm FAI...

Page 310: ...P Setup Screen GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 Select W CHECK Press numerical key 4 and then the ENT key 3 Checking action will automatically be taken During check the following display is presented CHECKING LAMP ENERGY W 4 After this check its result is indicated W ENERGY 405775 The indicated energy value corresponds to the reference side at 600 nm 3 28 ...

Page 311: ...Y Hg GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 4 After this check its result is indicated ACCURACY 254 nm GOOD 1nm Wavelength accuracy is checked utilizing the bright line of the mercury lamp at 254 nm When deviation is within 1 nm GOOD will be indicated If deviation exceeds 1 nm FAIL will be indicated When no bright line has been detected NOT DETECTED is indicated In this case co...

Page 312: ...th D2 lamp in memory 4 W REF ENERGY Stores the reference side energy spectrum with W lamp in memory 5 Hg Stores the energy spectrum of mercury lamp a Storing the Spectral Data in Memory 1 key followed by ENT key Set the minimum wavelength of scan range 5 SPECT Spectrum SPECTRUM MODE ABS 1 BACK GROUND 2 1 D2 REF 3 W REF 4 Hg 5 SCANNING WL RANGE WL1 WL2 nm ABS 200 850 200 600 Press numerical keys wi...

Page 313: ... spectral data storage the monitor screen automatically appears NOTE The stored spectral data is a value after automatic subtraction of the background spectrum Therefore before spectrum measurement correct background spectrum should be stored in memory If acquisition of spectral data has been attempted without acquisition of background spectrum the following screen appears 250 600 200 600 MEMORIZE...

Page 314: ...ollowed by ENT key Set the minimum wavelength of scan range Press numerical keys within 2 0 0 to 8 5 0 and then the ENT key Enterable range 200 to 850 nm enterable in 1 nm steps Set the maximum wavelength of scan range Press numerical keys within 2 5 0 to 9 0 0 and then the ENT key Enterable range Minimum scan range is 50 nm Measuring span is max 400 nm Input the number of spectral data WL nm SCAN...

Page 315: ...gth of scan range SCANNING WL RANGE WL1 WL2 nm W REF 200 850 200 600 Press numerical keys within 2 0 0 to 8 5 0 and then the ENT key Enterable range 200 to 850 nm enterable in 1 nm steps Set the maximum wavelength of scan range SCANNING WL RANGE WL1 WL2 nm W REF 250 600 200 600 Press numerical keys within 2 5 0 to 9 0 0 and then the ENT key Enterable range Minimum scan range is 50 nm Measuring spa...

Page 316: ...matically selected during spectrum scan Set the minimum wavelength of scan range SCANNING WL RANGE WL1 WL2 nm Hg Press numerical keys within 2 0 0 to 8 5 0 and then the ENT key Enterable range 200 to 850 nm enterable in 1 nm steps Set the maximum wavelength of scan range 200 850 200 600 SCANNING WL RANGE WL1 WL2 nm Hg Press numerical keys within 2 5 0 to 9 0 0 and then the ENT key Enterable range ...

Page 317: ...erical key within 1 to 3 and then the ENT key During spectrum acquisition the following screen is presented WL nm SCANNING SPECTRUM NO 1 MODE Hg After spectrum acquisition the monitor screen automatically appears 3 35 ...

Page 318: ...he Full Scale Range of Recorder 1 key followed by ENT key Press numerical keys within 0 0 0 1 to 2 5 0 0 and then the ENT key Enterable range 0 001 to 2 500 AU enterable in 0 001 AU steps b Setting the Spectrum Output Speed of Recorder 2 key followed by ENT key 1 SPECT RCD 3 RCD RANGE 0 001 2 500 AU FS 2 500 RCD SPEED 40 nm min 1 60 nm min 2 1 RECORD RCD RANGE 1 RCD SPEED 2 For 40 nm min Press num...

Page 319: ...ted In the REF data mode The output wait screen appears When the spectrum has been acquired with the W lamp W REF is indicated When the spectrum has been acquired with the Hg lamp Hg is indicated Press the START key During spectrum output the following screen is presented 1 RCD NO SPEED WL RANGE MODE ABS 1 60 200 600 PRESS START RCD NO WL ABS SPEED 1 250 0 0000 60 RCD NO SPEED WL RANGE MODE D2 REF...

Page 320: ...ess numerical key within 1 to 9 and then the ENT key Next input the number of the program to be created or modified Pressing the ESC key returns display to the monitor screen without modifying the setting The mode selection screen appears Input Numeral Function 0 MODIFY Adds or modifies the stored time program 1 NEW Deletes the stored time program and creates a new time program Setting of each Ste...

Page 321: ...ange 190 to 900 nm enterable in steps of 1 nm Upon pressing the ENT key the cursor moves to BASE c Baseline Processing Press numerical key 1 or 2 and then the ENT key Input Numeral Function 1 A Z Auto zero will be executed 2 HOLD Baseline will not deviate Pressing the ENT key displays the next step Function of other keys during time program editing 1 clear Clears an input numeral 2 delete Deletes ...

Page 322: ...eing updated 3 4 6 Stop of Time Program 8 STOP Stop The time program stops and display returns to the monitor screen TIME WL ABS PROG LAMP I 0 0 250 0 0000 1 D2 W 3 4 7 Example of Time Program Operation An example of time program operation is described here a Setting of Time Program Auto zero Hold START STOP Time minute WL nm Fig 3 3 Time Program and Measuring Wavelength 0 0 20 0 10 0 250 270 A Z ...

Page 323: ... time program ends Press key Press numerical key 1 and then the ENT key Press numerical key 1 and then the ENT key Press numerical key 0 and then the ENT key Press numerical keys 2 5 0 and then the ENT key Press numerical key 1 Press the ENT key Press numerical keys 1 0 and then the ENT key Press numerical keys 2 7 0 and then the ENT key Press numerical key 2 Continued PROG SET PROGRAM NO 1 9 0 TI...

Page 324: ... this key to display the time program setup screen Input the number of the program to be checked by pressing numerical key within 1 to 9 and then the ENT key Press numerical key 0 and then the ENT key Continued PROG SET PROGRAM NO 1 9 1 EDIT MODE MODIFY 0 NEW 1 0 1 TIME WL BASE A Z 1 HOLD 2 10 0 270 2 1 TIME WL BASE A Z 1 HOLD 2 _ 1 TIME WL BASE A Z 1 HOLD 2 20 0 270 1 0 0 250 0 0000 1 D2 W TIME W...

Page 325: ...BASE A Z 1 HOLD 2 _ 0 0 250 1 1 TIME WL ABS PROG LAMP I 0 0 250 0 0000 1 D2 W When the time program ends measurement is automatically terminated and the monitor screen appears At this time the wavelength is the one indicated on the monitor screen before execution of the time program NOTE At WL it is recommended to set the same wavelength as at 0 0 minute or leave the wavelength on the first line o...

Page 326: ...ection screen appears POWER UTLTY SET UP Setup SETUP DETECTOR THERMO CONTRAST S NO CH1 NO USE 4 1401 001 SETUP ITEMS DETECTOR 1 THERMO CELL 2 1 CONTRAST 3 Input Numeral Function 1 DETECTOR Used for setting a communication channel 2 THERMO CELL Used for setting use or non use of the thermostatic flow cell 3 CONTRAST Used for setting an LCD contrast level 3 44 ...

Page 327: ...y 1 and then the ENT key For selecting channel 1 Press numerical key 1 and then the ENT key For selecting channel 2 Press numerical key 2 and then the ENT key New setting is accepted after turning on power supply again UTLTY SET UP POWER SETUP DETECTOR THERMO CONTRAST S NO CH1 NO USE 4 1401 001 SETUP ITEMS DETECTOR 1 THERMO CELL 2 1 CONTRAST 3 DETECTOR CH1 1 CH2 2 1 3 45 ...

Page 328: ...al key 0 and then the ENT key For selecting use of thermostatic flow cell Press numerical key 1 and then the ENT key After setting use or non use of the thermostatic flow cell ON or OFF is indicated on the monitor screen 2 WL SAMP REF CELL I 250 301000 492000 ON When the thermostatic flow cell is not yet connected will be indicated on the monitor screen 2 WL SAMP REF CELL I 250 301000 492000 New s...

Page 329: ...NO CH1 NO USE 4 1401 001 Press the ENT key The selection screen appears SETUP ITEMS DETECTOR 1 THERMO CELL 2 1 CONTRAST 3 Press numerical key 3 and then the ENT key LCD CONTRAST 1 7 4 Press numerical key within 1 to 7 and then the ENT key For lowest contrast 1 For highest contrast 7 New setting is accepted after turning on power supply again 3 47 ...

Page 330: ...t once Leakage of solvent or waste solution Leakage of solvent inside the instrument Beware of an ignition hazard due to static electricity when using flammable chemicals To prevent a build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of vapor from flammable chemicals If a flammable chemical such as organic s...

Page 331: ... 3 6 1 Precautions on Selection and Handling of Mobile Phase 1 Pay enough attention to the characteristics of the mobile phase to be used and a restriction on its operating temperature Refer to the organic solvent characteristics in Table 3 2 2 For high sensitivity analysis with the UV detector use a solvent which is particularly low in UV absorption characteristic A commercially available solvent...

Page 332: ...tion column etc are made of stainless steel SUS 316 Therefore use of the solvents and reagents which can corrode this material may be somewhat restricted The typical example of such reagents are solvents and solutions containing halogen ions of HCl KCl NaCl NH4Cl etc The reagents whose use may be restricted are listed in Table 3 1 Utilize it as a referential table NOTE If an undesirable but indisp...

Page 333: ...the mobile phase may not be sucked in the early stage after pump start In this case aspirate the mobile phase into the furnished syringe and discharge the mobile phase from the suction valve to the discharge valve side Discharge valve Suction valve Syringe Fig 3 4 Pump Front 3 51 ...

Page 334: ... acid up to pH3 Hydrochloric acid up to pH3 Potassium nitrate Sodium hydrogen carbonate Sodium carbonate Ammonium chloride Potassium chloride Sodium chloride Trifluoroacetic acid Note 1 Maximum concentration of the above reagents should be limited to 5 6 Note 2 If the above reagents were used unavoidably be sure to wash the entire flow path adequately with distilled water Other reagents which can ...

Page 335: ... if an abnormality is found stop operation at once Leakage of solvent or waste solution Leakage of solvent inside the instrument Beware of an ignition hazard due to static electricity when using flammable chemicals To prevent a build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of vapor from flammable chemica...

Page 336: ...or injury For details of the properties of each solvent and how to handle it refer to Material Safety Data Sheet MSDS Be sure to handle each solvent properly a Wear proper protective means e g safety goggles so that a solvent will not come into direct contact with the skin eye etc b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor 3 54 ...

Page 337: ...5 1 501 1 424 1 353 1 442 1 443 1 424 1 394 1 408 1 445 1 381 1 400 1 359 1 422 1 370 1 362 1 410 1 586 1 387 1 394 1 344 1 510 1 38 1 361 1 329 1 427 1 372 1 333 210 210 210 210 210 210 210 380 265 225 220 290 220 225 285 225 280 220 290 245 245 330 220 230 330 380 220 260 260 210 275 380 210 305 220 210 210 210 210 40 21 7 46 1 20 17 8 30 12 8 9 4 o 17 2 m 25 p 25 27 8 32 2 4 4 17 8 32 2 11 1 45...

Page 338: ...obile phase For mobile phase use a solvent having a boiling point of 55 C or higher Use of a low boiling point is not only dangerous but also gives rise to air bubbles during suction by the pump which may disable the pump from delivering liquid normally 3 For high sensitivity analysis with the UV detector use a solvent which absorbs minimum UV Generally used high grade reagents such as methanol an...

Page 339: ...for waste solution in order to prevent a build up of static electricity b Do not bring a flame source near the instrument In a high performance liquid chromatograph flammable organic solvents are often used Therefore adequate attention should be paid to a heat or flame source Static electricity is built up in a liquid chromatograph because thin tubes are used If discharge occurs due to accumulatio...

Page 340: ...f used at a high pressure 1 deterioration of mobile phase sample 2 fall in column efficiency due to bubbles 3 increase in detector noise due to bubbles 4 fluctuations of pump pressure and 5 degradation of gradient mixing ratio accuracy 2 The mobile phase can be degassed with a degassing unit or manually Degassing method is explained in 3 7 2 3 Be sure to use the mobile phase which does not contain...

Page 341: ...nic washer a In an ultrasonic washer place a mobile phase container after adequate stirring see below For using a mixed mobile phase complete mixing by means of a stirrer is required Otherwise poor reproducibility or baseline drift will be caused NOTE The mobile phase of an organic solvent must always be degassed with an ultrasonic washer containing water b Turn ON the power switch of the ultrason...

Page 342: ...sure to fill the bath with water 2 Aspirator having a rubber plug which matches the mouth of the mobile phase container to be used Match rubber plug with container Mobile phase container Ultrasonic washer Aspirator a In an ultrasonic washer place the mobile phase container after adequate stirring see below For using a mixed mobile phase complete mixing by means of a stirrer is required Otherwise p...

Page 343: ...bbles are discharged remove the rubber tube of aspirator from the mobile phase container g Close the tap water spigot h Turn OFF the power switch of the ultrasonic washer i Take out the mobile phase container from the ultrasonic washer and wipe off moisture adequately Then set the container in a liquid chromatograph NOTE Discharge of bubbles varies with the composition of mobile phase In case of a...

Page 344: ...your analytical purpose 1 Example of Mobile Phase Filtration with Membrane Filter Decontamination and degassing can be achieved simultaneously by passing the mobile phase through a 0 45 μm membrane filter Membrane filter NOTE Remove dust from the mobile phase using a 0 45 μm membrane filter Avoid using filter paper because it will become a source of dust generation 3 62 ...

Page 345: ... removed efficiently by this method NOTE There are various sample filtration methods Select a method suitable for the volume of your sample Filtration with 0 45 μm membrane filter of cartridge type Clean sample after filtration b Example of inclusion removal from sample In analysis with a reversed phase column such as ODS column for example take a sample into a syringe and filtrate it with a norma...

Page 346: ...repare the instrument as instructed in Appendix 1 2 Turn on the power switch of this detector 3 Confirm that measuring conditions time constant output range etc can be set normally WL 4 Confirm wavelength operation using key A Z 5 Confirm auto zero action using key 4 1 ...

Page 347: ...mps due to their characteristics 2 Measurement of Wavelength Accuracy See 4 4 1 Check wavelength accuracy using the bright lines of D2 lamp at 486 and 656 nm and the bright line of Hg lamp at 254 nm Specification Wavelength accuracy of each bright line shall be within 1 nm 3 Measurement of Baseline Conditions Room temperature constant air in flow cell time constant 2 0 s Noise in data sampling per...

Page 348: ...ne For this measurement the following devices should be prepared Recorder or Model D 2500 chromato integrator Vernier caliper max measurable length 200 mm or more minimum readable value 0 1 mm or less NOTE When the inside of flow cell is wetted with liquid baseline noise and drift may increase To prevent this wash the flow cell with an organic solvent such as methanol and then conduct purging adeq...

Page 349: ...s 2 5 0 and then the ENT key 2 Carry out auto zero A Z Press key 0 0 250 0 0000 1 D2 TIME WL ABS PROG LAMP I 3 Start the chromato integrator and record the baseline for 15 minutes 4 From the recorded chart figure out noise value according to ASTM1657 98 JAIMAS 0005 2008 Y2 Y3 Y1 15 minutes CENTER X2 X3 X1 Noise value Xn is given in steps of 30 seconds R n YR n R l Excerpt from JAIMAS 0005 2008 4 4...

Page 350: ... cell with an organic solvent such as methanol and then conduct purging adequately using nitrogen gas While an organic solvent such as methanol or acetonitrile is delivered through the cell the baseline noise and drift may be reduced Conditions Wavelength 250 nm Time constant response 2 sec Sampling period of chromato integrator 1600 ms Measurement time 1 hour Warm up 1 hour 1 After turning on pow...

Page 351: ...rmance Specifications 3 Start the chromato integrator and record the baseline for 1 hour 4 From the recorded chart figure out drift value according to ASTM1657 98 JAIMAS 0005 2008 Drift value D Excerpt from JAIMAS 0005 2008 4 6 ...

Page 352: ... 1 Leak Sensor Mounting Position NOTE When using the liquid leak sensor follow the instructions given below a Before using a solvent the leak sensor function should be activated b The leak sensor function of this detector may fail to work for leak in a very small amount The function may also fail to work for a solvent having a high volatility Always check for liquid leak so as to circumvent a seri...

Page 353: ...nsor and drain tray Then fasten the leak sensor to the drain tray again NOTE When washing the leak sensor be careful not to damage the leak sensor tip If damaged the leak sensor may not work normally or an error may occur Leak sensor fastening screw Fig 4 2 Leak Sensor Fastening Screw NOTE Mount the leak sensor at the correct position If the mounting position is inappropriate or the leak sensor is...

Page 354: ...the leak sensor to malfunction 2 Lighting of lamp Every day Check that the D2 LAMP LED is lit 3 Check for absorbance Every day Activate the auto zero function and check if ABS indication becomes zero 4 Life of light source lamp Every month 1 Judge whether the lamp has reached the end of its service life by checking for poor energy and for arrival at the maximum allowable total ON time 2 Judge whet...

Page 355: ...ion exceeds 1 nm FAIL will be indicated When no bright lines have been detected NOT DETECTED is indicated In this case confirm mounting of the flow cell and then turn on power supply again If the situation does not improve contact the nearest maintenance service company authorized by Hitachi High Technologies NOTE When the D2 ENERGY level has fallen to 50 or lower of the level at the start of lamp...

Page 356: ...Lamp 1 D2 Lamp The cumulative ON period number of ON times and replacement date of the D2 lamp can be checked by the GLP function Press 1 ENT 1 ENT 1 and ENT keys in this order GLP The following screen appears D2 LAMP SWITCHING LAST CHANGED DATE 123 h 23 times 2 25 2010 The cumulative ON period number of ON times and the input date of replacement month day year are indicated at D2 LAMP SWITCHING a...

Page 357: ...ollowing conditions and if an abnormality is found stop operation at once Leakage of solvent or waste solution Leakage of solvent inside the instrument Beware of an ignition hazard due to static electricity when using flammable chemicals To prevent a build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of vapor...

Page 358: ...vent properly a Wear proper protective means e g safety goggles so that a solvent will not come into direct contact with the skin eye etc b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor If there is contamination inside the flow cell cleaning is required Items to be prepared for flow cell cleaning Injector made of glass having a capacity of about...

Page 359: ...ning is required Detergent to be used varies with the mobile phase which has been used When the mobile phase used is aqueous deliver distilled water with the pump at flow rate 1 0 mL min and pressure 1 0 MPa or lower at first for cleaning and deliver ethanol acetone etc when the mobile phase used is an organic solvent CAUTION If the flow cell is pressurized excessively it may be broken Be sure to ...

Page 360: ... or waste solution Leakage of solvent inside the instrument Beware of an ignition hazard due to static electricity when using flammable chemicals To prevent a build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of vapor from flammable chemicals If a flammable chemical such as organic solvent leaks from the flo...

Page 361: ...perly a Wear proper protective means e g safety goggles so that a solvent will not come into direct contact with the skin eye etc b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor If contamination still remains on the flow path despite the above mentioned cleaning disassemble the flow cell and then clean the components as instructed below 1 Remove...

Page 362: ...1 4 inch Liquid leaking hole Fastening screw M3 Sleeve 638 1099 Fig 4 5 Disassembly of Flow Cell Main Frame 3 Wash all the parts of flow cell with an ultrasonic washer 4 Wipe off contaminants from the surface of the flow cell with gauze soaked in acetone or ethanol 5 After washing assemble the parts in reverse to the disassembly referring to the disassembling diagram The pressure withstanding cell...

Page 363: ...this time tighten the window supports further about 5 Clamp screws 1 and 2 should be tightened manually as far as possible and then further tighten about 120 with a double ended wrench bolt diameter 1 4 inch The cell lid pressure withstanding cell and cell receptacle have holes for liquid leaking After assembling be sure to confirm that those holes are positioned at the bottom NOTE The flow cell w...

Page 364: ...I D 1 m Teflon tube or the like should be added For details contact the nearest maintenance service company authorized by Hitachi High Technologies 4 Impurities are contained in solvent Check the solvent Purify or replace the solvent Check for regularity in occurrence 5 Trouble has occurred on pump Check for noise at pump stop Make sure the pump is normal 3 Noise is too large 6 D2 lamp has reached...

Page 365: ...edy 1 Liquid has leaked Visual check Wipe off the liquid that has leaked in drain receiver Wipe off the liquid that has adhered to leak sensor 5 Leak error occurs 2 Contaminant has stuck to leak sensor Visual check Wipe off contaminant from the leak sensor 4 20 ...

Page 366: ...ey 2 Confirm proper mounting of the flow cell and then turn on power supply again 3 Contact the maintenance service company authorized by Hitachi High Technologies WL MOTOR DRIVE DRIVER ERROR Motor driver for wavelength is faulty 1 Turn on power supply again 2 Contact the maintenance service company authorized by Hitachi High Technologies WL CALIBRATION ERROR PRESS CL KEY TO CLEAR MESSAGE The 656 ...

Page 367: ...FER OVERFLOW PRESS CL KEY TO CLEAR MESSAGE During data acquisition data transmission to interface board has become impossible and data buffer is overflowed 1 Clear the message by CL key 2 Confirm connection with the interface board Hg LAMP ERROR PRESS CL KEY TO CLEAR MESSAGE Hg lamp goes off though unintended or does not come on 1 Clear the message by CL key 2 Turn on power supply again 3 Renew th...

Page 368: ... 2 4 9600 hours 5 years Packing for cell window material PTFE 892 7012 Photocell circuit board 9600 hours 5 years 1 893 0821 Thermostatic inlet tube 9600 hours 5 years Length 458 mm Inner diameter 0 25 mm Outer diameter 1 57 mm Material SUS 893 0822 Standard inlet tube 9600 hours 5 years Length 458 mm Inner diameter 0 25 mm Outer diameter 1 57 mm Material SUS 893 0823 Drain tube 9600 hours 5 years...

Page 369: ... outlet and inlet tube For standard flow cell Length 350 mm Inner diameter 0 25 mm Outer diameter 1 57 mm Material SUS PTFE for coating M790019 Screw S SUS 9600 hours 5 years Example use Connecting pipe L329109 Ferrule SUS 9600 hours 5 years Example use Connecting pipe 1 Only the maintenance service company authorized by Hitachi High Technologies is allowed to replace this item 5 2 ...

Page 370: ...ust not be released intentionally Otherwise there is a risk of electric shock due to wrong operation CAUTION Burns due to hot temperature The lamp and lamp cover are hot during and immediately after use of the lamp There is a risk of burns due to contact with the hot lamp or its cover when replacing the lamp Before start of lamp replacement turn off the power switch and wait for half an hour or lo...

Page 371: ...owing The power switch of this instrument is turned off The power cord is unplugged from the instrument 3 How to Replace D2 Lamp a Detach the lamp cover by removing 2 fastening screws Fastening screw ｃ Lamp cover b Loosen three screws of D2 lamp lead wires connected on the terminal block and pull out the wires Fastening screw Terminal block Lead wire 5 4 ...

Page 372: ...revolutions with a blade edged screwdriver Fastening screw e Pull out the D2 lamp while turning it clockwise f Fit a new D2 lamp and turn it counterclockwise until there is no gap between the mounting hole and the fastening screw Then tighten the 3 fastening screws evenly in an alternate order with the blade edged screwdriver Good example Bad example No gap allowable D2 lamp Mounting hole Fastenin...

Page 373: ...d wires one by one through the cover holes Then attach the cover Cover Fastening screw h Connect the lead wires to the terminal block R terminal B1 terminal B2 terminal i Attach the lamp cover at the original position Fastening screw 5 6 ...

Page 374: ...acement and as a historical record of D2 lamp replacement Monitor Screen 2 250 191000 202000 ON WL SAMP REF CELL I 6 Enter the lamp replacement date as follows a Press key and the following screen will appear GLP 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 GLP LOGBOOK 1 KEY LOCK 2 b Press numerical key 1 and then the ENT key The following screen appears 1 LAMP SELECT D2 1 W 2 Hg 3 c Press numerical key 1 an...

Page 375: ... reset to 1 NOTE The logbook data is reset when the numeric value of the year and ENT are keyed in Therefore even if the same year as that of replacement is indicated the year must be numerically input followed by pressing the ENT key 5 2 2 Replacement of W Lamp 1 Part and Tool to be Prepared New W lamp Phillips screwdriver 2 Check the following The power switch of this instrument is turned off Th...

Page 376: ...or hook from the W lamp lead wire W lamp cover W lamp lead wire Connector hook Enlarged view Pull down while pressing c Remove two W lamp cover fastening screws and detach the W lamp cover Fastening screw 2 pcs W lamp cover 5 9 ...

Page 377: ...t the original position f Reconnect the connector hook of the W lamp lead wire g Attach the lamp cover at the original position by tightening 2 fastening screws 4 Operation Check Plug the power cord into the instrument and turn on the power switch Make sure the lamp comes on NOTE The W lamp does not come on if it has not been mounted properly 5 10 ...

Page 378: ... the ENT key The following screen appears 1 12 _9 15 2010 W LAMP CHANGE MM DD YYYY e Key in the date of replacement in the format of month day year For instance if the lamp is replaced on March 1 2010 key in the date as shown below 3 ENT 1 ENT 2 0 1 0 ENT Thus the date of lamp replacement is stored in memory At the same time the cumulative turn on time of the W lamp is cleared to zero 0 and the tu...

Page 379: ...er switch of this instrument is turned off The power cord is unplugged from the instrument 3 How to Replace Hg Lamp a Detach the lamp cover by removing 2 fastening screws and then separate the Hg lamp cover by removing 2 fastening screws b Remove the fastening screw Fastening screw Hg lamp cover Lamp cover Fastening screw Fastening screw 5 12 ...

Page 380: ... the lamp replacement date as follows a Press key and the following screen will appear GLP GLP LOGBOOK 1 KEY LOCK 2 1 D2 CHECK 3 W CHECK 4 Hg CHECK 5 b Press numerical key 1 and then the ENT key The following screen appears LAMP SELECT D2 1 W 2 Hg 3 1 c Press numerical key 3 and then the ENT key The following screen appears LOGBOOK REPORT 1 RESET 2 1 d Press numerical key 2 and then the ENT key Th...

Page 381: ...us the date of lamp replacement is stored in memory At the same time the cumulative turn on time of the Hg lamp is cleared to zero 0 and the turn on count is reset to 1 NOTE The logbook data is reset when the numeric value of the year and ENT are keyed in Therefore even if the same year as that of replacement is indicated the year must be numerically input followed by pressing the ENT key 5 14 ...

Page 382: ...lvents 3 53 Check against packing list APPENDIX1 8 Checking and cleaning of flow cell 4 12 Confirmation of basic actions 4 1 D D2 lamp 5 1 Degassing of mobile phase 3 59 Disassembling and cleaning of flow cell 4 15 Drift 4 5 E ENT 2 3 ESC 2 3 Energy of light source lamp 4 10 Error messages 4 21 e Line APPENDIX1 10 F Frequency APPENDIX1 3 G GLP 2 3 6 1 ...

Page 383: ...asurement of wavelength accuracy 4 10 Measuring wavelength 3 8 N Noise 2 8 O OFFSET 3 10 Operation 3 1 P POLARITY 3 10 PROCESSOR 2 4 PROG 2 1 Performance specification check 4 2 Place for installation APPENDIX1 1 Power capacity APPENDIX1 3 Power supply voltage APPENDIX1 3 R RECORDER 2 4 Rear panel 2 4 Replacement of D2 lamp 5 4 6 2 ...

Page 384: ... 5 1 S Sample treatment 3 63 Selection of mobile phase 3 49 Setting of time program 3 38 Shutdown 3 9 Specifications 2 6 T Time constant 3 10 Time program 3 13 Troubleshooting 4 19 Tubing 1 15 Turning on power supply 3 1 U UI PAD 2 2 UTLTY 3 10 Unpacking APPENDIX1 1 W W lamp 5 1 Wavelength accuracy 2 7 4 2 6 3 ...

Page 385: ...rer or its authorized service agent Before installation however the user shall make adequate preparations for installing the instrument referring to this instruction manual If relocation of the instrument becomes necessary after delivery consult your dealer or nearest Hitachi High Technologies service representative in order to avoid possible trouble involved in relocation 2 Place for Installation...

Page 386: ...hall be free from strong vibration or shock which can be felt by your body d Shall be free from a heating device such as gas burner electric heater or oven in the vicinity e Shall be away from strong electric field generating equipment such as electric welder high frequency electric furnace and pole transformer f Shall be free from excessive dust Otherwise performance degradation might be caused g...

Page 387: ...r Chromaster 5310 column oven and Chromaster 5410 5420 5430 5450 detector Confirm the necessary power capacity taking actual system configuration and OA equipment in the installation room into account and prepare a power supply having an adequate power capacity 4 Power outlet Power supply shall be obtainable near the place for installing the system inclusive of this detector This detector requires...

Page 388: ...of a different type of power cable may result in an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet as a rule b If a grounded 3P power outlet is not available use a 3P table tap with a grounding wire or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or larger and a turn count of...

Page 389: ... 5420 UV VIS detector Ground resistance 100 Ω or less 750 mm or more below ground Copper plate Organizer or AC adapter option Connector Rear panel Grounding electrode underground section 300 mm Grounding construction f 100 Ω or less or 2 mm 10 mm Example of grounding electrode Appended Fig 1 1 Grounding Method APPENDIX 1 5 ...

Page 390: ...ng construction for 100 Ω or less Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Chromaster 5420 UV VIS detector Connecto Organizer or AC adapter option r Rear panel 10 mm 2 mm 300 mm Power outlet with grounding terminal 2P 3P adapter Chromaster 5420 UV VIS detector Grounding terminal Organizer or AC adapter option Connector Grounding wire green Rear p...

Page 391: ...o that the clearance between the two blocks becomes 100 mm If the clearance between the blocks is wider than 100 mm the length of DC power cable may become inadequate For installation prepare a level and sturdy bench which withstands a load of 150 kg or more The system conceived here is an example in which Chromaster organizer Chromaster 5110 pump Chromaster 5210 autosampler Chromaster 5310 column...

Page 392: ... authorized service agent 5 1 Removal of Transport Screws 1 There are three screws for transport on the bottom panel of the detector 2 Remove the screw A for transport using a Phillips screwdriver 3 Remove the screw B for transport and set it at the position A 4 Remove the screw C for transport using a Phillips screwdriver 5 At the position C set the furnished screw M5 put in a bag stuck to the fr...

Page 393: ...riginal positions D A B C Appended Fig 1 3 Bottom Panel of Detector NOTE If the screws are not set at the positions A and C after transport baseline noise and baseline drift might increase D Appended Fig 1 4 Front Panel of Detector APPENDIX 1 9 ...

Page 394: ...nd Chromaster 5440 fluorescence detector the power cord needs to be connected to the column oven unit If a single organizer is inadequate due to use of 2 detectors for example an AC adapter option that matches the detector concerned needs to be used Connect the power cable from the organizer or AC adapter to the power connector at the rear left of the detector Power connector Detector rear panel s...

Page 395: ...le 1 P N 892 6909 attached to organizer Connector cable 2 P N 892 6910 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 4 P N 892 6912 attached to organizer AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster 5210 autosampler a...

Page 396: ...e Used Connector cable 1 P N 892 6909 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 5 P N 892 6914 separately available Connector cable 6 P N 892 6913 separately available AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster ...

Page 397: ...ure Gradient System Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump e Line cable 1 e Line cable 2 Appended Fig 1 8 e Line Cable Connection Appended Table 1 3 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosamp...

Page 398: ...Chromaster 5210 autosampler Interface control board e Line cable 1 e Line cable 2 Chromaster organizer Chromaster 5110 pump Appended Fig 1 9 e Line Cable Connection Appended Table 1 4 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampler fluorescence detector and interface control board APPENDIX 1 14 ...

Page 399: ...column and detector through the central hole of each module unit Drain receiver 1 Isocratic System Detergent Mobile phase liquid Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Chromaster 5110 pump Drain Injection valve Column Syringe valve Degassing unit Appended Fig 1 10 Tubing Diagram of Isocratic System stacked in o...

Page 400: ...m stacked in two blocks Connect the inlet tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the inlet of pump Connect the purge valve of pump to port 4 of the injection valve in the autosampler Connect port 5 of the injection valve to the inlet of column To the outlet of column connect the inlet tube of detector cell Connect the deterg...

Page 401: ...420 5430 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Low pressure gradient unit proportioning valve Chromaster 5110 pump Drain Degassing unit Syringe valve Injection valve Appended Fig 1 12 Tubing Diagram of Low Pressure Gradient System stacked in one block APPENDIX 1 17 ...

Page 402: ...et tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the IN port of proportioning valve Connect the OUT port of the proportioning valve in the low pressure gradient unit to the 4 way joint Then connect the purge valve of pump to port 4 of the injection valve in the autosampler Also connect port 5 of the injection valve to the inlet of ...

Page 403: ...for Drain when stacking module units in one block Appended Table 1 5 Drain Tubes to be Used Drain tube A2 P N 893 2874 attached to organizer Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 P N 893 2872 attached to organizer Drain tube 4 P N 893 2873 attached to organizer Drain tube P N 080 3090 attached to autosampler T joint P N 810 1362 attached to organizer T joint N1 P N 890 349...

Page 404: ...ng module units in two blocks Appended Table 1 6 Drain Tubes to be Used Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 1 2 P N 893 2872 attached to autosampler Drain tube A1 3 P N 893 2872 attached to organizer Drain tube 1 P N 080 3090 attached to autosampler Drain tube 2 P N 080 3090 separately available T joint P N 810 1362 attached to organizer T joint N1 P N 890 3493 attached ...

Page 405: ...vention of Instrument Tipover Personal injury could be incurred if the instrument tips over When installing the instrument provide a proper means for preventing the instrument from tipping over accidentally On the rear of each module unit a cabling cover is attached The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers Fastening plate Fastenin...

Page 406: ......

Page 407: ...t via 3 pin connector Their names and functions vary with the unit A name that indicates the function is given at each connector Example of output contact signal EVENT of pump Example of input contact signal LAMP OFF IN of detector 2 Contact Signals Entering e Line Connectors Each unit has two e Line connectors at the rear of the main frame and the respective signals of these connectors are connec...

Page 408: ... cable 890 6145 3 pin connector e DIO cable 890 6145 e Line connector To L 2000 series unit 2 Connection with D 2500 For connection use the e DIO cable 890 6146 START COM EXTERNAL H L BUSY BUSY START G L H e Line connector D 2500 To Chromaster series unit Connect the L and G terminals of the START line of e DIO cable 890 6146 to the EXTERNAL COM terminal of D 2500 APPENDIX 2 2 ...

Page 409: ...These are contact signal output terminals for control of an external unit using contact signals The output circuit is as shown in Appended Fig 2 4 The rating of contacts used is 12 V 0 1 A Make sure the load connected does not exceed this rating e Line cable Other unit Chromaster series unit A Chromaster series unit B Appended Fig 2 1 e Line Cable Connection Appended Fig 2 2 e Line Contact Circuit...

Page 410: ...er series Activated upon shorting contacts of external unit External unit Appended Fig 2 3 Contact Signal Input Circuit 30 V max 1 2 3 0 1 A max Chromaster series External unit Appended Fig 2 4 Contact Signal Output Circuit APPENDIX 2 4 ...

Page 411: ...ented at first upon starting the instrument Auto zero Adjusts signal level of the detector to zero thereby canceling a rise of the baseline Generally activated just before or after start AUTO ZERO IN A function for activating auto zero according to external contact signals Key lock A protective function for rejecting a key input made in error during instrument run Grating An optical device for dis...

Page 412: ... data processor Flow cell A sample container for measuring a sample continuously Photo cell circuit board An electronic circuit for detecting light and converting it into an electric signal MARKER IN A function for entering a marker on chromatogram according to an external contact signal LAMP OFF IN A function for turning off the light source lamp according to an external contact signal Lamp selec...

Page 413: ...tructions in this manual and the WARNING CAUTION labels on the instrument Keep this manual in a safe place nearby so it can be referred to whenever needed 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 3rd Edition June 2011 Copyright C Hitachi High Technologies Corporation 2011 1st Edition 2011 All rights reserved Printed in Japan Part No 892 9720 2 HH R FT HMS ...

Page 414: ... party in any form or by any means without the express written permission of Hitachi High Technologies Corporation 3 Hitachi High Technologies Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 415: ...ences adverse to safety Note that it is allowed only for persons having a basic knowledge of chemical analysis procedures to use this instrument Carefully read this instruction manual before attempting operation For proper use of the software please acquaint yourself with it The liquid chromatograph system comprises a pump unit for delivering mobile phases a sample introduction unit for injecting ...

Page 416: ...on 1 OVERVIEW Basic Operation Section 2 FUNCTIONS Name and Function of Each Part on FL detector Section 3 OPERATION Basic Operation Section 4 MAINTENANCE TROUBLESHOOTING Operational Check Section 5 SPARE PARTS Replacement Parts and Consumables Section 6 INDEX APPENDIX1INSTRATTION APPENDIX2DESCRIPTION ON CONTACT SIGNAL COMMUNICATION APPENDIX3GLOSSARY First of all read IMPORTANT and SAFETY SUMMARY a...

Page 417: ...e of Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be available in origina...

Page 418: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 419: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Technologies does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Technologies or its related companies or application of said instrument Installation Re...

Page 420: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 421: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 422: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 423: ...sible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power device Trademark Acknowledgments EmpowerTM are register...

Page 424: ...word NOTICE or NOTE is used to indicate precautionary instructions concerning possible property damage NOTICE Used to indicate a potentially hazardous situation which if not avoided will or can result in damage to user s property serious damage to the instrument damage to data or environmental pollution though personal injury may not be incurred NOTE Used to indicate explanatory information for en...

Page 425: ...tric shock or fire Radiation from the Laser Light Source WARNING The internal CD ROM or CD R W drive of the PC is provided with a laser beam source In normal operation of the PC containing the laser beam source no laser beam harmful to human health will be emitted outside Note however that if a laser beam leaking out of the PC accidentally gets into the eye eye injury could occur When using the PC...

Page 426: ...r waste solution Leakage of solvent inside the instrument Section 3 6 4 4 When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution employ and provide proper grounding connection to it Section 3 6 4 4 Explosion of Vapor from Flammable Chemicals If a flammable chemical such ...

Page 427: ...n an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet b If a grounded 3P power outlet is not available use a grounded 3P table tap or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 mm APPEN...

Page 428: ...non lamp 1 000 hours Section 3 5 At replacement Before removing the xenon lamp for replacement turn off the xenon lamp turn off power to the instrument and then wait for at least one hour until the xenon lamp becomes sufficiently cool to reduce its internal pressure the normal safety level Section 5 2 If a strong shock or impact is applied to the xenon lamp or if the surface of its quartz glass pa...

Page 429: ...excessively is used continuously pressure inside the lamp bulb may become too high causing possible explosion To prevent this replace the lamp with a new one immediately if its cathode has been consumed substantially Section 5 2 If the nut on the lamp base and wiring part is loose the contact resistance between them will increase due to poor contacting This could generate a large amount of heat to...

Page 430: ... is lit Be sure to wear tinted safety glasses to prevent possible eye damage Section 5 2 Heavy Instrument This instrument weight as much as 23 kg When carrying this instrument exercise care not to incur injury by dropping it accidentally Be sure to hold the right and left parts of the instrument securely when moving it Section 2 1 Prevention of Instrument Tipover Personal injury could be incurred ...

Page 431: ...tual parts Periodically check the appearances of these warning labels to see if they are clean to allow easy reading over a safe distance If any one of the warning labels becomes illegible due to deterioration contact your local Hitachi High Technologies Corporation sales representative or service office of Hitachi High Technologies Corporation sales representative for replacement with a new one 1...

Page 432: ...AUTION Labels on Instrument 2 Explosion of Vapor from Flammable Chemicals 3 Electric Shock due to Contact with Light Source Power Supply Front View 5 Explosion of Xenon 6 Burns due to Contact with Hot Part 4 Ignition of Flammable Chemicals ...

Page 433: ...SAFETY 10 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument 7 Before Turning on Xenon Lamp Front View ...

Page 434: ...Furthermore leakage of a highly volatile solvent may not be detected Be sure to check for liquid leakage regularly to prevent a possible serious accident regardless of whether the leak sensor is activated or not a In routine inspection of the instrument visually check for liquid leakage before attempting measurements b In periodic inspection of the instrument check that the leak sensor works norma...

Page 435: ... of occurrence of a carryover Otherwise a correct judgment may not be formed Since fluororesin and quartz materials are used for the wetted parts of piping particular attention should be paid when analyzing samples that are likely to be adsorbed by these materials Before Turning on Xenon Lamp Again After the xenon lamp is turned off it remains very hot for a while Under this condition it is not al...

Page 436: ...y Precautions SAFETY 2 WARNING Precautions in the Manual SAFETY 3 CAUTION Precautions in the Manual SAFETY 7 WARNING and CAUTION Labels on Instrument SAFETY 8 NOTICE Precautions SAFETY 11 1 OUTLINE 1 1 1 1 Isocratic System 1 1 1 2 Low Pressure Gradient System 1 2 2 FUNCTIONS 2 1 2 1 Name and Function of Each Part on FL detector 2 1 2 2 Name and Function of Each Part on UI Pad Option 2 3 2 3 Descri...

Page 437: ... 4 4 Time program operation examples 3 33 3 4 5 Spectrum measurement 3 37 3 4 6 Recorder and spectrum output factors setting 3 41 3 4 7 Marker operation 3 45 3 5 Set Up Setting 3 46 3 5 1 Communication channel CH setting 3 46 3 5 2 Thermo cell setting 3 47 3 5 3 Liquid crystal display contrast setting 3 49 3 5 4 Standard xenon lamp lifetime setting 3 50 3 6 Before Performing Analysis 3 52 3 6 1 Se...

Page 438: ...Parts and Consumables 5 1 5 2 Lamp Replacement 5 3 5 2 1 Xe lamp replacement 5 3 5 2 2 Hg lamp replacement 5 17 5 3 Fuse Replacement 5 20 6 INDEX 6 1 APPENDIX APPENDIX 1 INSTALLATION APPENDIX1 1 1 Unpacking APPENDIX1 1 2 Installation Conditions APPENDIX1 2 3 Installation Place APPENDIX1 5 4 Installation Environment APPENDIX1 5 5 Checking the Contents APPENDIX1 6 6 Assembling APPENDIX1 7 6 1 Remova...

Page 439: ...ying a mixing ratio of eluents with time and other optional devices are incorporated in the system 1 1 Isocratic System The isocratic system has a simple configuration in which single solvent analysis is performed Chromaster 5440 Fluorescence detector Detector cell Column Chromaster 5210 Autosampler Chromaster 5310 Column oven Mobile phase Wash fluid Injection valve Wash pump Syringe valve Degassi...

Page 440: ... Mixer Proportioning valve 4 way joint Chromaster 5440 Fluorescence detector Chromaster 5310 Column oven Drain Syringe valve Injection valve Wash pump Detector cell Colum n Chromaster 5210 Autosampler 1 Each of plural eluents is fed from the degassing unit to the low pressure unit 2 In the low pressure unit the eluents are mixed at a pre specified ratio 3 Through the mixer the mixture eluent is de...

Page 441: ... provided for indicating the following states Doors upper and lower right left Three doors are provided Drain tray A tray for liquid leakage Designation Color LED Indication CH1 blue orange Blue CH1 operation mode Orange An error has occurred in CH1 operation mode CH2 blue orange Blue CH2 operation mode Orange An error has occurred in CH2 operation mode Xe LAMP blue Blue Xe lamp is lit PROG RUN bl...

Page 442: ...red signal or the acquired spectral data to other units on the e line Also used to send receive the instrument parameter data via the e line 1 The florescence intensity data is output 2 Used for input output of each contact signal 2 START IN The program is initiated ERROR IN An error condition in another instrument is checked ERROR OUT An error condition on this instrument is indicated 1 e line BU...

Page 443: ...ntegrator 1 The florescence intensity value at each point of time 2 Stored spectral data The florescence intensity value data is output 2 2 Name and Function of Each Part on UI Pad Option A UI pad will be used when a chromato data station or a GUI controller option won t be used for an instrument controlling The UI pad will be invalid when the chromato data station or GUI controller option is conn...

Page 444: ...lamp energy and wavelength accuracy Displays and resets lamp logbook 2 Sets the key lock 2 Press the ESC key to release the key lock 5 PROG Set program Selects and sets the time program 6 Arrow 1 The monitor screen key Accesses the previous screen key Accesses the next screen 2 Editing program key Displays the previous screen Indicates the last line if it is the first line key Displays the next sc...

Page 445: ...d while editing a time program Deletes the step which the cursor is pointed in the input part of TIME Deletes the item when the cursor points a part other than the input part of TIME When the ESC key is pressed while is displayed on the screen the screen returns to the monitor screen and cancels the DEL key processing is displayed after pressing the DEL key and the processing will be determined by...

Page 446: ...transition Fig 2 4 Typical Organic Molecular Energy Level Diagram Figure 3 4 shows the energy level transitions of an organic molecule for the various processes involved in absorption fluorescence and phosphorescence Radiationless transition Absorption Excitation light Excited triplet state Excited state V Phosphorescence Ground state V 3 0 1 2 Light Light 3 Fluorescence 0 1 2 2 6 ...

Page 447: ...d by the substance is lost as vibrational energy the energy emitted by the excited state is less than that absorbed by the compound i e the fluorescence wavelength is longer than the excitation wavelength Stokes Law The ratio of the number of photons emitted during fluorescence to the number of photons absorbed is called the quantum efficiency of fluorescence Fluorescence Yield If two compounds ab...

Page 448: ...ncertainty in the concentration measurement is 20 In contrast in fluorometry a difference in the signal is directly proportional to the concentration of sample An analysis of the error in the measurement is as follows Output signal level at measurement of sample Value corresponding to blank 100 0 1 0 0 1 Difference proportional to concentration of sample 100 0 2 As is evident from this example the...

Page 449: ...elength is different from the excitation wavelength incident beam wavelength scattering due to the excitation radiation is negligible High concentration Low concentration High concentration Low concentration Io IF IF IF Is It Io Is It Amplification a Absorptiometry b Fluorometry Fig 2 5 Comparison of Absorptiometry and Fluorometry In addition to providing high sensitivity fluorescence detection ca...

Page 450: ... B Excitation spectra Component A Fluorescence spectra Component B a Absorptiometry b Fluorometry Fig 2 6 Spectroscopic Measurement of a Sample Containing Two Components Table 3 1 compares the analytical information obtained via absorptiometry and fluorometry Table 2 4 Comparison of Analytical Information Attainable with Absorptiometry and Fluorometry Absorptiometry Fluorometry Absorption spectra ...

Page 451: ...es Both Rayleigh and Raman scatterings occur due to a solvent Take care not to mistake them for fluorescence peaks Table 3 2 presents the position of the Raman peak for a variety of excitation wavelengths In liquid chromatography the Raman scattering appears as a background rise This means that baseline noise increases to disturb high sensitivity measurement Table 2 5 Raman Spectral Peak Position ...

Page 452: ...elatively high various error factors will arise The greatest factor is that the excitation beam is substantially absorbed near the entrance slit of a cell and it cannot reach the cell center adequately An extreme situation is shown in Fig 3 8 Fluorescence is emitted near the entrance slit of a cell but it will not be taken into the emission monochromator Excitation beam Fluorescence emitted Fluore...

Page 453: ...ence occurs when the tail of the shorter wavelength side of fluorescence spectrum overlaps the tail of the long wavelength side of the excitation spectrum When this phenomenon occurs the fluorescence spectrum appears to be somewhat shifted toward the longer wavelength This phenomenon will very rarely cause a substantial error in quantitation when fluorescence detection is used and should not be a ...

Page 454: ...d third order radiation it is simply necessary to place a short wavelength cutoff filter in the path of fluorescing radiation When the second and or third order radiation poses a particular problem it is recommended to use the optional filter set accessory In measurement with a chromatograph the second and third order radiation appears as a background rise Therefore baseline noise will increase to...

Page 455: ...ng to the explanation given above 5 Temperature Dependency of Fluorescence Intensity In most cases the fluorescence intensity decreases by 1 to 2 as the temperature of sample increases by 1 C It should be noted however that in some biochemical samples the fluorescence intensity decreases by approx 10 as the temperature of sample increases by 1 C 2 15 ...

Page 456: ...r Plane mirror Fig 2 11 Functional Block Diagram The beam from the xenon lamp strikes the excitation monochromator that disperses the radiation Only radiation of the specified wavelength is allowed to pass through the exit slit After the exit slit the excitation radiation strikes the sample The fluorescence emitted radiation enters the emission monochromator where it is dispersed by the monochroma...

Page 457: ...instrument 2 4 Specifications 1 Optical system Ratio photometry intensity of transmitted beam is monitored 2 Light source Xe lamp 150 W Hg lamp for checking wavelength 3 Excitation wavelength range 200 to 850 nm Zero order 4 Emission wavelength range 250 to 900 nm Zero order Photomultiplier must be changed at emission wavelength greater than 731 nm 5 Spectral bandwidth on excitation side 15 nm 6 S...

Page 458: ...angent method b With emission side spectral bandwidth set at 30 nm S N ratio for Raman peak of water 900 or more Baseline method Wavelength 350 nm Time constant 2 0 s 14 Auto Zero range 0 to 1000 FLU 15 Offset range 0 to 1000 FLU settable in steps of 1 16 Spectrum memory Memorized contents Excitation and fluorescence spectra Number of spectra memorized 4 Measuring wavelength range Changeable in me...

Page 459: ...tput terminal Option Processor 1 V Full scale Recorder 10 mV Full scale 23 External I O contact terminals Time Program Start Error Input Output Busy Output Above contacts are incorporated in e Line connector and effective with analog connection Auto Zero Input Lamp Off Input 24 Flow cell Standard Constant temperature flow cell Option 25 Flow cell capacity Standard 12 μL irradiated capacity 26 Flow...

Page 460: ... 31 Dimensions 340 W mm 440 D mm 280 H mm 32 Weight Approx 25 kg NOTE Please contact your local Hitachi High Technologies Corporation sales representative about a purchas of the Thermo cell 2 20 ...

Page 461: ...monitor for a long time take a break for 10 to 15 minutes per hour for health of your eyes and body 3 1 Basic Operation First turn on the power supply to display the 1st LCD monitor screen Spend one hour or more for warming up time to stabilize the xenon lamp The numerical value indicated before input is default values or currently set values 3 1 1 Power supply The power activation operation of au...

Page 462: ...ed out The current channel setting LED and the Xe LAMP LED will light in blue Initial screen FL Detector 8928148 00 Hitachi High Technologies Corp 2010 Initializing screen WL DRIVE LAMP INITIALIZING The sequence of wavelength drive check of reference point for drive lighting of the lamp and auto zeroing is performed 3 The first monitor screen will be indicated after initialize processing is comple...

Page 463: ...ntensity FL is indicated within a range from 1000 0 to 1000 0 If the intensity is outside this range is indicated e The thermo cell indication is as follows ON The thermo cell option is running OFF The thermo cell is suspended The thermo cell is disconnected f Status indicators should be read as follows I Initial status R Time program running status B Busy status L Key locked status Elapsed time E...

Page 464: ...9 1 Parameter name Input range Input part b Plural numeric input LAMP CHANGE MM DD YYYY 1 12 Parameter name Input item Input range Input part c Numericl value selection TIME CONSTSANT 0 01s 1 0 02s 2 0 05s 3 4 0 1s 4 0 5s 5 1 0s 6 2 0s 7 Parameter name Selection item Input part d Program setup screen TIME Ex Em BASE PMT 0 0 250 350 1 3 1 Input item Input part 3 4 ...

Page 465: ...you made an error in entering data but have NOT pressed the ENT key press the CL key then re edit the value b If you made an error in entering data and HAVE pressed the ENT key press the ESC key for return to the 1st monitor screen then re edit the value c Press the DEL key to delete the item in the input part while editing the program When the ESC key is pressed while setting plural parameters th...

Page 466: ...e range is exceeded an error message is displayed 3 1 4 Wavelength setting Specify Ex Excitation wavelength and Em Emission wavelength 1 Press the WL key 2 The following display will be presented Set an excitation wavelength Ex cursor appears under Ex Ex wavelength setting screen Ex Em 200 850 0 nm 250 350 Press numeric keys 2 0 0 to 8 5 0 and then the ENT key This wavelength is settable within a ...

Page 467: ...gth 4 Wavelength setting is now completed and the 1st monitor screen returns At Ex and Em the set values are indicated 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 Xe 3 1 5 Shutdown procedure Turn the power supply of the detector off to shut it down The set measurement conditions are retained by the memory even when the power is switched off When power is turned on again the cond...

Page 468: ...1 Press the UTLTY SET UP key 2 The following display will be presented Utility initial screen UTILITY OFFSET 1 TIME CONSTANT 2 _1 USE PROG 3 PMT VOLT 4 OTHERS 5 Select OFFSET Press numeric key 1 and then the ENT key 3 The following display will be presented Offset setting screen OFFSET 0 1000 _ 0 Set an offset value Press numeric key 0 to 1 0 0 0 usually input 0 and then the ENT key An offset valu...

Page 469: ...ssor see Fig 3 2 b 0 10 mV a Offset is not used b Offset is used Fig 3 2 Example of Offsetting 4 Offset setting is now completed and the 1st monitor screen returns Though no value is indicated for FL will be displayed when selecting a value other than 0 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 Xe 3 2 2 Time constant setting Specify electrical response time 1 Press the UTLTY S...

Page 470: ...now completed and the 1st monitor screen returns 3 2 3 Use time program setting It is selectable whether or not to use automatic change of measurement parameters in response to measurement time time program 1 Press the UTLTY SET UP key 2 The following display will be presented Utility initial screen UTILITY OFFSET 1 TIME CONSTANT 2 _3 USE PROG 3 PMT VOLT 4 OTHERS 5 Select USE PROG Press numeric ke...

Page 471: ... is avoided is indicated for PROG 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 Xe 3 2 4 PMT voltage setting Set photomultiplier voltage for fluorescence detection 1 Press the UTLTY SET UP key 2 The following display will be presented Utility initial screen UTILITY OFFSET 1 TIME CONSTANT 2 _4 USE PROG 3 PMT VOLT 4 OTHERS 5 Select PMT VOLT Press numeric key 4 and then the ENT key 3 T...

Page 472: ... bandwidth value of the emission monochromator is settable Standard is 15 nm and wide setting is 30 nm a Press the UTLTY SET UP key b The following display will be presented Utility initial screen UTILITY OFFSET 1 TIME CONSTANT 2 _5 USE PROG 3 PMT VOLT 4 OTHERS 5 Select OTHERS Press numeric key 5 and then the ENT key c The following display will be presented Others setting screen OTHERS Em BANDWID...

Page 473: ...T setting It is selectable whether to enable or disable the error signal output When enabled the following errors can be indicated Xenon lamp error Thermo cell error Thermo cell connection error ADC error DAC error Data buffer overflow CDS system Overheat Refer to Section 4 7 a Press the UTLTY SET UP key b The following display will be presented Utility initial screen UTILITY OFFSET 1 TIME CONSTAN...

Page 474: ...valid 0 or valid 1 status of error out signal output is settable Press numeric key 0 or 1 and then the ENT key Default value 1 e Error out setting is now completed and the 1st monitor screen returns 3 LEAK SENSOR setting Whether to use the liquid leak sensor or not is settable a Press the UTLTY SET UP key b The following display will be presented Utility initial screen UTILITY OFFSET 1 TIME CONSTA...

Page 475: ...e ENT key Default value 0 When use ON 1 of the leak sensor is selected an error message will be indicated upon detection of liquid leakage Refer to Section 4 6 When power supply is restored setting will be use ON 1 of the leak sensor e Selection or avoidance of the leak sensor is now completed and the 1st monitor screen returns 4 LAMP setting ON or OFF status of the xenon lamp is selectable in the...

Page 476: ...amp Press numeric key 0 or 1 usually input 1 and then the ENT key Default value 1 e Xenon lamp setting is now completed and the 1st monitor screen returns When the xenon lamp is lit Xe is displayed for LAMP And when the lamp is extinguished OFF is displayed for LAMP 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 OFF The Xe lamp will light up when this unit is powered on NOTE A xeno...

Page 477: ... desired is already indicated it must be reentered without fail 3 3 1 Xe lamp logbook data display Total on period of the Xe lamp and its standard lifetime in parentheses under Xe LAMP the number of switching on times and the date of the last lamp change can be indicated 1 Press the GLP key 2 The following display will be presented GLP initial screen GLP LOGBOOK 1 KEY LOCK 2 1 WL CHECK 3 Xe CHECK ...

Page 478: ...ge will be indicated Logbook report screen Xe LAMP SWITCHING LAST CHANGED DATE 123h 500 23 times 9 1 2010 Press the ENT or ESC key 6 Logbook display is now completed and the 1st monitor screen returns 3 3 2 Xe lamp logbook data resetting Total on period of the Xe lamp the number of switching on times and the date of the last lamp change are reset 1 Press the GLP key 2 The following display will be...

Page 479: ...lamp change date setting screen for setting the date of xenon lamp change 5 Set the date of xenon lamp change in the following procedure a Input a month for MM cursor appears under MM Xe lamp change date setting screen month Xe LAMP CHANGE MM DD YYYY 1 12 9 1 2010 Press numeric key 1 to 1 2 and then the ENT key The cursor moves to DD b Input a day for DD Xe lamp change date setting screen day Xe L...

Page 480: ...eriod of the Xe lamp and the number of switching on times will be automatically reset accordingly 3 3 3 Hg lamp logbook data display Total on period of the Hg lamp the number of switching on times and the date of the last lamp change can be indicated 1 Press the GLP key 2 The following display will be presented GLP initial screen GLP LOGBOOK 1 KEY LOCK 2 1 WL CHECK 3 Xe CHECK 4 Select LOGBOOK Pres...

Page 481: ...ED DATE 12h 56 times 9 1 2010 Press the ENT or ESC key 6 Logbook display is now completed and the 1st monitor screen returns 3 3 4 Hg lamp logbook data resetting Total on period of the Hg lamp the number of switching on times and the date of the last lamp change are reset 1 Press the GLP key 2 The following display will be presented GLP initial screen GLP LOGBOOK 1 KEY LOCK 2 1 WL CHECK 3 Xe CHECK...

Page 482: ...edure a Input a month for MM cursor appears under MM Hg lamp change date setting screen month Hg LAMP CHANGE MM DD YYYY 1 12 _9 1 2010 Press numeric key 1 to 1 2 and then the ENT key The cursor moves to DD b Input a day for DD Hg lamp change date setting screen day Xe LAMP CHANGE MM DD YYYY 1 31 9 1 2010 Press numeric key 1 to 3 1 and then the ENT key The cursor moves to YYYY c Input a year for YY...

Page 483: ...ill be presented GLP initial screen GLP LOGBOOK 1 KEY LOCK 2 2 WL CHECK 3 Xe CHECK 4 Select KEY LOCK Press numeric key 2 and then the ENT key 3 The following display will be presented Key lock selecting screen KEY LOCK YES 1 NO 0 1 Set selection 1 or avoidance 0 of KEY LOCK Press numeric key 1 or 0 usually input 1 and then the ENT key Default value 0 Even with the keys locked the monitor screen ca...

Page 484: ...rs and it is checked whether wavelength is normal or not WL accuracy checking screen running CHECKING WL ACCURACY If an Hg lamp lighting error occurs the error message shown below will appear Return to the 1st monitor screen by pressing the CL key Hg lamp error screen Hg LAMP ERROR PRESS CL KEY TO CLEAR MESSAGE 4 The result of excitation wavelength Ex check will be displayed automatically Ex side ...

Page 485: ... or ESC key the system will return automatically to the 1st monitor screen 6 When the wavelength accuracy check is finished the system returns to the 1st monitor screen 3 3 7 Xe lamp energy check Energy level of the xenon lamp can be checked using the xenon lamp beam at 254 nm 1 Press the GLP key 2 The following display will be presented GLP initial screen GLP LOGBOOK 1 KEY LOCK 2 4 WL CHECK 3 Xe ...

Page 486: ... without pressing ENT or ESC key the system will return automatically to the 1st monitor screen 5 When the Xe lamp energy check is finished the system returns to the 1st monitor screen NOTE When the temperature of the Xe lamp is high the sealed gas pressure will fluctuate and the lamp may be difficult to ignite Before restarting the instrument or re lighting the lamp wait at least five minutes for...

Page 487: ...go back to the preceding step or the V key to advance to the next step When the setting at each step is finished press the ESC key to return to the 1st monitor screen and the time program is registered NOTE When setting the time program be sure to set the TIME for the first step at 0 0 This cannot be changed or deleted And for the final step of the program be sure to set the measurement completion...

Page 488: ... appears 0 is always indicated here Mode setting screen EDIT MODE MODIFY 0 NEW 1 1 Press a numeric key 0 or 1 and then the ENT key to either use MODIFY 0 or delete NEW 1 the conditions in the time program No selected above 0 Conditions in the time program No selected above are used additions or changes can be made in the program 1 Conditions in the time program No selected above are deleted and ne...

Page 489: ... bottom right of the screen The cursor now moves to Ex b Set an Ex excitation wavelength Step setting screen Ex indicated TIME Ex Em BASE PMT 0 0 250 1 Press numeric keys 2 0 0 to 8 5 0 and then the ENT key Setting range 200 to 850 nm It is recommended to set the same wavelength as was set for Ex of the measuring wavelengths Initial default value blank The cursor next moves to Em c Set an Em emiss...

Page 490: ... executed Data baseline is set to the zero point of the recorder 2 HOLD is executed Baseline is held so that it doesn t fluctuate HOLD function is released by executing AUTO ZERO Initial default value 1 e Set the PMT photomultiplier voltage Step setting screen PMT indicated TIME Ex Em BASE PMT 0 0 250 350 1 3 1 Press a numeric key 1 to 5 and then the ENT key f When the setting for the first step i...

Page 491: ...ents of 0 1 minute The cursor now moves to Ex b Set an Ex excitation wavelength to be changed Step setting screen Ex indicated TIME Ex Em BASE PMT 10 0 400 1 1 Press numeric keys 2 0 0 to 8 5 0 and then the ENT key The cursor next moves to Em c Set an Em emission wavelength to be changed Step setting screen Em indicated TIME Ex Em BASE PMT 10 0 400 500 1 Press numeric keys 2 5 0 to 9 0 0 and then ...

Page 492: ...ess a numeric key 1 to 5 and then the ENT key f When the setting for the second step is completed return to the TIME setting on step setting screen If more parameters will be changed then repeat the operation in this subsection If parameters will not be changed advance to the final step setting 6 Setting of final step of time program a Set the measurement end TIME Step setting screen TIME indicate...

Page 493: ...ogram starting Press the START key to start the time program Status indication on the 1st monitor screen becomes R time program is running and the elapsed time is indicated at TIME The PROG RUN LED lights up in blue 1st monitor screen TIME Ex Em FL PROG LAMP R 250 350 0 0 1 Xe 3 4 3 Time program stopping Press the STOP key then the time program under execution stops and the 1st monitor screen retu...

Page 494: ...ed here is an example of newly setting a time program at program No 1 Ten minutes after the start 1 photomultiplier voltage is changed from MID to LOW excitation wavelength from 250 to 270 nm emission wavelength from 350 to 370 nm and hold function is applied then measurement is completed after 20 minutes 2 3 34 ...

Page 495: ...then the ENT key TIME Ex Em BASE PMT 0 0 250 350 1 3 1 Press 1 0 keys and then the ENT key Press 2 7 0 keys and then the ENT key Press 3 7 0 keys and then the ENT key Press 2 key and then the ENT key Press 2 key and then the ENT key TIME Ex Em BASE PMT 10 0 270 370 2 2 1 Press 2 0 keys and then the ENT key TIME Ex Em BASE PMT 20 0 1 Press the ESC key Time program setting is now finished TIME Ex Em...

Page 496: ...key EDIT MODE MODIFY 0 NEW 1 0 Press 0 key and then the ENT key Step at startup is indicated TIME Ex Em BASE PMT 0 0 250 350 1 3 1 Press V key to access the next step TIME Ex Em BASE PMT 10 0 270 370 2 2 1 Press V key to access the next step TIME Ex Em BASE PMT 20 0 1 Press the ESC key and the 1st monitor screen returns TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 Xe 3 36 ...

Page 497: ...e than 30 nm apart for measurement NOTE The maximum wavelength scan range from end to start wavelength for both excitation and emission is 400 nm For spectrum acquisition in a range greater than 400 nm the range should be divided into two for measurement NOTE Saved spectral data will not be retained when the power is turned OFF 1 Measurement and Recording of Spectrum for Excitation Ex Scan Range a...

Page 498: ... nm FL Ex 250 850 200 600 Press numeric keys 2 5 0 to 8 5 0 and then the ENT key Input value Value of less than 850 within WL1 50 to WL1 400 Setting range 250 to 850 nm Initial default value 600 Pressing U key prior to the ENT key will return to WL1 e A memorize spectrum setting screen will now appear Memorize spectrum setting screen MEMORIZE SPECTRUM NO 1 4 1 Set a memorize spectrum number for th...

Page 499: ...ve g When the spectral data memorization is completed the system returns to the 1st monitor screen automatically 2 Measurement and Recording of Spectrum for Emission Em Scan Range a Press the SPECT key b The scan mode setting screen will appear Scan mode setting screen SPECTRUM MODE FL Ex 1 FL Em 2 2 Press numeric key 2 and then the ENT key to select FL Em Now proceed to the scan range setting scr...

Page 500: ...Setting range 300 to 900 nm Initial default value 700 Pressing U key prior to the ENT key will return to WL1 e A memorize spectrum setting screen will now appear Memorize spectrum setting screen MEMORIZE SPECTRUM NO 1 4 1 Set a memorize spectrum No for the spectral data Press a numeric key 1 to 4 and then the ENT key Initial default value blank Upon entering a memorize spectrum No the previous spe...

Page 501: ...sion due to solvent or impurities in it and second or third order emission may be superimposed on the emission of the analyte element Similarly an excitation spectrum may be affected by scattered light at the emission wavelength by Raman scattering due to solvent by emission due to solvent or impurities contained in it and by second or third order scattered light of the excitation beam These facto...

Page 502: ...le range setting screen RCD RANGE 1 1000 1000 Press numeric keys 1 to 1 0 0 0 and then the ENT key to set a recorder full scale range Initial default value 1000 d When the setting of recorder full scale range is finished the system returns to the 1st monitor screen 2 Setting of Recorder Output Speed a Press the RECORD key b The recorder setting screen appears Recorder setting screen RECORD RCD RAN...

Page 503: ...RCD SPEED 2 3 SPECT RCD 3 Press numeric key 3 and then the ENT key to select SPECT RCD spectral recording c The output data spectrum No setting screen appears Output data spectrum No setting screen RECORD SPECTRUM NO 1 4 1 Press a numeric key 1 to 4 and then the ENT key to set a spectrum No to be output Initial default value 1 d The background spectrum No setting screen now appears The background ...

Page 504: ...e indicated below will appear Press the CL key and the 1st monitor screen will return Error display SPECTRA ARE MISMATCHED PRESS CL KEY TO CLEAR MESSAGE e The ready for output monitor screen will appear Ready for output monitor screen RCD NO SPEED WL RANGE Em WIDTH STD 1 60 200 600 PRESS START Press the START key Pressing the ESC key prior to the START key will cancel the process The output spectr...

Page 505: ...een will return automatically 3 4 7 Marker operation A marker line is indicated only on the recorder It is usable as an event marker to indicate for example the start of measurement or the point where set conditions were changed during measurement Press the 1 MARKER key to indicate a marker line on the recorder data 3 45 ...

Page 506: ...ion channel via the e Line in the following way 1 Turn on the power switch with the UTLTY SET UP key held down 2 The following display will be presented Setup initial screen SETUP DETECT THERMO CONTRAST S NO CH1 NO USE 4 02AB 111 Press the ENT key 3 The following display will be presented Setup items selecting screen SETUP ITEMS DETECTOR 1 THERMO CELL 2 1 CONTRAST 3 EXCHANGE STANDARD 4 Select DETE...

Page 507: ...n advance to LCD contrast setting The selected setting will be fetched upon turning on power supply at the next time 6 Turn off the power switch 3 5 2 Thermo cell setting It is selectable whether or not to use the optional thermo cell 1 Turn on the power switch with the UTLTY SET UP key held down 2 The following display will be presented Setup initial screen SETUP DETECT THERMO CONTRAST S NO CH1 N...

Page 508: ...ection or avoidance of the thermo cell is now completed and the setup initial screen appears Under THERMO the selected channel setting is indicated Setup initial screen SETUP DETECT THERMO CONTRAST S NO CH1 USE 4 02AB 111 When you press the ENT key here the setup items selecting screen is presented to allow reentry Or you can advance to LCD contrast setting The selected setting will be fetched upo...

Page 509: ...ng screen SETUP ITEMS DETECTOR 1 CONTRAST 2 3 CONTRAST 3 EXCHANGE STANDARD 3 Select CONTRAST Press numeric key 2 and then the ENT key 4 The following display will be presented LCD contrast setting screen LCD CONTRAST 1 7 3 Set a LCD CONTRAST value Press a numeric key 1 to 7 usually input 3 and then the ENT key 1 Dark 7 Bright Default value 4 5 LCD contrast setting is now completed and the setup in...

Page 510: ...ormally to cause a danger of burst etc Replace the xenon lamp with a new one before its cumulative turn on time exceeds the guaranteed useful lifetime The standard life time of the xenon lamp is settable This setting activates the following function If the total operation time of the Xe lamp is longer than the standard lifetime upon turning on the lamp an error message is indicated to notify that ...

Page 511: ...teed Life Limit Allowable Input 650 1500 150 W Xe lamp 150 hours 500 hours 500 or less 890 2019 Long life Xe lamp 500 hours 1 000 hours 1000 or less Default value 500 hours J851152 Xe lamp is attached with shipment 5 The setting of a standard Xe lamp lifetime is now completed and the following display will be presented Setup initial screen SETUP DETECT THERMO CONTRAST S NO CH1 USE 3 02AB 111 When ...

Page 512: ...peration immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemicals If a flammable chem...

Page 513: ...teristics of Organic Solvents 2 When performing high sensitivity analysis with a UV detector use solvents whose UV absorption characteristics are especially small Use solvents for liquid chromatograph commercially available Absorption characteristics of special grade reagents such as methanol ethanol and acetonitrile generally and widely used are greatly different in the short wavelength range dep...

Page 514: ...contain halogen ions such as HCl KCl NaCl NH4Cl are typical reagents Reagents which may be restricted are shown in Table 4 1 use the table as a rough standard NOTE When unsuitable reagents absolutely necessary for ingredient separation or reaction of a constituent have been used or when mobile phase which deposits salt has been used wash all the flow paths with distilled water after completing ana...

Page 515: ...e Ammonium phosphate Boric acid Formic acid up to pH3 Hydrochloric acid up to pH3 Potassium nitrate Sodium hydrogencarbonate Sodium carbonate Ammonium chloride Potassium chloride Sodium chloride Tolufluoroacetic acid Note 1 Max concentration of above reagents should be 5 6 Note 2 When the above reagents have been used necessarily wash all the flow paths with distilled water completely without fail...

Page 516: ...ormality is found stop operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemi...

Page 517: ...y For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper protective clothes e g safety goggles so that a solvent will not come into direct contact with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor 3 57 ...

Page 518: ... 1 4 Ethyl ether 0 38 1 353 220 45 180 1 9 48 2 6 35 0 7 Ethyl sulfide 0 38 0 23 1 442 290 Chloroform 0 40 0 45 1 443 245 Methylene chloride 0 42 0 57 1 424 245 50 518 9 3 8 15 4 2 2 38 5 0 9 Methyl i butyl ketone 0 43 0 44 1 394 330 Tetrahydrofurane 0 45 1 408 220 14 4 321 1 2 11 8 2 5 66 1 0 9 Ethylene dichloride 0 49 1 445 230 13 3 412 3 6 2 16 3 4 83 9 1 3 Methyl ethyl ketone 0 51 0 79 1 381 3...

Page 519: ...olvents whose boiling point is 55 C or higher Solvents of low boiling point are not only dangerous but also generate bubbles when sucked by pump so that normal pumping will be impossible 3 When performing high sensitivity analysis with UV detector use solvents which absorb especially small amount of UV light Since special grade reagents such as methanol and acetonitrile generally used absorb the s...

Page 520: ...tive container for waste solution and provide proper grounding connection to it Since flammable organic solvents are used for the high speed liquid chromatograph be careful about heat and fire Since thin tubings are used for the liquid chromatograph static electricity is easily generated If charged liquid is collected into an insulated waste container for example and an electric discharge occurs s...

Page 521: ...Variation of pump pressure e Reduced precision of gradient mixing ratio 2 For degassing mobile phase two methods are available Degassing unit and Manual Degassing method is explained in 3 7 2 3 Use mobile phase without dust Dust in mobile phase causes trouble in pumping and the pressure may vary 3 7 2 Degassing mobile phase There are various ways of degassing Perform degassing suitable for the pur...

Page 522: ...sonic cleaner c When degassing small bubbles are generated first then gradually larger bubbles are generated Continue degassing until bubbles are not generated anymore It takes 5 to 10 minutes to finish d When bubble generation finishes turn off the power of ultrasonic cleaner e Take out mobile phase container from ultrasonic cleaner wipe the water from the container and set the container to liqui...

Page 523: ... or drift of baseline may be caused NOTE Degas mobile phase of aqueous solution by using both ultrasonic cleaner with water and aspirator to decrease pressure Fix the degassing time b Insert rubber tube of aspirator into mouth of reagent bottle c Turn on the power of ultrasonic cleaner d Open the faucet of city water for aspirator to decrease pressure e When degassing small bubbles are generated f...

Page 524: ...ratio of mobile phase may be varied by degassing time boiling point of mobile phase would vary with a reduced pressure 3 7 3 Removing dust from mobile phase There are various ways to remove dust from mobile phase Remove dust in the way suitable for the purpose of use 1 Example of Filtering of Mobile Phase by Using Membrane Filter Removing dust and degassing can be performed simultaneously by filtr...

Page 525: ...of data e g generating abnormal peaks etc a Example of filtering samples Dust in sample can be removed easily as follows Take sample in Syringe attach cartridge type 0 45 µm membrane filter and perform filtering See the figure left NOTE There are various ways for filtering sample Filtering sample in the way suitable for the sample amount Filtered clean sample Filtering by cartridge type 0 45 µm me...

Page 526: ...foreign matters can be removed as follows Take sample in Syringe attach Normal Phase cartridge and perform filtering See the figure left NOTE There are various ways for removing foreign matters in sample Remove in the way suitable for the purpose of analysis Cartridge of silica gel Clean sample after removing foreign matters 3 66 ...

Page 527: ...heck the performance Positional adjustment of the lamp is necessary for an accurate performance check NOTE When this detector unit is used in combination with Hitachi Chromaster control option the lamp energy wavelength accuracy and sensitivity can be automatically calculated For details refer to the instruction manual of Hitachi Chromaster control option 4 2 1 Xe lamp energy check Check the energ...

Page 528: ...or the measurement The following items are required Pump Recorder or D 2500 chromato data processor Distilled water 1 Injection of Distilled Water Connect tubing as shown in Fig 4 1 supply distilled water at a flow rate of 1 mL min for 3 minutes with the Chromaster 5110 Pump in Manual mode then set the flow rate to 0 and stop the supply of water Remove the flow cell unit and check for any bubbles ...

Page 529: ... results see sections 3 4 2 3 4 3 3 4 5 and 3 4 6 Measure in the following sequence Excitation Ex wavelength 350 nm Time constant response 2 seconds Photomultiplier voltage MID Emission spectrum bandwidth STANDARD 15 nm or WIDE 30 nm Emission spectrum measuring wavelength 350 to 450 nm Spectrum No Any of 1 to 4 a Turn ON the power switch and the 1st monitor screen appears b Set an excitation wavel...

Page 530: ...hotomultiplier voltage and an emission spectrum bandwidth i Press the UTLTY SET UP key and the utility setting screen appears Utility setting screen UTILITY OFFSET 1 TIME CONSTANT 2 _2 USE PROG 3 PMT VOLT 4 OTHERS 5 Press numeric key 2 and then the ENT key ii The time constant setting screen appears Time constant setting screen TIME CONSTANT 0 01s 1 0 02s 2 0 05s 3 7 0 1s 4 0 5s 5 1 0s 6 2 0s 7 Pr...

Page 531: ... the utility setting screen reappears Utility setting screen UTILITY OFFSET 1 TIME CONSTANT 2 5 USE PROG 3 PMT VOLT 4 OTHERS 5 Press numeric key 5 and then the ENT key viii The others setting screen appears Others setting screen OTHERS Em BANDWIDTH 1 ERROR OUT 2 1 LEAK SENSOR 3 LAMP 4 Press numeric key 1 and then the ENT key ix The Em bandwidth setting screen appears Em bandwidth setting screen Em...

Page 532: ...range setting screen SCANNING WL RANGE WL1 WL2 nm FL Em 250 850 350 700 Press numeric keys 3 5 0 and the ENT key Enter an end wavelength maximum value for WL2 Scan range setting screen SCANNING WL RANGE WL1 WL2 nm FL Em 400 750 350 450 Press numeric keys 4 5 0 and the ENT key iii The memorize spectrum No setting screen appears Memorize spectrum No setting screen MEMORIZE SPECTRUM NO 1 4 1 Press a ...

Page 533: ...NGE 1 RCD SPEED 2 1 SPECT RCD 3 Press numeric key 1 and then the ENT key ii The recorder full scale setting screen appears Recorder full scale setting screen RCD RANGE 1 1000 1000 Press numeric keys 1 0 0 0 and then the ENT key iii The 1st monitor screen returns iv Press the RECORD key And the recorder setting screen appears Recorder setting screen RECORD RCD RANGE 1 RCD SPEED 2 2 SPECT RCD 3 Pres...

Page 534: ... 1 Press a numeric key 1 to 4 and then the ENT key Set the same number as was entered when making the setting for spectrum measurement ix The background spectrum No setting screen appears Background spectrum No setting screen BACKGROUND SPECTRUM NO 0 4 0 Press numeric key 0 and then the ENT key x The output ready monitor screen appears Output ready monitor screen RCD NO SPEED WL RANGE Em WIDTH STD...

Page 535: ...f the detector and data processor are connected via E Line digital start the output by pressing the ALL START key of the data processor 3 Determination of Raman Signal Intensity S tangent method Tangent Baseline S baseline method Fig 4 2 Measuring the Raman Signal Intensity Determine the voltage value corresponding to S in the figure When using the D 2500 chromato data processor calculation can be...

Page 536: ...or and record the baseline A suitable attenuator setting is ATT 0 when using the D 2500 Drift can also be measured if the measurement is continued for 15 minutes or longer NOTE In measurement with the emission spectrum bandwidth set at WIDE 30 nm the peak emission wavelength is shifted toward the shorter wavelength side from 397 nm Due to the WIDE setting the spectrum bandwidth widens for the scat...

Page 537: ...e Calculation extracted from JAIMAS 0005 1984 NOTE The Raman spectrum of water and the noise level may be affected by the purity of the water used and or the presence of air bubbles 7 Measurement of Raman Spectrum of Water Using a Time Program when Raman signal intensity obtained in the preceding subsection 2 is low If the sensitivity S N ratio of Raman peak of water is low recheck the following i...

Page 538: ...ell To prevent this first inject ethanol or the like and then water iii Change the method of spectrum measurement via time program Measure the Raman spectrum of water using a time program But first check the fluctuation of FL value via wavelength shift Set the excitation Ex wavelength at 350 nm and emission Em wavelength at 450 nm using the WL key Then zero the FL value with the A Z key Next with ...

Page 539: ...5 1 6 430 1 8 450 2 0 NOTE The above time program shows an example where the minimum FL value was obtained at 380 nm and the maximum at 400 nm For the top Em of the program set a wavelength that includes the wavelengths where the maximum and minimum FL values were obtained For instance if the maximum FL value was obtained at a wavelength of 397 nm then the wavelength at 1 1 minutes should be set a...

Page 540: ...m X ATT setting of data processor used in measurement Refer to previous subsections 4 through 6 for measurement and calculation of noise and calculation of S N ratio 8 Measurement of Drift Drift is measured by using the data and baseline obtained from the Raman spectrum of water measurement conditions are the same as in preceding subsection 4 but measuring time is 15 minutes For the sake of simpli...

Page 541: ...of the builtin Hg lamp As for the wavelength accuracy of the excitation side monochromator the Em side is fixed at the wavelength position where the abovementioned bright line was detected then the Ex wavelength where a Rayleigh scattering peak of 254 nm is produced is measured D Baseline emission wavelength 397 nm 15 minutes S tangent method Baseline baseline method A S Drift D A x 100 3 15min Ma...

Page 542: ...n 2 Calibration of Wavelength Accuracy If there is a wavelength deviation then adjust the wavelength in the wavelength calibration mode special mode a Calibration of excitation wavelength i Press the UTLTY SET UP key and the utility setting screen appears Utility setting screen UTILITY OFFSET 1 TIME CONSTANT 2 99 USE PROG 3 PMT VOLT 4 OTHERS 5 Press numeric keys 9 9 and then the ENT key ii The exc...

Page 543: ...G 3 PMT VOLT 4 OTHERS 5 Press numeric keys 9 8 and then the ENT key ii The emission wavelength calibration mode screen appears Emission wavelength calibration mode screen Em WL ADJUST 1 20 10 ONLY FOR FACTORY USE 2 The present offset value is indicated at Em WL ADJUST Indicated at the bottom right of the screen is the wavelength check result deviation of wavelength indication range of 10 to 10 Wav...

Page 544: ... detects a liquid leak 1 While a solvent is used the leak sensor function should be kept active 2 The leak sensor function of this instrument may not work when liquid leaks in a small amount Leakage of a highly volatile solvent may not be detectable either Even when the leak sensor function is activated you should be careful not to overlook liquid leakage for avoiding a serious situation 3 As a ro...

Page 545: ...the liquid leak sensor and drain tray and then fasten the sensor to the drain tray again NOTE While cleaning the liquid leak sensor be careful not to damage its tip If damaged the liquid leak sensor may not work properly or an error may occur Liquid leak sensor fastening screw Fig 4 7 Liquid Leak Sensor Fastening Screw NOTE Mount the leak sensor at the correct position If the sensor is mounted at ...

Page 546: ...ent will not come into direct contact with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor Refer to the following procedure for the drain tray check 1 Remove retaining screws to detach the drain tray NOTE Avoid breakage of the detached leak sensor to prevent malfunction 2 Pull out the drain tray from the unit 3 Wipe up the drain tray wi...

Page 547: ...y Yearly Check wavelength by using bright line of Hg lamp at 254 nm See 4 2 4 NOTE First adjust the xenon lamp position see 6 2 1 3 then make an energy check of the xenon lamp and a wavelength accuracy check using the Hg lamp Correct measurement results will not be obtained unless the lamp position is adjusted 4 3 1 Xe lamp energy check Check the energy level of the Xe lamp at a wavelength of 254 ...

Page 548: ...alibration is required Refer to section 4 2 4 2 for the calibration 4 3 3 Lamp logbook check The cumulative turn on time number of lightings and last replacement date for the Xe and Hg lamps can be checked via the GLP function see 3 3 4 22 ...

Page 549: ...aste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemicals If a flammable chemical such as organic solvent leaks from the ...

Page 550: ...of Flow Cell 1 Loosen the retaining screw of the flow cell unit see Fig 4 8 2 Pull the flow cell unit straight out 3 Check the inside of the cell visually to see if it is contaminated with any foreign substance crystallized substance etc 4 Check the outside of the cell for any leakage 5 If contamination is observed inside the cell it must be cleaned with an appropriate solution If an aqueous solve...

Page 551: ...the wash fluid with the mobile phase that is used for separation and repeat the procedure in step 5 7 If air bubbles are observed in the flow cell supply solution into the cell with the pump at a flow rate within 1 0 mL min and a pressure within 1 0 MPa While the solution is being supplied into the flow cell pinch the end of the drain tube with your fingers for a few seconds to increase the pressu...

Page 552: ...assembly and cleaning of flow cell 1 Disassembly of Flow Cell If contamination is not removed by just flushing the interior of the flow cell then disassemble and clean the cell in the procedure below Shielding plate Retaining screw 1 Retaining screw 2 Setscrew 1 Setscrew 2 Fig 4 11 Flow Cell Unit a Loosen retaining screws 1 and 2 and detach the shielding plate b Detach the cell window 4 26 ...

Page 553: ...eaner In this case be sure to put the flow cell in a paper or plastic container and then place it in the ultrasonic cleaner so as to avoid scratching the cell b Wipe the surface of the flow cell with gauze that is moistened with acetone or ethanol NOTE Be careful not to scratch the flow cell surface when disassembling it NOTE Make sure to put the flow cell in a paper or plastic container when clea...

Page 554: ...is no leakage NOTE Be careful not to scratch the flow cell surface when assembling it NOTE Take care about the orientation of the polished surfaces of the flow cell when putting it into the cell holder see Fig 4 11 A mistake in the orientation may preclude obtaining the proper performance from the instrument NOTE Tighten setscrew 1 fully with hand and then tighten setscrew 2 about 30 manually or t...

Page 555: ...rs though liquid comes out of the tube normally setscrew tightening may be slightly inadequate Retighten setscrew 1 lightly about 10 to 20 with a wrench or setscrew 2 lightly about 10 to 20 manually 4 Wipe up any liquid spilt on the outside of the flow cell 5 Before returning the flow cell unit into position supply liquid with the pump and make sure there is no more leakage NOTE It is important th...

Page 556: ... few days clean the flow cell interior thoroughly by pumping distilled water or alcohol through it and then store it in a safe place If the period of nonuse is less than a few days the inside of the cell may be filled completely with a solvent such as ethanol or acetonitrile and then stored 4 30 ...

Page 557: ...e monitor screen Press the ESC key The READY status will be presented The xenon lamp is still hot Turn on the lamp again For turning on the lamp again wait at least 5 minutes after the Xe lamp went out The xenon lamp does not light The Xe lamp has reached the end of its useful life Check the cumulative turn on time of Xe lamp Replace the Xe lamp with a new one The flow cell is contaminated Visual ...

Page 558: ...gy level Adjust lamp position 5 2 1 Error in flow cell mounting Visual check Correctly mount flow cell 4 4 Poor S N ratio Flow cell surface scratched Visual check Replace flow cell 4 4 Water is not injected in the flow cell Inject water into the flow cell Bubbles have entered the flow cell Visual check Remove bubbles 4 4 Poor adjustment of xenon lamp position Check lamp energy level Adjust Xe lamp...

Page 559: ...monitor screen returns 2 Turn on power again 3 Contact your nearest service office of Hitachi High Technologies sales representative Ex Em SIDE OF WL DRIVE MECHANISM ERROR Failure in detecting Ex or Em wavelength origin during self diagnosis test initialization 1 Cannot be released by key operation 2 Turn on power again 3 Contact your nearest service office of Hitachi High Technologies sales repre...

Page 560: ... exchange time 1 Press CL key and 1st monitor screen returns 2 Replace the lamp with a new one A Z OVER RANGE PRESS CL KEY TO CLEAR MESSAGE Allowable auto zero range has been exceeded 1 Press CL key and 1st monitor screen returns 2 Change the wavelength 3 Replace the solvent with another one 4 Clean the flow cell NO SPECTRA PRESS CL KEY TO CLEAR MESSAGE Spectrum of specified No is not found 1 Pres...

Page 561: ...ation 2 Turn on power again 3 Contact your nearest service office of Hitachi High Technologies sales representative THERMO CELL ERROR An error has occurred at the thermo cell 1 Cannot be released by key operation 2 Turn on power again 3 Contact your nearest service office of Hitachi High Technologies sales representative An error message will be displayed together with the alarm buzzer sounding NO...

Page 562: ... to customer 890 2019 Long life xenon lamp Special accessory Guaranteed life 500 hours Limit 1000 hours Warranty period 6 months after delivery to customer 890 2662 Mercury lamp Guaranteed life 100 hours 2 years J821349 Time lag fuse 5 A 890 2932 Flow cell 12 μL 9600 hours 5 years 890 2684 Drain tube ID 0 33 0 62 T 9600 hours 5 years Length 2 m Outside diameter 1 57 mm 893 0833 Inlet tube ID 0 25 ...

Page 563: ...s Example use Piping between column outlet and inlet tube For standard flow cell Length 350 mm Inner diameter 0 25 mm Outer diameter 1 57 mm Material SUS PTFE for coating M790019 Screw S SUS 9600 hours 5 years Example use Connecting pipe L329109 Ferrule SUS 9600 hours 5 years Example use Connecting pipe 5 2 ...

Page 564: ...e hot xenon lamp or its housing could result in severe burns Before proceeding to lamp replacement turn off the power switch and then wait for at least one hour until the lamp and its housing cool down sufficiently For replacing the xenon lamp immediately after the use the lamp must be cooled first of all because it is still hot Once the Xe lamp has been cooled adequately you can proceed to its re...

Page 565: ...hen the ENT key c The Xe lamp setting screen appears Xe lamp setting screen Xe LAMP ON OFF OFF 0 ON 1 0 Press numeric key 0 and then the ENT key d The 1st monitor screen appears and OFF is indicated at LAMP 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 OFF e The xenon lamp is thus turned off Although the lamp is off the fan continues rotating so as to cool down the lamp Wait for a...

Page 566: ...jury due to Xenon Lamp Explosion If a strong shock or impact is applied to the xenon lamp or if the surface of its quartz glass part is scratched it may explode and scatter glass pieces resulting in personal injury Be sure to wear proper protective gear such as safety goggles safety mask thick long sleeves and gloves when handling the xenon lamp a Turn OFF the power switch and unplug the power cor...

Page 567: ...n body and loosen the lamp house retaining screw Lamp house Retaining screw Grip Connecter Fig 5 2 Removal of Connector and Retaining Screw e Lift the grip of the lamp house lightly and pull it toward you then detach the lamp house from the main body Lamp house Grip Fig 5 3 Removal of Lamp House 5 6 ...

Page 568: ...used xenon lamp wrap it with a thick cloth e g triple folded cotton cloth completely and crush its glass part with a hammer or the like Then discard the xenon lamp as a dangerous waste item properly If the xenon lamp is discarded without being crushed it could explode due to possible impact at the time of disposal scattering glass pieces to cause personal injury WARNING Injury due to Xenon Lamp Ex...

Page 569: ... thin metal wire is attached near the center of the bulb which facilitates ignition of the lamp Take care not to break this wire when handling the lamp g Loosen the cathode nut and remove the cathode lead plate Fig 5 5 Anode cord Anode nut Metal fixture Cathode nut Cathode lead plate Lamp bulb Ceramic plate Cathode cord Lamp protrusion Metal wire Fig 5 5 Detachment of Xenon Lamp 5 8 ...

Page 570: ...n lamp in the specified direction If the mounting direction polarity is wrong the cathode will be consumed significantly to disable turn on of the lamp Mount the lamp so that the anode mark on it will be positioned at the support metal of the lamp holder If the lamp with its cathode consumed excessively is used continuously pressure inside the lamp bulb may become too high causing possible explosi...

Page 571: ...ont panel Fig 5 7 Be careful not to touch the lamp bulb Note that a thin metal wire is attached near the center of the bulb which facilitates ignition of the lamp Take care not to break this wire when handling the lamp Also if the thin metal wire is not located on the side of the lamp having the small protrusion slide the wire so it is properly positioned there New xenon lamp Anode nut Cathode nut...

Page 572: ... NOTE Mount the xenon lamp so that the protrusion on the bulb faces the instrument front panel Fig 5 4 A mistake in the orientation may cause an increased light loss and preclude obtaining the desired performance from the instrument j After mounting the Xe lamp in the lamp house assemble it into the main body Fig 5 2 Raise the lamp house and insert it into the main body then lower it and press it ...

Page 573: ... when it is lit Be sure to wear tinted safety glasses to prevent possible eye damage The position of the beam slightly differs from one lamp to another so it is necessary to adjust the lamp position before the detector is first used or when the lamp is replaced Use the three adjusting screws on the right side of the instrument for the adjustment HORIZONTAL For adjusting horizontal position FOCUS F...

Page 574: ... Adjustment Screw Cover HORIZONTAL FOCUS VERTICAL Fig 5 9 Lamp Positional Adjustment a Coarse adjustment Set the excitation Ex wavelength at 550 nm and make the adjustment while observing the image of the light beam Take the following steps for the adjustment see section 3 1 4 5 13 ...

Page 575: ... appears 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 Xe ii In the present status pull out the flow cell unit see Fig 5 2 will be indicated at FL on the 1st monitor screen 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 1 Xe 5 14 ...

Page 576: ...tor screen appears 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 550 350 1 Xe vi In this status place a paper strip at the Ex beam exit center of the sample compartment as shown in Fig 5 9 and observe the condition of the excitation beam Repeat the VERTICAL HORIZONTAL and FOCUS adjustments in this order little by little until the excitation beam rainbow color becomes brightest The coarse adjust...

Page 577: ...erving the data Take the procedure given below refer to sections 3 1 1 3 1 4 i Re mount the flow cell unit ii Press the WL key and the wavelength setting screen appears Set an excitation Ex wavelength Wavelength setting screen Ex indicated Ex Em 200 850 0 350 350 Press numeric keys 3 5 0 and then the ENT key iii Emission Em wavelength will not be set here Leave the present setting as it is 5 16 ...

Page 578: ...his value is maximum When a maximum value is reached the fine adjustment of the lamp position is completed vii Press U V or ESC key and the 1st monitor screen will return 4 Entry of Lamp Replacement Date When the above procedure is finished enter a lamp replacement date see 3 3 2 With this entry the cumulative on time is set to 0 and the number of lightings to 1 5 2 2 Hg lamp replacement Item to p...

Page 579: ...c Loosen the screw retaining the mercury lamp cover Fig 5 12 Hg lamp cover Retaining screw Fig 5 12 Removal of Hg Lamp Cover d Pull the Hg lamp cover straight out and the Hg lamp will be seen attached at the right side interior of the main body Fig 5 13 5 18 ...

Page 580: ... a new Hg lamp in place Fasten the lamp with the two retaining screws then connect the connector with the main body g Reattach the flow cell unit and light source cover in their original positions 2 Entry of Lamp Replacement Date When the above procedure is finished enter a lamp replacement date see 3 3 4 With this entry the cumulative on time is set to 0 and the number of lightings to 1 5 19 ...

Page 581: ...ord before proceeding to fuse replacement Item to prepare Item to prepare 2 new fuses P N J821349 T5A 1 Items to Check Prior to fuse replacement make sure the power switch of the instrument is off and the power cord is unplugged 2 Replacement of Fuse a Hold the tabs on both sides of the fuse holder and detach the holder Tabs Fuse holder Fig 5 14 Fuse Replacement b Replace two fuses with new ones t...

Page 582: ...ter 2 5 ERROR IN 2 2 Error Messages 4 33 ERROR OUT 2 2 ESC Escape 2 5 F FOCUS 5 12 Fastening between Component Units APPENDIX1 15 Flow Cell Check and Washing 4 24 Flow Cell Disassembly 4 26 Flow Cell Leakage 4 29 Fluorometry Notes on Handling Samples That Contain a High Concentration of the Compound of Interest 2 12 Fluorometry Advantages of Fluorometry 2 8 Fluorometry An Example of a Fluorescence...

Page 583: ... Fluorometry Temperature Dependency of Fluorescence Intensity 2 15 Frequency APPENDIX1 2 Fuse Replacement 5 20 G GLP 2 4 3 17 4 22 H Hg Lamp Replace 5 17 HORIZONTAL 5 12 HOLD 3 30 I INSERT 3 33 Installation APPENDIX1 1 Installation Conditions APPENDIX1 2 Installation Place APPENDIX1 5 Installation Unpacking APPENDIX1 1 L LAMP 4 1 LAMP OFF IN 2 2 LCD 3 1 LED 3 2 LOCK OFF 2 5 LOGBOOK 4 22 M MARKER 2...

Page 584: ...down Procedure 3 7 Power Supply voltage APPENDIX1 2 PROCESSOR option 2 3 PROG 2 4 Power consumption 2 19 R Raman Scattering 2 11 Raman Signal Intensity Measuring 4 9 Raman Spectrum of Water Measuring 4 3 READY BUSY OUT 2 2 Rear Panel 2 2 RECORD 2 5 RECORDER option 2 3 RECORDER Background Spectrum 3 43 S Sample Pretreatment 3 65 Sensitivity Check of Sensitivity 4 2 SET UP 2 4 Specifications 2 17 SP...

Page 585: ...on 2 1 UTILTY Utility 2 4 V VERTICAL 5 12 W WL Wavelength 2 4 Wavelength Accuracy Checking by using Hg Lamp 4 2 4 21 Wavelength Calibration of Wavelength Accuracy 4 17 Wavelength Setting 3 6 Wiring Arrangement APPENDIX1 10 X Xenon Lamp Positional Adjustment 5 12 Xenon Lamp Cool Down 5 3 Xenon Lamp Replacement 5 3 6 4 ...

Page 586: ... installation at the time of delivery For ensuring safety and high accuracy in operation of the instrument installation of the instrument shall be carried out by qualified service personnel trained by the manufacturer or its authorized maintenance service agent Before installation however the user shall make adequate preparations for installing the instrument referring to this instruction manual I...

Page 587: ...ore for the total system The total system shown comprises Chromaster organizer Chromaster 5110 pump Chromaster 5210 column oven and Chromaster 5440 fluorescence detector Check and prepare a power supply meeting the power supply requirements for your actual system configuration and OA equipment to be used in combination Power outlet A power outlet shall be available near the installation position o...

Page 588: ...nded 3P table tap or a 3P to 2P adapter In this case be sure to provide a proper grounding connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 mm 2 Ground Terminal Shall have a grounding construction for a ground resistance of 100 Ω or less a Ordinary Grounding Connection Grounded 3P powe...

Page 589: ...wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm b 1 With 2P Power Outlet Connection Rear panel Copper plate 300 mm 2 mm 10 mm Ground terminal Power outlet having a ground terminal 3P to 2P adapter Chromaster 5440 fluorescence detector Connector Rear panel Ground wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm b 2 With Power Outl...

Page 590: ...ter 5440 fluorescence detector stacked in two blocks are included Check and prepare an installation place satisfying the space requirements for your actual system and OA equipment to be used in combination 4 Installation Environment The following environmental conditions must be satisfied 1 Operating Ambient Temperature Within a range of 4 to 35 C And temperature variation should be minimum during...

Page 591: ...gh frequency furnace pole transformer etc f Protect the instrument from excessive dust Dust would degrade the performance g Connect the instrument to a line that is free from abrupt voltage fluctuations Such would increase the detector noise h If a motor driven apparatus such as stirrer or vibrator not having a noise suppressing device is connected to the same power line as this instrument avoid f...

Page 592: ...ewdriver Transport screw 1 For the instrument fixing Transport screw 2 For the instrument fixing Transport screw 3 For lamp house fixing Appended Fig 1 3 Removal of Transport Screws 2 Pull out the lamp house from the instrument see to in section 6 2 1 2 3 A transport screw is installed in the lamp house Remove the transport screw with the phillips screwdriver APPENDIX 1 7 ...

Page 593: ...lamp house And mount it to the instrument see to in section 6 2 1 2 5 Adjust the position of the xenon lamp The xenon lamp position had drastically moved to the downward of the vertical direction to fix the transport screws For this reason adjust VERTICAL first see section 6 2 1 3 NOTE After removing the transport screws please store them APPENDIX 1 8 ...

Page 594: ...pended Fig 1 5 Power Cable Connection Diagram Appended Table 1 1 Cables to be Used Connector cable 1 P N 892 6909 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 5 P N 892 6914 separately available Connector cable 6 P N 892 6913 separately available AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer an...

Page 595: ...ed to connect the e Line cable between the instruments On the left rear of each instrument insert the e Line cable into the e Line connector e Line connector Rear side of the instrument Appended Fig 1 6 e Line Connector on the Rear of Instrument APPENDIX 1 10 ...

Page 596: ...romaster 5210 autosampler Interface control board e Line cable 1 e Line cable 2 Chromaster organizer Chromaster 5110 pump Appended Fig 1 7 e Line Cable Connection Appended Table 1 2 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 892 6107 attached to autosampler fluorescence detector and interface control PC board APPENDIX 1 11 ...

Page 597: ...310 column oven Chromaster 5210 autosampler Drain Column Injection valve Wash pump Detector cell Appended Fig 1 8 Isocratic System Connect the inlet tube of the mobile phase container to the IN port of the degassing unit Connect the OUT port of the degassing unit to the inlet of the pump Connect the drain valve of the pump to port 1 of the injection valve of the autosampler Connect port 2 of the i...

Page 598: ...inlet tube of the mobile phase container to the IN port of the degassing unit Connect the OUT port of the degassing unit to the IN port of the proportioning valve Connect the OUT port of the proportioning valve to the four way joint Connect the mixer of the pump to port 1 of the injection valve of the autosampler Connect port 2 of the injection valve to the column inlet Connect the column outlet t...

Page 599: ... stacking module units in two blocks Appended Table 1 3 Drain Tubes to be Used Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 1 2 P N 893 2872 attached to autosampler Drain tube A1 3 P N 893 2872 attached to organizer Drain tube 1 P N 080 3090 attached to autosampler Drain tube 2 P N 080 3090 separately available T joint P N 810 1362 attached to organizer T joint N1 P N 890 3493 at...

Page 600: ... CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over When installing the instrument provide a proper means for fastening between module units On the rear of each module unit a cabling cover is attached The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers Fastening plate Fastening screw Append...

Page 601: ...the time of delivery For ensuring safety and high accuracy in operation of the instrument installation of the instrument shall be carried out by qualified service personnel trained by the manufacturer or its authorized maintenance service agent 1 Turn off the power to the instrument 2 Remove the inlet tube connected to the bulkhead union of the standard flow cell 3 Loosen the retention screws to r...

Page 602: ...gnals that are input and output via 3 pin connector Their names and functions vary with the unit A name that indicates the function is given at each connector Example of output contact signal EVENT of pump Example of input contact signal LAMP OFF IN of detector 2 Contact Signals Entering the e Line Connector Each unit has two e Line connectors for connection at the rear of the main unit and the si...

Page 603: ...s Use the e DIO cable 890 6145 for connection ERROR STOP START e Line connector To L 2000 series instrument To Chromaster series instrument e Line connector BUSY 3 pin connector e DIO cable 890 6145 e DIO cable 890 6145 APPENDIX 2 2 ...

Page 604: ...e 890 6146 for connection D 2500 START COM EXTERNAL H L G START BUSY e Line connector To Chromaster series instrument H L BUSY Connect the START L and G terminals of the e DIO cable 890 6146 to the EXTERNAL COM terminal of the Model D 2500 APPENDIX 2 3 ...

Page 605: ...utput Terminals These are contact signal input terminals for control using contact signals of an external unit The output circuit is shown in Fig 4 The rating of contacts used is 12 V 0 1 A Make sure the load connected does not exceed this rating e Line cable Other unit Chromaster series unit A Chromaster series unit B Fig 1 e Line Cable Connection 5 V 320 Ω IN Max 10 mA unit Max 0 1 A OUT 4 7 kΩ ...

Page 606: ...rting contacts of external unit Fig 3 Contact Signal Input Circuit Fig 4 Contact Signal Output Circuit Chromaster series unit External unit Max 10 mA 0 1 A max 1 2 3 30 V max 1 2 3 Chromaster series unit External unit APPENDIX 2 5 ...

Page 607: ...ey Lock This protective function prevents an erroneous key input during operation of the instrument GLP The confidence function is used to check the status of instrument Fluorescence A kind of luminescence which is emitted from a sample when a stimulating excitation beam is given to it Emission Fluorescence intensity Unit of fluorescence Relavive intensity Emission Fluorescence wavelength A partic...

Page 608: ... a filter is used to remove or cut off the 2nd order scattered light Full scale Used to determine the magnitude of output to such an external device as data processor chromato integrator Processor The terminal for analog output to the data processor Flow Cell Contains a sample for measurement Photomultiplier Used to detect fluorescence emission Marker in The external contact signal can be input to...

Page 609: ...ndicates a cumulative total time of lamp turn on periods Ex Excitation wavelength Used for exciting a sample Recorder RECORDER Used for analog output to a recorder Logbook Means the information containing records of instrument operating conditions Utility Used to set up operating conditions of the instrument APPENDIX 3 3 ...

Page 610: ...en Chromaster 5210 Autosampler Drain Chromaster 5440 FL Detector Syringe valve Injection valve Wash pump Detector cell Inlet tube 0 25 ST 0 33 TT 0 25 ST 0 25 ST 1 5 TT 1 5 TT Chromaster Organizer 2 Low Pressure Gradient System Mobile phase Wash fluid Chromaster Organizer Degassing unit Chromaster 5440 FL Detector Chromaster 5310 Column Oven Drain Syringe valve Injection valve Wash pump Detector c...

Page 611: ...tructions in this manual and the WARNING CAUTION labels on the instrument Keep this manual in a safe place nearby so it can be referred to whenever needed 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 3rd Edition June 2011 Copyright C Hitachi High Technologies Corporation 2011 1st Edition 2011 All rights reserved Printed in Japan Part No 892 9320 2 HH R RG HMS ...

Page 612: ... party in any form or by any means without the express written permission of Hitachi High Technologies Corporation 3 Hitachi High Technologies Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 613: ...would result not only in wrong analytical data but also in consequences adverse to safety Note that it is allowed only for persons having a basic knowledge of chemical analysis procedures to use this instrument Carefully read this instruction manual before attempting operation For proper use of the software please acquaint yourself with it The liquid chromatograph system comprises a pump unit for ...

Page 614: ...Column Oven Section 2 FUNCTIONS Name and Function of Each Column Part Specifications Section 3 OPERATION Basic Operation UTLTY Setting GLP and Preparation Section 4 MAINTENANCE INSPECTION Performance and Specifications Check Section 5 PARTS REPLACEMENT Consumables and Spare Parts Section 6 INDEX APPENDIX1INSTRATTION APPENDIX2Description on Contact Signal Communication APPENDIX3Terminology First of...

Page 615: ...e of Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be available in origina...

Page 616: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 617: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Technologies does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Technologies or its related companies or application of said instrument Installation Re...

Page 618: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 619: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 620: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 621: ...affected by electromagnetic noise within the permissible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power devi...

Page 622: ...word NOTICE or NOTE is used to indicate precautionary instructions concerning possible property damage NOTICE Used to indicate a potentially hazardous situation which if not avoided will or can result in damage to user s property serious damage to the instrument damage to data or environmental pollution though personal injury may not be incurred NOTE Used to indicate explanatory information for en...

Page 623: ...tric shock or fire Radiation from the Laser Light Source WARNING The internal CD ROM or CD R W drive of the PC is provided with a laser beam source In normal operation of the PC containing the laser beam source no laser beam harmful to human health will be emitted outside Note however that if a laser beam leaking out of the PC accidentally gets into the eye eye injury could occur When using the PC...

Page 624: ...r waste solution Leakage of solvent inside the instrument Section 2 3 3 6 When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution employ and provide proper grounding connection to it Section 2 3 3 6 Explosion of Vapor from Flammable Chemicals If a flammable chemical such ...

Page 625: ...esult in an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet b If a grounded 3P power outlet is not available use a grounded 3P table tap or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 m...

Page 626: ...eration This instrument is designed in conformity with the specifications of Class I in Annex H of the IEC 61010 1 International Electrotechnical Commission Standards Issue 1 To prevent an electric shock hazard provide a proper grounding connection a Be sure to use the grounded 3P power cable which is supplied as a standard accessory for the instrument The use of a different type of power cable ma...

Page 627: ...rence to actual parts Periodically check the appearances of these warning labels to see if they are clean to allow easy reading over a safe distance If any one of the warning labels becomes illegible due to deterioration contact your local Hitachi High Technologies Corporation sales representative or service office of Hitachi High Technologies Corporation sales representative for replacement with ...

Page 628: ...SAFETY 7 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument Front View 2 Do Not Touch Hot Part 3 Explosion of Vapor from Flammable Chemicals ...

Page 629: ...mall Furthermore leakage of a highly volatile solvent may not be detected Be sure to check for liquid leakage regularly to prevent a possible serious accident regardless of whether the leak sensor is activated or not a In routine inspection of the instrument visually check for liquid leakage before attempting measurements b In periodic inspection of the instrument check that the leak sensor works ...

Page 630: ...TY SUMMARY NOTICE precaution Continued Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally If necessary conduct measurement on a control sample ...

Page 631: ...1 General Safety Precautions SAFETY 2 WARNING Precautions in the Manual SAFETY 3 CAUTION Precautions in the Manual SAFETY 5 WARNING and CAUTION Labels on Instrument SAFETY 6 NOTICE Precautions SAFETY 8 1 OUTLINE 1 1 1 1 Outline of Chromaster 5310 Column Oven 1 1 1 2 Configuration of Liquid Chromatograph System 1 3 1 2 1 Isocratic System 1 3 1 2 2 Low Pressure Gradient System 1 4 2 FUNCTIONS 2 1 2 ...

Page 632: ...s of Organic Solvents 3 25 3 6 3 Cautions on Static Electricity 3 29 3 7 Preparation 3 30 3 7 1 Degassing and Removing Dust from Mobile Phase 3 30 3 7 2 Degassing Mobile Phase 3 30 3 7 3 Removing Dust from Mobile Phase 3 33 3 7 4 Sample Pretreatment 3 34 4 Maintenance Inspection 4 1 4 1 How to Check the Specifications and Performance 4 1 4 1 1 Items to Prepare in Advance 4 1 4 1 2 Check of Tempera...

Page 633: ...eating Tubing APPENDIX 1 13 5 4 Assembling of Pre heating Tubing for Pre heating of 0 5 Line or of More Than 1 5 Line APPENDIX 1 15 5 5 System Tubing APPENDIX 1 17 5 6 GUI Controller APPENDIX 1 22 5 7 Fastening between Component Units APPENDIX 1 23 6 Assembling of Optional Component Part Switching Valve APPENDIX 1 24 6 1 Type APPENDIX 1 24 6 2 Tubing Connection of Switching Valve APPENDIX 1 24 7 A...

Page 634: ...within SD 0 2 C is attainable in the entire range of temperature control 3 Usable for Extensive Applications such as Method Development and Sample Concentrating Treatment The Chromaster 5310 can mount and control either 3 column selector valve or 6 way 2 position valve in an optional arrangement The Chromaster 5310 is also equipped with a time programming function for enabling a changeover in temp...

Page 635: ...e a stable peak retention time even if the ambient temperature varies and to minimize a dead volume for reducing possible peak diffusion Minimum preheating capacity 0 63 μL in use of piping 0 1 mm in diameter NOTE This instrument is designed on the presupposition that preheating is performed before analysis Be sure to carry out preheating before proceeding to analytical operation with this instrum...

Page 636: ...a separated component of the sample In addition a degassing unit for deaerating an eluent a gradient device for varying a mixing ratio of eluents with time and other optional devices are incorporated in the system 1 2 1 Isocratic System The isocratic system has a simple configuration in which single solvent analysis is performed Fig 1 1 Isocratic System Chromaster 5110 pump Chromaster 5310 column ...

Page 637: ...from which a liquid feed is performed by a single pump The composition of an eluent is made to vary with time in chromatographic separation In the low pressure gradient system two or more solvents are mixed in its low pressure section from which a liquid feed is performed by a single pump The composition of an eluent is made to vary with time in chromatographic separation Wash fluid Fig 1 2 Low Pr...

Page 638: ... mixed at a pre specified ratio 3 Through the mixer the mixture eluent is delivered 4 A sample is injected by the autosampler 5 The injected sample is separated through the column which is maintained at a constant temperature by the column oven 6 Each component separated from the sample is detected as a signal by the detector 1 5 ...

Page 639: ...ont door R L allows you to access an internal space that protected with a black cover UI pad A keypad to be used for stand alone operations option LED Four LED indicators are equipped Shown below are LED status indications Table 2 1 LED Status Indications Name LED Status OVEN Blue POWER ON Orange ERROR CONTROL Blue Temperature control under way by Peltier element READY Blue Temperature ready PROG ...

Page 640: ...is fixed with four tabs Inside cover fixing tab It locks the inside cover For unlocking the cover slide two upper side tabs downward and two lower side tabs upward Drain tray A drain pan for liquid leakage Liquid leak sensor A sensor for detecting liquid leakage Main power switch Fig 2 3 Right Side Panel Main power switch Main power switch of Chromaster 5310 column oven 2 2 ...

Page 641: ...ee terminals Power connector For connecting the power cable Analog output connector A connector for analog output of a temperature indication Two kinds of output temperature indications are selectable oven temperature indication and environment room temperature indication e Line connector A connector for e Line connection between instrument units in the Chromaster series 2 3 ...

Page 642: ... control The UI pad is ineffective when either chromatography data station or a GUI controller option is connected with this column oven Description is given for each key on the optional UI pad control panel 7 6 1 9 2 3 4 5 8 Fig 2 5 Control Panel of UI Pad for Column Oven NOTE If a mistake has been made during operation click the ESC key In most cases the initial status will return upon clicking ...

Page 643: ...ing whether or not to use the optional selector valve SET UP 2 Clicking this together with key opens the SETUP screen Hold key down until SETUP screen appears Used to select GLP information 1 Indicates number of selections of option selector valve and sets valve seal replacement date 4 GLP 2 Sets the key lock 2 Key lock is released by clicking ESC key 5 INSERT set program 1 For selecting and setti...

Page 644: ...the DEL key the is displayed and the process is registered by pressing the ENT key 11 clear If a mistake is noticed before clicking ENT key after numerical or decimal input clear the entry with this key and displays the cursor in the beginning of the entry field The previous input value is displayed as a setup value 12 enter Registers the entered parameters 13 arrow Used to select monitor indicati...

Page 645: ...temperature ready status Parameters settable are Tolerance and Wait Time and when the measured temperature of the oven is maintained within the set temperature tolerance during the wait time the temperature ready status is assumed See Fig 2 6 Temperature C Time min Set temperature Wait time Set temperature tolerance Temperature busy status Temperature ready status Fig 2 6 Temperature Control 2 7 ...

Page 646: ...n due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemicals If a flammable chemical such as organic solvent leaks from the flow path of the instrument and its vapor concentration exceeds the explosion limit it may cause spontaneous combustion...

Page 647: ...re control of the column oven is halted Upon detection of a leak error the buzzer sounds for five seconds After this the buzzer will stop but the error will not be reset until the CL key is clicked NOTE 1 The detection sensitivity of the leak sensor varies with the kind of solvent An organic solvent whose vapor pressure is low might not be detected so a visual check should be made for leakage 2 Th...

Page 648: ...ient temperature 2 0 C in the range of 4 to 35 C 5 Temperature Control Precision SD 0 2 C measured at the specified point in the oven 6 Safety a Overheat preventing mechanism by means of a thermal protector 105 C b Organic solvent vapor leak sensor Temperature control is forced to stop upon detection of leakage of organic solvent vapor Leak detection level setting is allowed c Door sensor Temperat...

Page 649: ...ROR IN level ERROR OUT level START IN pulse or start up External output Analog temperature output 100 C V Output voltage mV Indicated temperature C 10 9 6 Two kinds of temperature sensors oven temperature ambient temperature are selectable 14 Time Program a Setup items i Temperature setting ii Selector valve position changeover b Number of programs Up to nine programs c Setting time Up to 600 minu...

Page 650: ...lector valves One of the following two kinds of optional valves is selectable i 3 column selector valve Model RV500 100 IDEX Health Science LLC USA Wetted part SUS316 PEEK Pressure tightness 35 MPa Solvents not allowed Concentrated sulfuric acid and concentrated nitric acid are not applicable ii 6 way 2 position valve Model RV700 100 IDEX Health Science LLC USA Wetted part SUS316 PEEK Pressure tig...

Page 651: ...g with the display monitor in the same posture for long hours your eyes and body will be fatigued When working with the display monitor for a long time take a break for 10 to 15 minutes per hour for health of your eyes and body NOTE Prior to connecting a new column make sure to fill the flow path with a mobile phase so that air won t enter the column 3 1 ...

Page 652: ...n to turn on the power supply 3 At the start LCD indicates startup screen After a few seconds initial screen will be indicated and an initialize processing test is executed simultaneously LED indicates OVEN in blue light a Startup screen Column Oven 8928130 00 C Hitachi High Technologies Corp 2010 Initializing self testing and indicating a copyright are performed The program No and version will be...

Page 653: ... is 0 Description of status indication at upper right of monitor screen I Oven temperature is in ready status R Run status Time program is running B Oven temperature is in busy status L Keyboard is locked Status other than above temp control stopped c 2nd Monitor Screen Ambient Temperature Indication 25 0 1 TEMP AMBIENT VALVE 1 Indication Description AMBIENT Indication of ambient room temperature ...

Page 654: ...on of selector valve option indicated if valve is not connected PROG Time program number Refer to 6 for the description of status indication at upper right of monitor screen e Monitor Screen Changeover TEMP MONITOR SET READY RANGE WAIT 25 1 40 39 5 40 5 5 0 1st monitor screen oven temperature indication TEMP AMBIENT VALVE1 25 0 1 2nd monitor screen ambient temperature indication TIME MONITOR SET V...

Page 655: ...Single numeric PROGRAM NO 1 9 1 Parameter name Input range Input field b Plural numeric VALVE1 SEAL CHANGE MM DD YYYY 1 12 Parameter name Input range Input Item Input field c Numerical selection UTILITY LEAK SENSOR 1 ANALOG OUT 2 1 ERROR OUT 3 CALIBRATION 4 Parameter name Selection item Input field d Program setup screen TIME TEMP VALVE1 1 Input Item Input field 3 5 ...

Page 656: ...put value and waits for retype Press the ESC key to return to the initial screen monitor screen Even if the ESC key is pressed during input the inputting parameter won t be renewed NOTE When turning on the power supply default numbers are indicated in the selection item When the CL key is pressed in the input field indication in the field is deleted and the cursor returns to the first character in...

Page 657: ...t are entered and ENT key clicked on the temperature setting screen the settings will not be updated 2 The temperature upper limiter should normally be set at 70 C or higher except for a special reason If the limiter were erroneously set near the ambient temperature then a temperature limiter error may be caused by ambient temperature fluctuation 3 If a temperature upper limiter error occurs the t...

Page 658: ...y clicked on the temperature ready condition setting screen the settings will not be updated 2 If NO is selected for USE TOLERANCE the temperature ready status is provided regardless of the current oven temperature TOLERANCE C WAIT TIME min 0 1 9 9 1 0 5 TOLERANCE C WAIT TIME min 0 99 1 0 5 Set a tolerance range 1 0 ENT Set a wait time 5 ENT Monitor screen USE TOLERANCE YES 1 NO 0 0 Specify whethe...

Page 659: ...able unless the selector valve setting has been made 2 For use of the 3 column selector valve the allowable input range is 1 3 For use of the 6 way 2 position valve the allowable input range is 1 2 Valve type is recognized according to the actual instrument configuration 3 1 6 Closing Operation Carry out the closing operation of Chromaster 5310 column oven 1 Press the power switch to turn off the ...

Page 660: ...OG OUT 2 1 ERROR OUT 3 CALIBRATION 4 SELECT SENSOR GAS 1 LIQUID 2 1 LEAK GAS MONITOR 1 SET LEVEL 2 1 SENSOR MONITOR ALARM LEVEL 400 1200 Monitor screen SET ALARM LEVEL 0 4095 1200 Monitor screen 1 ENT 1 ENT Monitor the gas leak sensor output 1 ENT 2 ENT SET UP UTLTY ENT or ESC key Set up a gas leak detection level 1200 ENT initial value 1200 3 10 ...

Page 661: ...ctuates largely from this range then the threshold must be adjusted 3 Since the leak sensor output is unstable for about five minutes after turning ON the power switch leak detection cannot be made during this while 2 Set the ON OFF status of the liquid leak sensor ON status or use of the leak sensor is set immediately after turning on power supply again SET UP UTILITY LEAK SENSOR 1 ANALOG OUT 2 1...

Page 662: ...n the rear of the instrument Output temperature conforms to the relational expression given below Temperature C output voltage mV 9 6 10 SET UP UTLTY 2 ERROR OUT 3 CALIBRATION 4 ANALOG OUTPUT TYPE OVEN 1 AMBIENT 2 Select an output temperature 1 ENT Monitor screen 1 2 ENT UTILITY LEAK SENSOR 1 ANALOG OUT 2 3 12 ...

Page 663: ... Monitor screen SET UP UTLTY NOTE Error contact output will always be issued regardless of the setting of ERROR OUT contacts for only leak error occurrence 3 2 4 Setting of Temperature Calibration If there is a deviation between the indicated temperature of the Chromaster 5310 column oven and the actual temperature the deviation can be corrected by setting for temperature calibration For instance ...

Page 664: ...on 0 5 ENT SELECT MODE OFFSET 1 OFFSET 2 1 OFFSET C 1 0 Present setting is indicated SET UP UTLTY NOTE 1 For conducting temperature calibration be sure to use a calibrated thermometer for measuring temperature 2 There is a slight difference between the set and actual temperatures depending on the temperature setting In temperature calibration it is recommended to determine the deviation at the set...

Page 665: ...This function serves to lock the keys on the keyboard and thus prevent erroneous activation of keys on the control panel GLP GLP LOGBOOK 1 KEY LOCK 2 2 KEY LOCK YES 1 NO 0 1 2 ENT 1 ENT Monitor screen Clicking the ESC key releases the keylock LOCK OFF 3 15 ...

Page 666: ...n Carry out setting for the logbook in which maintenance information is recorded 2 ENT VALVE1 SEAL CHANGE MM DD YYYY 2000 2100 9 1 2010 VALVE1 SEAL CHANGE MM DD YYYY 1 12 _9 1 2010 Enter the month when v seal was replaced 6 ENT alve VALVE1 SWITCHING LAST CHANGED DATE 23 times 9 1 2010 Monitor screen ENT or ESC key Check the logbook information 1 ENT Enter the day when valve seal was replaced 2 ENT...

Page 667: ...TIME TEMP VALVE1 EVENT _ 1 Enter a time program number 1 ENT Select a mode MODIFY For editing an existing time program NEW For deleting an existing time program and creating a new one 0 ENT Indicates the number assigned to the time program being edited Time setting Enter a preset time ENT Temperature setting Enter a preset temperature 40 ENT Valve setting 2 ENT PROG New step For the 2nd step onwar...

Page 668: ...ming although a temperature level can be changed a temperature rising time cooling time cannot be specified Table 3 1 Key Function in Time Program Editing No Key Function 1 Goes to the next step or back to the previous step 2 set program insert Inserts a new step 3 LOCK OFF CL escape lock off Returns to the monitor screen 4 CL clear Clears an input numeric value 5 DEL delete Deletes each step PR G...

Page 669: ...zed SET UP SETUP VALVE1 CONTRAST S NO NO USE 4 02AB 111 USE VALVE NO USE 0 VALVE USE 1 1 SETUP ITEMS USE VALVE 1 1 CONTRAST 2 SETUP VALVE1 CONTRAST S NO USE 4 02AB 111 POWER ON SETUP monitor screen ENT key Specify whether or not to use an optional selector valve 1 ENT Specify which valve is to be set 1 ENT ENT key Turn power on again UTLTY 3 19 ...

Page 670: ...procedure shown below LCD CONTRAST 1 7 1 SETUP VALVE1 CONTRAST S NO USE 4 02AB 111 SETUP ITEMS USE VALVE 1 1 CONTRAST 2 SETUP VALVE1 CONTRAST S NO USE 4 02AB 111 POWER ON SETUP monitor screen ENT key Specify an LCD contrast level 2 ENT ENT key 1 ENT Turn power on again SET UP UTLTY 3 20 ...

Page 671: ...ality is found stop operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemical...

Page 672: ... Table 3 3 Characteristics of Organic Solvents 2 When performing high sensitivity analysis with a UV detector use solvents whose UV absorption characteristics are especially small Use solvents for liquid chromatograph commercially available Absorption characteristics of special grade reagents such as methanol ethanol and acetonitrile generally and widely used are greatly different in the short wav...

Page 673: ...gen ions such as HCl KCl NaCl NH4Cl are typical reagents Reagents which may be restricted are shown in Table 3 2 use the table as a rough standard NOTE When unsuitable reagents absolutely necessary for ingredient separation or reaction of a constituent have been used or when mobile phase which deposits salt has been used wash all the flow paths with distilled water after completing analysis withou...

Page 674: ...perchlorate Ammonium phosphate Boric acid Formic acid up to pH3 Hydrochloric acid up to pH3 Potassium nitrate Sodium hydrogencarbonate Sodium carbonate Ammonium chloride Potassium chloride Sodium chloride Tolufluoroacetic acid Note 1 Max concentration of above reagents should be 5 6 Note 2 When the above reagents have been used necessarily wash all the flow paths with distilled water completely wi...

Page 675: ...f an abnormality is found stop operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammab...

Page 676: ...flammation or injury For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper protective clothes e g safety goggles so that a solvent will not come into direct with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor 3 26 ...

Page 677: ... 368 1 378 1 496 1 389 1 525 1 501 1 424 1 353 1 442 1 443 1 424 1 394 1 408 1 445 1 381 1 400 1 359 1 422 1 370 1 362 1 410 1 586 1 387 1 394 1 344 1 510 1 38 1 361 1 329 1 427 1 372 1 333 210 210 210 210 210 210 210 380 265 225 220 290 220 225 285 225 280 220 290 245 245 330 220 230 330 380 220 260 260 210 275 380 210 305 220 210 210 210 210 40 21 7 46 1 20 17 8 30 12 8 9 4 o 17 2 m 25 p 25 27 8...

Page 678: ...bile phase Use solvents whose boiling point is 55 C or higher Solvents of low boiling point are not only dangerous but also generate bubbles when sucked by pump so that normal pumping will be impossible 3 When performing high sensitivity analysis with UV detector use solvents which absorb especially small amount of UV light Since special grade reagents such as methanol and acetonitrile generally u...

Page 679: ...nductive container for waste solution and provide proper grounding connection to it Since flammable organic solvents are used for the High Speed Liquid Chromatograph be careful about heat and fire Since thin tubings are used for the liquid chromatograph static electricity is easily generated If charged liquid is collected into an insulated waste container for example and an electric discharge occu...

Page 680: ...y bubbles d Variation of pump pressure e Reduced precision of gradient mixing ratio 2 For degassing mobile phase two methods are available Degassing unit and Manual Degassing method is explained in 4 8 2 3 Use mobile phase without dust Dust in mobile phase causes trouble in pumping and the pressure may vary 3 7 2 Degassing Mobile Phase There are various ways of degassing Perform degassing suitable...

Page 681: ...sonic cleaner c When degassing small bubbles are generated first then gradually larger bubbles are generated Continue degassing until bubbles are not generated anymore It takes 5 to 10 minutes to finish d When bubble generation finishes turn off the power of ultrasonic cleaner e Take out mobile phase container from ultrasonic cleanser wipe the water from the container and set the container to liqu...

Page 682: ...r drift of baseline may be caused NOTE Degas mobile phase of aqueous solution by using both ultrasonic cleaner with water and aspirator to decrease pressure Fix the degassing time b Insert rubber tube of aspirator into mouth of reagent bottle c Turn on the power of ultrasonic cleaner d Open the faucet of city water for aspirator to decrease pressure e When degassing small bubbles are generated fir...

Page 683: ...bile phase may be varied by the degassing time boiling point of mobile phase would vary with a reduced pressure 3 7 3 Removing Dust from Mobile Phase There are various ways to remove dust from mobile phase Remove dust in the way suitable for the purpose of use 1 Example of Filtering of Mobile Phase by Using Membrane Filter Removing dust and degassing can be performed simultaneously by filtration w...

Page 684: ...nto a syringe attach cartridge type 0 45 μm membrane filter and perform filtering See the figure at left NOTE There are various ways of filtering sample Filter the sample in the way suitable for the sample amount Filtering by cartridge type 0 45 μm membrane filter Filtered clean sample b Example of Removing Foreign Matter from Sample For example when analysis is performed with a reversed phase col...

Page 685: ...3 7 4 NOTE There are various ways of removing foreign matter from sample Remove in the way suitable for the purpose of analysis Cartridge of silica gel Clean sample after removing foreign matter 3 35 ...

Page 686: ...d item or an equivalent product Thermometer one that is calibrated and able to measure down to 0 1 C Recorder Micro syringe for 50 μL Methanol 4 1 2 Check of Temperature Control Operation Check in the following procedure whether the Chromaster 5310 column oven is controlled to the set temperature 1 Set the oven temperature to room temperature or 25 C 2 After the oven stabilizes at the set temperat...

Page 687: ...ucted below 1 Set the oven temperature to 40 C 2 After the temperature stabilizes at 40 C aspirate 50 μL of methanol with the micro syringe and inject the methanol into the oven through the piping connection opening Specification A gas leak error should be indicated properly NOTE 1 Even if the sensor output exceeds the threshold a gas leak error will not appear on the gas leak sensor monitor scree...

Page 688: ... Leak Sensor Drip about 0 5 mL of water on the liquid leak sensor Drip water Leak sensor Fig 4 1 Leak Sensor Mounting Position NOTE When using the liquid leak sensor the instructions given below should be followed a When a solvent is used turn on the liquid leak sensor function b The liquid leak sensor may not detect a drop of leakage or high volatile solvents Always check the leakage even while t...

Page 689: ...y b Wipe moisture off the leak sensor and drain tray and then fasten the sensor to the drain tray again NOTE Be careful not to damage the tip of the leak sensor during its cleaning If damaged the leak sensor may not function normally or an error may be caused Leak sensor fastening screw Fig 4 2 Leak Sensor Fastening Screw NOTE Please install the liquid leak sensor in the correct position Otherwise...

Page 690: ... Chromaster 5310 column oven to remove an inside cover 2 Remove the two screws which fasten the preheat plate at the center using the furnished hexagonal wrench and fasten the protective tube of the temperature sensor by placing it between the preheat section and preheat plate Protect tube 300 mm long Fig 4 3 Temperature Sensor sketch Temperature sensor position Preheat plate screw Preheat plate P...

Page 691: ... measured accurate temperature data may not be attained 3 Attach the inside cover And before closing the front door of the column oven run the wires of the temperature sensor through the piping connection opening 4 Set the terminal of the thermocouple to the thermometer and set the column oven temperature to 40 C 5 When the column oven temperature indication has stabilized measure the thermocouple...

Page 692: ... of the preceding section for checking the temperature setting accuracy and connect the thermometer output to a recorder 2 Set the column oven parameters as follows Temperature setting 40 C Tolerance range 1 0 C Wait time 20 min 3 Once the READY LED comes on output the oven temperature to the recorder for 10 minutes Specification Variation width of oven temperature over 10 minutes should be within...

Page 693: ... despite there being no leakage then the alarm level of the gas leak sensor must be adjusted Carry out the adjustment in the procedure given below NOTE 1 A gas leak error won t occur even if the sensor output exceeds the alarm level on the gas leak sensor monitor screen And since the sensor output is unstable for about 5 minutes after turning ON the power switch gas leak detection is not made duri...

Page 694: ... detection threshold When a gas leak error occurs open the front door and wipe up all the leaked liquid before reusing the instrument The detection sensitivity of the gas leak sensor varies with the solvent see Fig 4 5 If a gas leak is not detected at the occurrence of a leak with the solvent being used or if a gas leak error occurs frequently try adjusting the alarm level in the aforementioned wa...

Page 695: ...he indicated temperature of the column oven is 40 0 C then set a value of 0 5 C offset value for correcting the difference NOTE 1 For temperature calibration be sure to measure temperature with a calibrated thermometer 2 Difference from the actual temperature will vary somewhat with the temperature setting For the temperature calibration it is recommended to use the most frequently employed temper...

Page 696: ... setting in time program 8 TEMP CONTROL OFF BY EXTERNAL ERROR PRESS CL KEY TO CLEAR MESSAGE Temperature control has been stopped due to external contact input Press the CL key for clearing an error indication 9 TEMP CONTROL OFF BY LEAKAGE GAS PRESS CL KEY TO CLEAR MESSAGE 1 Solvent leaks from flow path in column oven 2 Solvent remains in oven 3 Alarm level of gas leak sensor is too low 1 Wipe up l...

Page 697: ...occurrence of temp upper limit error 1 Close the inside cover 2 Eliminate cause of error then reset error 3 Reset temperature and upper limiter 1 Front door is open 1 Close the front door 16 READY status not attained 2 Error has occurred 2 Eliminate cause of error then reset error 1 TOLERANCE setting is too low 1 Increase the TOLERANCE setting 17 Takes much time to attain READY status 2 WAIT TIME ...

Page 698: ... 4 Detach tubing from the valve section downward and locate faulty part 2 VALVE 1 ERROR 1 PRESS CL KEY TO CLEAR MESSAGE 1 Valve seal not attached correctly 2 Faulty operation of valve 1 1 Attach the seal correctly 2 Turn on valve power again and make sure the valve is changed over correctly 3 VALVE1 ERROR 2 PRESS CL KEY TO CLEAR MESSAGE Faulty operation of valve 1 control circuit board Turn on val...

Page 699: ...18005XP 893 0836 Pipe for Chromaster 5310 0 25mmI D 800 mm SUS 893 0825 Fitting PEEK For 1 16 inch OD 1 57 mm SUS tube 890 4175 Valve seal for 3 column selector stator rotor seal 6000 operations Option 893 0837 Pipe for AS to Valve Option common accessory for 3 column separator valve and 6 way 2 position valve 0 25 mm I D 900 mm SUS 890 4330 Pipe for Valve to Column Option common accessory for 3 c...

Page 700: ...on preheat pipe kit accessory For mobile phase flow rate 0 7 mL min 0 25 mm I D 500 mm SUS 893 3321 Pipe 1 0 Option preheat pipe kit accessory For mobile phase flow rate 1 5 mL min 0 25 mm I D 500 mm SUS 893 3322 Pipe 2 0 Option preheat pipe kit accessory For mobile phase flow rate 3 0 mL min 0 25 mm I D 500 mm SUS 893 3323 Pipe 3 0 Option preheat pipe kit accessory For mobile phase flow rate 3 7 ...

Page 701: ...eeding to fuse replacement 1 Item to Prepare New fuse P N J821349 Make sure to use a time lag fuse of the specified rating T5AL for 250 V 2 Check Items Make sure the power switch is OFF and the power cord is disconnected from the instrument prior to fuse replacement 3 Fuse Replacement a Detach the fuse holder by pressing the knobs at both sides Knobs C941322 Fuse holder Fig 5 1 Fuse Replacement b ...

Page 702: ... position valve with the hexagon wrench attached to the valve seals and then detach the stator and the stator seal 3 Remove four stator ring retaining screws with the hexagon wrench attached to the valve seals and then pull out the stator ring and the rotor seal 4 Replace the stator and rotor seals with new ones attach the seals in the order opposite to removal and fasten the stator ring retaining...

Page 703: ...5 2 2 Positioning pin Rotor seal Stator ring Stator ring retaining screw Stator seal Stator seal Stator retaining screw Fig 5 2 Replacement of Selector Valve Seals 5 5 ...

Page 704: ...put connector 2 3 Analog temperature output 3 12 Assembling APPENDIX1 8 B Burns SAFETY 5 C CL key 2 6 3 18 COND key 2 5 Cabling APPENDIX 1 11 Consumables 5 1 Corrosive solvent SAFETY 8 D Disposal of waste solution SAFETY 8 Drain 1 3 1 4 APPENDIX1 17 APPENDIX1 18 E ENT key 2 6 ERROR OUT 2 11 3 10 ESC key 2 5 3 18 Electric shock SAFETY 4 APPENDIX1 4 Error Out Contact 3 13 Explosion of Vapor from Fla...

Page 705: ...emicals by static electricity SAFETY 3 3 29 Installation space APPENDIX1 7 Instrument tipover SAFETY 5 Isocratic system 1 3 APPENDIX1 11 K KEY LOCK 3 15 Keylock 3 15 L LED 2 1 LOCK OFF key 2 5 LOGBOOK 3 15 3 16 Leak sensor 2 5 3 10 4 2 Liquid leak 4 3 4 7 Logbook 3 16 Low pressure gradient system 1 4 APPENDIX1 11 M MAX LIMIT 3 7 MONITOR 3 3 Monitor display screen 3 2 3 3 O OFFSET 3 14 6 2 ...

Page 706: ...recision SAFETY 9 R RANGE 3 3 Replacement of seals for selector valve option 5 4 Rotor seal 5 4 S SET 3 3 SET TMP key 3 7 SET UP key 2 5 Specifications 2 10 System cabling APPENDIX1 11 T Temperature busy status 2 7 Temperature calibration 3 13 4 9 Temperature control 2 7 Temperature control accuracy 4 7 Temperature control operation 4 1 4 7 Temperature ready status 2 5 3 8 Temperature setting 3 7 ...

Page 707: ...APPENDIX1 24 U UI pad 2 1 2 4 2 12 3 1 UTLTY key 2 5 3 10 Unpacking APPENDIX1 1 V VALVE key 2 5 VALVE1 SEAL 3 16 Valve seal 3 16 5 1 Valve seal for 3 column selector 5 1 Valve seal for 6 way 2 position valve 5 1 W WAIT 3 3 WARNING and CAUTION labels on instrument SAFETY 7 Wait Time WAIT TIME 2 7 3 8 Warranty on Product IMPORTANT 1 6 4 ...

Page 708: ...rer or its authorized service agent Before installation however the user shall make adequate preparations for installing the instrument referring to this instruction manual If relocation of the instrument becomes necessary after delivery consult your dealer or nearest Hitachi High Technologies service representative in order to avoid possible trouble involved in relocation 2 Place for Installation...

Page 709: ...hall be free from strong vibration or shock which can be felt by your body d Shall be free from a heating device such as gas burner electric heater or oven in the vicinity e Shall be away from strong electric field generating equipment such as electric welder high frequency electric furnace and pole transformer f Shall be free from excessive dust Otherwise performance degradation might be caused g...

Page 710: ...er 5310 column oven and Chromaster 5410 UV detector Confirm the necessary power capacity taking actual system configuration and OA equipment in the installation room into account and prepare a power supply having an adequate power capacity 4 Power outlet Power supply shall be obtainable near the place for installing the system inclusive of this detector This detector requires a single grounded pow...

Page 711: ...of a different type of power cable may result in an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet as a rule b If a grounded 3P power outlet is not available use a 3P table tap with a grounding wire or a 3P 2P adapter In this case be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or larger and a turn count of...

Page 712: ... attached to instrument Chromaster 5310 column oven Ground resistance 100 Ω or less 750 mm or more below ground Connector Rear panel Copper plate Grounding electrode underground section 300 mm Grounding construction f 100 Ω or less or 2 mm 10 mm Example of grounding electrode Appended Fig 1 1 Grounding Method APPENDIX 1 5 ...

Page 713: ...nt Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Chromaster 5310 column oven Connector Rear panel 10 mm 2 mm 300 mm b 2 With 2P power outlet having a grounding terminal Power outlet with grounding terminal Grounding terminal 2P 3P adapter Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Chromaster 5310 colum...

Page 714: ...cks becomes 100 mm If the clearance between the blocks is wider than 100 mm the length of DC power cable may become inadequate For installation prepare a level and sturdy bench which withstands a load of 150 kg or more The system conceived here is an example in which Chromaster organizer Chromaster 5110 pump Chromaster 5210 autosampler Chromaster 5310 column oven and Chromaster 5410 5420 5430 5450...

Page 715: ...master 5110 pump one Chromaster 5210 autosampler one Chromaster 5410 5420 5430 5450 detector and one IFC board can be connected For the Chromaster 5310 column oven and Chromaster 5440 fluorescence detector the power cord needs to be connected to the column oven unit If a single organizer is inadequate due to use of 2 detectors for example an AC adapter option that matches the detector concerned ne...

Page 716: ...le 1 P N 892 6909 attached to organizer Connector cable 2 P N 892 6910 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 4 P N 892 6912 attached to organizer AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster 5210 autosampler a...

Page 717: ...e Used Connector cable 1 P N 892 6909 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 5 P N 892 6914 separately available Connector cable 6 P N 892 6913 separately available AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster ...

Page 718: ...re Gradient System Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump e Line cable 1 e Line cable 2 Appended Fig 1 6 e Line Cable Connection Appended Table 1 3 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampl...

Page 719: ...Chromaster 5210 autosampler Interface control board e Line cable 1 e Line cable 2 Chromaster organizer Chromaster 5110 pump Appended Fig 1 7 e Line Cable Connection Appended Table 1 4 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampler fluorescence detector and interface control board APPENDIX 1 12 ...

Page 720: ...ferring to Table 1 shown below Preparation items Hexagon screw wrench P N N315004 Size B3 Pre heating section Appended Fig 1 8 Front Elevation View of Column Oven with the Door Open Appended Table 1 5 Relationships between Operating Flow Rate and Optimum Number of Lines to Be Used for Pre heating for SUS Tubing of 0 25 mm in Inner Dia Applied Range of Flow Rate mL min 0 7 or less 0 71 to 1 5 1 51 ...

Page 721: ...ch attached Appended Fig 1 9 Disassembling of Pre heating Plate 2 Prepare a tube of approx 800 mm long Excluding the portions on both ends 100 mm on the column side and 500 mm on the autosampler connected side install the remainder of the tube into the grooves in the pre heating base Column connected side 100 mm Pre heating base Groove Autosampler connected side 500 mm Appended Fig 1 10 Assembling...

Page 722: ... heating base with the tube not properly set may damage the tubing or lead to incorrect results 5 4 Assembling of Pre heating Tubing for Pre heating of 0 5 Line or of More Than 1 5 Line Where a flow rate at lower than 0 7 mL min is used set the tubing from the center of the pre heating section as shown in Appended Fig 1 11 below 0 5 line Column connected side 100 mm Set the tubing from the center ...

Page 723: ... as shown in Appended Fig 1 12 below When turning around install the tube to the next groove with one line of groove skipped Turn around with one line of groove skipped Appended Fig 1 12 Assembling of Tubing Where a Flow Rate at Higher Than 1 51 mL min Is Used APPENDIX 1 16 ...

Page 724: ...column and detector through the central hole of each module unit Drain receiver 1 Isocratic System Detergent Mobile phase liquid Chromaster organizer Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Chromaster 5110 pump Degassing unit Drain Injection valve Column Syringe valve Appended Fig 1 13 Tubing Diagram of Isocratic System stacked in o...

Page 725: ...m stacked in two blocks Connect the inlet tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the inlet of pump Connect the purge valve of pump to port 4 of the injection valve in the autosampler Connect port 5 of the injection valve to the inlet of column To the outlet of column connect the inlet tube of detector cell Connect the deterg...

Page 726: ...420 5430 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Low pressure gradient unit proportioning valve Chromaster 5110 pump Drain Degassing unit Syringe valve Injection valve Appended Fig 1 15 Tubing Diagram of Low Pressure Gradient System stacked in one block APPENDIX 1 19 ...

Page 727: ...et tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the IN port of proportioning valve Connect the OUT port of the proportioning valve in the low pressure gradient unit to the 4 way joint Then connect the purge valve of pump to port 4 of the injection valve in the autosampler Also connect port 5 of the injection valve to the inlet of ...

Page 728: ...for Drain when stacking module units in one block Appended Table 1 6 Drain Tubes to be Used Drain tube A2 P N 893 2874 attached to organizer Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 P N 893 2872 attached to organizer Drain tube 4 P N 893 2873 attached to organizer Drain tube P N 080 3090 attached to autosampler T joint P N 810 1362 attached to organizer T joint N1 P N 890 349...

Page 729: ...organizer Drain tube A1 1 2 P N 893 2872 attached to autosampler Drain tube A1 3 P N 893 2872 attached to organizer Drain tube 1 P N 080 3090 attached to autosampler Drain tube 2 P N 080 3090 separately available T joint P N 810 1362 attached to organizer T joint N1 P N 890 3493 attached to autosampler I joint P N 893 2876 attached to autosampler L joint P N L369125 attached to organizer 5 6 GUI C...

Page 730: ... instrument provide a proper means for preventing the instrument from tipping over accidentally On the rear of each module unit a cabling cover is attached The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers Fastening plate Fastening screw Appended Fig 1 19 Fastening between Component Units APPENDIX 1 23 ...

Page 731: ...n operation of the instrument installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its authorized service agent 6 2 Tubing Connection of Switching Valve Shown below is an example of the system tubing configuration of each switching valve 1 For 3 column Selector Valve Chromaster 5310 column oven Column 1 Column 2 Column 3 ...

Page 732: ...s as an automatic recording system in which the Chromaster 5310 column oven automatically records the history data including the number of injections into each column and analysis pressure on the recording tags attached to the columns For the operating method see the instruction manual provided for the column management system NOTE It is not permitted for the user to carry out installation at the ...

Page 733: ... tags to each appropriate slot according to the figure below The tag connected to an inappropriate slot will prevent correct history data management A 1 A 2 A 3 G 1 G 2 G 3 Appended Fig 1 22 Slot numbers 1 Where No Switching Valve is Used Where the column management system is used in the Chromaster 5310 column oven which is set not to use a switching valve the data on the tags which are connected ...

Page 734: ...or 6 way 2 position Valve For a 6 way 2 position valve the slot of the tag on which data is updated differs depending on whether the valve is used as a column selector in which case switching does not occur by the time program or as a switching valve in which case switching occurs by the time program Where the valve is used as a column selector Slot No of the Tag on which Data is Updated Valve Pos...

Page 735: ...gnals that are input and output via 3 pin connector Their names and functions vary with the unit A name that indicates the function is given at each connector Example of output contact signal EVENT of pump Example of input contact signal LAMP OFF IN of detector 2 Contact Signals Entering the e Line Connector Each unit has two e Line connectors for connection at the rear of the main unit and the si...

Page 736: ...ne connector BUSY 3 pin connector e DIO cable 890 6145 e DIO cable 890 6145 2 Connection with Model D 2500 Use the e DIO cable 890 6146 for connection D 2500 START COM EXTERNAL H L BUSY H L G START BUSY e Line connector To Chromaster series instrument Connect the START L and G terminals of the e DIO cable 890 6146 to the EXTERNAL COM terminal of the Model D 2500 APPENDIX 2 2 ...

Page 737: ...utput Terminals These are contact signal input terminals for control using contact signals of an external unit The output circuit is shown in Fig 4 The rating of contacts used is 12 V 0 1 A Make sure the load connected does not exceed this rating Other unit e Line cable Chromaster series unit A Chromaster series unit B Fig 1 e Line Cable Connection 5 V 320 Ω IN Max 10 mA unit OUT 4 7 kΩ H Max 12 V...

Page 738: ...romaster series unit External unit Activated upon shorting contacts of external unit Fig 3 Contact Signal Input Circuit 0 1 A max 1 30 V max 2 3 Chromaster series unit External unit Fig 4 Contact Signal Output Circuit APPENDIX 2 4 ...

Page 739: ...nterface board required for controlling the Chromaster series from a PC One IFC board is required per system UI pad Keypad with LCD for operating the instrument itself Isocratic system A system for delivering a single liquid with a single pump Time program A program for changing the temperature setting the valve position in the option valve and the event output according to the measuring timing Lo...

Page 740: ...etect a leakage of organic solvent in the column oven Detection is made by means of the vapor emitted from organic solvent when a leakage occurs Liquid leak sensor A sensor that can detect a liquid leakage in the column oven APPENDIX3 2 ...

Page 741: ...ve the instructions and warnings given in this manual and on the warning labels Keep this manual in a safe place nearby so it can be referred to whenever needed 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 3rd Edition June 2011 Copyright C Hitachi High Technologies Corporation 2011 1st Edition 2011 All rights reserved Printed in Japan Part No 892 9122 2 HH R RG LT ...

Page 742: ... party in any form or by any means without the express written permission of Hitachi High Technologies Corporation 3 Hitachi High Technologies Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 743: ...NUAL The operating procedures maintenance checkup instructions and precautions for the 6 channel degassing unit for Chromaster 5110 pump are described in this manual This manual consists of the following sections IMPORTANT contains details of warranty installation relocation after sale technical service useful life of this instrument etc SAFETY SUMMARY Chapter 1 OVERVIEW Chapter 2 FUNCTIONS Front ...

Page 744: ...arranty Scope of Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be availabl...

Page 745: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 746: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Technologies does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Technologies or its related companies or application of said instrument Installation Re...

Page 747: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 748: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 749: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 750: ...affected by electromagnetic noise within the permissible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power devi...

Page 751: ...r can result in minor or moderate injury or serious damage of the product In addition the following signal words are used for ensuring proper use of the product NOTICE Indicates a potentially hazardous situation which if not avoided can result in serious damage to property data and or the environment NOTE Used to indicate an instruction for ensuring correct trouble free use and avoiding minor dama...

Page 752: ...rrectly If a problem occurs with the instrument or if you have any question concerning the instruction manual contact our service representative nearest you Keep in mind that the hazard warnings in the manual or on the product cannot cover every possible case as it is impossible to predict and evaluate all circumstances beforehand Always be alert and use your common sense ...

Page 753: ...y our sales or service representative nearest you Injury due to irradiation with laser beam The CD ROM or CD R W drive in the PC incorporates a laser source In normal use of the PC equipped with a laser source a laser beam harmful to the human body is not irradiated outside of the equipment But if a leakage occurs and the laser beam strikes a person s eyes it could damage the person s eyesight Be ...

Page 754: ...ic solvent leaks from the flow path of the instrument and its vapor concentration reaches the explosion limit it could cause spontaneous combustion with dangerously explosive results When using a flammable and readily volatile chemical be sure to check for leakage from the instrument flow path and ventilate the laboratory room adequately Chapter 3 CAUTION There is no precautionary item classified ...

Page 755: ...r EU Countries IMPORTANT 6 Other Precautions IMPORTANT 6 SAFETY SUMMARY SAFETY 1 COMMON SAFETY PRECAUTIONS SAFETY 3 WARNING INDICATIONS APPEARING IN MANUAL SAFETY 4 WARNING SAFETY 4 CAUTION SAFETY 4 1 OVERVIEW 1 1 2 FUNCTIONS 2 1 2 1 Front Panel 2 1 2 2 Specifications 2 2 3 OPERATION 3 1 3 1 Selection of Mobile Phase 3 1 3 2 Operating Procedure 3 2 3 3 Error Output 3 3 3 4 Caution on Handling 3 4 ...

Page 756: ...degassing unit is built in the Chromaster 5110 pump and used in combination with other system components units of your liquid chromatograph For handling operation etc of the units which are not covered in this instruction manual refer to the instruction manuals of the respective units Before using the 6 channel degassing unit be sure to read the instruction manual of Chromaster 5110 pump 1 1 ...

Page 757: ...tus of vacuum pump Lamp Color Vacuum Pump Status Orange blinking Vacuum pump begins running upon turning on power supply Green blinking Vacuum level has reached the upper limit of control range Green Vacuum level has reached the set control point Orange The vacuum pump has stopped due to occurrence of an error 2 Flow Path Inlet Outlet Inlets and outlets for solvents before and after degassing Beca...

Page 758: ...l HPLC grade in which the air is dissolved up to saturation is delivered at flow rate 1 mL min at liquid temperature 25 C with cell length 10 mm 4 Internal Volume About 480 μL 1 flow path excluding tube 5 Vacuum Level 6 7 kPa 6 Maximum Withstand Pressure 0 2 MPa Note that normal flow into the degassing unit shall be made by means of suction A load of pressure to the flow path in the degassing unit...

Page 759: ...y 9 W 11 Dimensions 53 W 297 D 100 H mm 12 Operating Principle The liquid to be degassed is flowed through a special synthetic resin membrane placed in the vacuum chamber of 6 channel degassing unit The molecules of gases dissolved in liquid are small and have a higher mobility than the liquid and a high affinity to the resin membrane Therefore the gases are selectively transmitted through the mem...

Page 760: ...ory room adequately 3 1 Selection of Mobile Phase NOTE Restrictions on the use of mobile phase depending on its characteristics and temperature shall be followed carefully Refer to the table of organic solvent characteristics in the instruction manual of Chromaster 5110 pump Particularly solvents having a low boiling point cannot be used because bubbles may be formed in the degassing unit Substanc...

Page 761: ...a high concentration buffer solution or salt containing solvent be sure to wash with distilled water Otherwise the instrument may be damaged due to formation of crystals in the flow path 3 2 Operating Procedure 1 Turning on Power Supply After turning on the power switch the vacuum pump in the instrument starts Immediately after turning on the power supply the monitor LED blinks in orange The monit...

Page 762: ...reached 11 kPa at 10 minutes after start of the vacuum pump drive b When vacuum level has exceeded 13 kPa c At occurrence of pressure sensor error NOTE When an error output is issued in the 6 channel degassing unit analysis cannot be started from CDS 2 Release of Error Error status can be released by turning on power supply to the Chromaster 5110 pump again NOTE If the error recurs despite restart...

Page 763: ...t of an organic solvent with a salt containing solvent adequate replacement with distilled water is also required in the same way as above The internal volume of the degassing chamber in this degassing unit including tubes is about 5 mL per flow path For complete solvent replacement about 15 mL of solvent is required for each flow path And for solvent replacement by use of the pump a flow rate of ...

Page 764: ...d off However before a long time stop of the degassing unit turn off the power supply wash adequately with ion exchanged water run methanol or the like replace the flow paths with the air etc and then plug the tubes securely This is always required after use of a buffer because there is a possibility of salt precipitation growth of algae microorganisms etc in the membrane 3 5 ...

Page 765: ...dequately with hand c Solvent filter is clogged c Wash the solvent filter d An excessive negative pressure is caused because of solvent position d Position the solvent container at the same height as the instrument 2 Bubbles are discharged through outlet e Solvent replacement is inadequate e Carry out solvent replacement adequately a Tube joint is loose a Tighten the joint adequately with hand b S...

Page 766: ...aler or nearest Hitachi High Technologies service representative in order to avoid possible trouble involved in relocation 1 1 Check against Packing List 1 Exterior Check of Package First of all check the exterior of product package If damaged is found or you have any question contact your dealer 2 Unpacking Unless the exterior of product package is abnormal unpack the product so as not to give sh...

Page 767: ...0 to 25 C 2 Operating Humidity 25 to 85 3 Atmospheric Gas a Adequate ventilation is required b The room shall not be filled with highly corrosive gas of acid or alkali 4 Other General Precautions a Shall not be exposed to direct sunlight Performance degradation or coating discoloration might be caused b Shall be free from strong vibration or shock which can be felt by your body Fine adjustment of ...

Page 768: ...e inlet tubes attached to the pump and autosampler The tubes should be connected carefully with hand without using a tool 2 Connection of Connecting Tubes on OUT side of degassing unit For connection from the 6 channel degassing unit to the pump proportioning valve and autosampler 6 kinds of special connecting tubes attached to the degassing unit should be used For connection to the proportioning ...

Page 769: ... Attached to Chromaster 5110 Pump 6 channel degassing unit Low pressure gradient unit proportioning valve Appended Fig 2 2 Tubing between 6 channel Degassing Unit and Proportioning Valve Tube for port 1 Tube for port 2 Appended Fig 2 3 Tubes Attached to Wash Pump of Chromaster 5210 Autosampler APPENDIX 2 3 ...

Page 770: ...ated with the aspiration syringe attached to the pump The total internal volume per flow path of the tubes for pump and the degassing chamber of 6 channel degassing unit is about 5 mL So eluent should be aspirated in a few steps When the proportioning valve is used eluent aspiration is required for each valve flow path APPENDIX 2 4 ...

Page 771: ...tructions in this manual and the WARNING CAUTION labels on the instrument Keep this manual in a safe place nearby so it can be referred to whenever needed 24 14 Nishi Shimbashi 1 chome Minato ku Tokyo Japan 4th Edition June 2011 Copyright C Hitachi High Technologies Corporation 2011 1st Edition 2011 All rights reserved Printed in Japan Part No 892 9220 3 HH R GG HMS ...

Page 772: ... party in any form or by any means without the express written permission of Hitachi High Technologies Corporation 3 Hitachi High Technologies Corporation assumes no liability for any direct indirect or consequential damages arising from use not described in this manual Utmost care must be exercised when using the instrument 4 This document does not provide any warranty or permission for industria...

Page 773: ...e to safety Note that it is allowed only for persons having a basic knowledge of chemical analysis procedures to use this instrument Carefully read this instruction manual before attempting operation For proper use of the software please acquaint yourself with it The liquid chromatograph system comprises a pump unit for delivering mobile phases a sample introduction unit for injecting samples auto...

Page 774: ...on 2 FUNCTIONS The Instrument Keypad Section 3 OPERATION Basic Operation Measuring Operation Section 4 MAINTENANCE Checking the Performance and Specifications Section 5 PARTS REPLACEMENT Consumables and Spare Parts Section 6 ACCESSORIES Thermostat Sample Racks Section 7 INDEX APPENDIX1INSTRATTION APPENDIX2EXPLANATION OF CONTACT SIGNALS APPENDIX3TERMINOLOGY First of all read IMPORTANT and SAFETY SU...

Page 775: ...e of Warranty Any parts which prove to be defective in design or workmanship during the warranty period will be repaired adjusted or replaced without charge A substitute part may be used for repair or replacement with an equivalent product may be made instead of repair Such system components as a personal computer and printer to be updated frequently for improvement may not be available in origina...

Page 776: ...rements specified by the manufacturer b Failure due to power supply voltage frequency other than specified by the manufacturer or due to abnormality in power supply c Corrosion or deterioration of the tubing due to impurities contained in reagent gas air or cooling water supplied by the user d Corrosion of the electric circuits or deterioration of the optical elements due to highly corrosive atmos...

Page 777: ...isclaimer of Liability for Industrial Properties of a Third Party Hitachi High Technologies does not assume any liability for a third party s complaint regarding infringement of any patent rights or industrial properties with respect to products manufactured through use of the equipment supplied by Hitachi High Technologies or its related companies or application of said instrument Installation Re...

Page 778: ...ot be available in the event of discontinuance of manufacture of the main unit If repair cannot be provided in the case of instrument malfunction we recommend that you consider discontinuing use and replacing the instrument Technical Seminars and Training Courses for Users We offer technical seminars and training courses at either our or user s facilities to ensure proper and safe operation of the...

Page 779: ... providing insulation on its positive and negative terminals with adhesive vinyl tape or the like Precautions on CE Conformity Marking In consideration of use in the European countries this instrument bears the CE mark indicating the conformity to the requirements mentioned below Electromagnetic Compatibility Requirement This instrument is designed to satisfy the European Norm EN61326 1 2006 for t...

Page 780: ...cycle of the product You might be charged for the costs arising from take back and recycling 2 In other Countries outside the EU If you wish to discard this product please contact your local authorities and ask for the correct method of disposal Other Precautions Handling of Chemicals and Samples a The user is responsible for following relevant laws and regulations in handling storage and disposal...

Page 781: ...affected by electromagnetic noise within the permissible range of this standard Also data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction In the room where this instrument is installed the following electric devices must not be brought Devices which emit radio waves such as mobile phone transceiver wireless telephone and similar small power devi...

Page 782: ...word NOTICE or NOTE is used to indicate precautionary instructions concerning possible property damage NOTICE Used to indicate a potentially hazardous situation which if not avoided will or can result in damage to user s property serious damage to the instrument damage to data or environmental pollution though personal injury may not be incurred NOTE Used to indicate explanatory information for en...

Page 783: ...tric shock or fire Radiation from the Laser Light Source WARNING The internal CD ROM or CD R W drive of the PC is provided with a laser beam source In normal operation of the PC containing the laser beam source no laser beam harmful to human health will be emitted outside Note however that if a laser beam leaking out of the PC accidentally gets into the eye eye injury could occur When using the PC...

Page 784: ...nition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution employ and provide proper grounding connection to it Section 3 4 Explosion of Vapor from Flammable Chemicals If a flammable chemical such as organic solvent leaks from the flow path of the instrument and its vapor concentration reaches the explosion limit it could cause spon...

Page 785: ...ng connection For grounding connection use a screw having a diameter of M4 or higher and a turn count of 3 or more in threading and a wire having a thickness of 1 25 mm APPENDIX 1 Inflammation or Injury due to Toxic Corrosive or Stimulative Solvent When using a toxic corrosive or stimulative solvent be careful not to incur a physical inflammation or injury For details of the properties of each sol...

Page 786: ...t APPENDIX 1 Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over When installing the instrument provide a proper means for preventing the instrument from tipping over accidentally APPENDIX 1 Fatigue due to Long Hour Operation If you keep working with the display monitor and keyboard for long hours your eyes and body will be fatigued to jeopardize your hea...

Page 787: ...he appearances of these warning labels to see if they are clean to allow easy reading over a safe distance If any one of the warning labels becomes illegible due to deterioration contact your local Hitachi High Technologies Corporation sales representative or service office of Hitachi High Technologies Corporation sales representative for replacement with a new one 1 Ignition of Flammable Chemical...

Page 788: ...MMARY WARNING and CAUTION Labels on Instrument 4 Injury of Hand by Needle or Internal Mechanism Left side view 5 Electric Shock due to Contact with Inside of Instrument when equipped with optional cooling unit Rear Panel ...

Page 789: ...ases where the amount of leakage is too small Furthermore leakage of a highly volatile solvent may not be detected Be sure to check for liquid leakage regularly to prevent a possible serious accident regardless of whether the leak sensor is activated or not a In routine inspection of the instrument visually check for liquid leakage before attempting measurements b In periodic inspection of the ins...

Page 790: ...TY SUMMARY NOTICE precaution Continued Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally If necessary conduct measurement on a control sample ...

Page 791: ...Safety Precautions SAFETY 2 WARNING Precautions in the Manual SAFETY 3 CAUTION Precautions in the Manual SAFETY 5 WARNING and CAUTION Labels on Instrument SAFETY 6 NOTICE Precautions SAFETY 8 1 OUTLINE 1 1 1 1 Isocratic System 1 1 1 2 Low Pressure Gradient System 1 2 2 FUNCTIONS 2 1 2 1 The Instrument Keypad 2 1 2 1 1 Name and Function of Each Part on Autosampler 2 1 2 1 2 Name and Function of Eac...

Page 792: ...75 4 MAINTENANCE 4 1 4 1 Checking the Performance and Specifications 4 1 4 1 1 Preparation of Items 4 1 4 1 2 Preparation of Operation 4 2 4 1 3 Reproducibility Check 4 5 4 2 Periodic Maintenance 4 8 4 2 1 Liquid Leak Check 4 8 4 2 2 Washing the Flow Path 4 8 4 2 3 Cleaning 4 9 4 2 4 Waste solution tube 4 9 4 2 5 Liquid Leak Sensor 4 9 4 2 6 Drain tray 4 11 4 3 Positioning the Mechanism 4 12 4 3 1...

Page 793: ...r APPENDIX1 4 Appendix 1 3 1 Power Supply Arrangement APPENDIX1 4 Appendix 1 3 2 Installation Space APPENDIX1 11 Appendix 1 4 Checking the Contents APPENDIX1 11 Appendix 1 5 Assembling APPENDIX1 12 Appendix 1 5 1 Removal of Transport Screws APPENDIX1 12 Appendix 1 5 2 Attachment of Waste Solution Tube APPENDIX1 14 Appendix 1 5 3 System Power Supply APPENDIX1 15 Appendix 1 5 4 System Cabling APPEND...

Page 794: ... the sample In addition a degassing unit for deaerating a mobile phase a gradient device for varying a mixing ratio of mobile phases with time and other optional devices are incorporated in the system 1 1 Isocratic System The isocratic system has a simple configuration in which single solvent analysis is performed Wash fluid Chromaster 5110 pump Chromaster 5310 column oven Chromaster 5210 autosamp...

Page 795: ...ent System In the low pressure gradient system two or more solvents are mixed in its low pressure section from which a liquid feed is performed by a single pump The composition of a mobile phase is made to vary with time in chromatographic separation Fig 1 2 Low Gradient System Wash fluid Mobile phase Chromaster organizer Chromaster 5410 5420 5430 detector Chromaster 5310 column oven Injection val...

Page 796: ... mixed at a pre specified ratio 3 Through the mixer the mixture mobile phase is delivered 4 A sample is injected by the autosampler 5 The injected sample is separated through the column which is maintained at a constant temperature by the column oven 6 Each component separated from the sample is detected as a signal by the detector 1 3 ...

Page 797: ...LED lights in a specific color for the determined indication Name color LED Status AS blue orange Blue Power is on Orange Error of autosampler THERMO blue orange Blue Under temperature control with thermostat 1 option Orange Error of thermostat option RUN blue Blue Sequential program under execution when using stand alone Or analysis by a GUI controller or when injecting when the system is control...

Page 798: ...e and mobile phase to the column Syringe valve Selects the aspirating discharging direction of sample and detergent Syringe Aspirates and discharges a sample and detergent Syringe Sample rack Injection valve 3 way switching valve Wash pump Wash port Syringe valve Degassing unit Drain tray Port 1 Solvent 1 Port 2 Solvent 2 2 1 Wash pump 2 2 ...

Page 799: ... switching valve A valve for switching flow path of wash fluid1 and wash fluid2 Wash pump A pump for delivering wash fluid Degassing unit option Wash fluid1 and wash fluid2 is degassed Door lock mechanism Locks doors during an analysis Arm Needle Sample loop Leak sensor Injection port Fig 2 3 Front View C 2 3 ...

Page 800: ...T OFF IN START OUT ALL END OUT Fig 2 4 Rear View Wiring cover Removal of the left wiring cover as seen from the front gives access to the e Line connector for connecting the units of Chromaster series and the power connector Grounding terminal Grounds the autosampler Thermostat power supply depend on the optional Used for the optional thermostat IFC board option An interface control board option r...

Page 801: ... when the ALL END time is reached under the condition of ALL END OUT setting Effective in use as stand alone 2 1 2 Name and Function of Each Part on UI Pad option 1 Operation Keys Each key on the UI pad option type operation panel is explained here Use the UI pad or the chromatography data station for the instrument operation Refer to the following table for key roles For details see the section 3...

Page 802: ...en the analysis condition setting is to be interrupted And also press this key for unlocking the key lock 11 LOCK OFF Use this key for unlocking the keys 12 FUNC Moves the mechanism for maintenance etc 13 SELECT Used for selecting a setting item when setting the rack parameter in the robotic mode 14 DEL Used for deleting a step in a sequential program 15 IDLE Returns the autosampler to the idle po...

Page 803: ...vertical axis Z whereby the needle can move freely among the sample vials wash port and injection port To the needle a valve and a syringe are connected so a sample can be aspirated and dispensed After a sample is aspirated through the needle tip the needle is washed in the wash port and the sample is led into the flow path with the injection valve set on the injection side When the UI pad option ...

Page 804: ...ler Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger Wash Needle Injection port 5 4 3 2 1 from Pump to Column 6 Loop Waste solution 2 Sample Rack Degassing unit Wash fluid1 P 3 way solenoid valve Waste solution Wash fluid2 2 8 ...

Page 805: ...uitable for analysis of minute samples since no part of the sample is washed The sample loop is filled with sample for measurement This method provides the best repeatability of sample injection volume in analysis Measurement method Syringe Syringe Loop Measurement method details Discharge rate from Syringe Aspiration Discharge rate from syringe The summation of the capacity of the flow pass in th...

Page 806: ... volume requires the double loop capacity 0 10 20 30 40 50 60 70 80 90 100 20 40 60 80 100 120 140 160 180 200 Loop Capacity µl Sample Injection Volume µl Fig 2 7 Cut Injection Method All Volume Injection Method When applying all volume injection method the loop capacity much more than the injection volume is required Select loop capacity within the area indicated in the following figure The sampl...

Page 807: ...elect sample introduction volume within the area indicated in the following figure The sample introduction volume is selected within the shadow area of the following figure to fill a loop with the density of the 99 of the sample For example more than 25 µL sample is required when injecting 5 µL sample 5 µL loop capacity This means that quintuple sample volume is required 5 10 15 20 25 50 75 100 Am...

Page 808: ...ueous solvent 2 Gradient initial solvent 1 Weak wash 1 As a washing solution in cases where a solvent containing a buffer solution or salt has been fed as the mobile phase use a mobile phase solvent containing no salt When 20 mmol L KH2PO4 CH3CN 50 50 is used for the mobile phase use H2O CH3CN 50 50 If a solvent containing salt is used for washing it causes damages such as the surface of the glass...

Page 809: ...e injection volume the lead volume the rear volume and the air volume are restricted by the following relational expression A stroke of the syringe capacity can t be used all 175 µL of Standard syringe vi vl vr va 165 µL vi Injection volume The sample net volume to the flow path vl Lead volume The disposal volume of the lead part of a sample vr Rear volume The disposal volume of the rear part of a...

Page 810: ...yringe via the 3 way solenoid valve the wash pump and the port3 of the syringe valve Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Needle Injection port 5 4 3 2 1 From Pump To Column 6 Waste solution Loop Wash port Sample Rack Wash fluid2 P Waste solution Degassing unit 3 way solenoid valve Wash fluid1 2 14 ...

Page 811: ...after the needle has moved into the wash port the same as the procedure 9 And when fluid2 wash is set wash the injection port flow paths using the wash fluid2 the same as the procedure 10 v v v v v d Dead volume the instrument inside parameter i Injection volume the sample net volume to the flow path l Lead volume forward part cut volume r Rear volume rearward part cut volume a Air volume the air ...

Page 812: ...ide parameter vi Injection volume the sample net volume to the flow path vl Lead volume forward part cut volume vr Rear volume rearward part cut volume va Air volume the air volume which sample is sandwiched Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash From Pump To Column vr vi vl Injection port 5 4 3 2 1 6 Waste solution Loop Waste solution Wash port Sample Rack Wash flu...

Page 813: ...e valve Syringe Wash pump 5 1 3 2 4 Plunger wash From Pump To Column Injection port 5 4 3 2 1 6 Waste solution Loop Waste solution Wash port Sample Rack Wash fluid2 Wash fluid1 P Needle va 2 va 2 Degassing unit vd Dead volume the instrument inside parameter Injection volume the sample net volume to the flow path Lead volume forward part cut volume Rear volume rearward part cut volume Air volume th...

Page 814: ...ume the sample net volume to the flow path vl Lead volume forward part cut volume vr Rear volume rearward part cut volume va Air volume the air volume which sample is sandwiched Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash From Pump To Column Injection port 5 4 3 2 1 6 Waste solution Loop Waste solution Wash port Sample Rack Wash fluid2 Wash fluid1 P Needle vl vl va 2 vd ...

Page 815: ...me to the flow path vl Lead volume forward part cut volume vr Rear volume rearward part cut volume va Air volume the air volume which sample is sandwiched Syringe Wash pump 5 1 3 2 4 Plunger wash Waste solution Wash port Sample Rack Wash fluid2 Wash fluid1 P Needle Injection valve From Pump To Column Injection port 5 4 3 2 1 6 Waste solution Degassing unit vl Loop Degassing unit 3 way solenoid val...

Page 816: ... cut volume vr Rear volume rearward part cut volume va Air volume the air volume which sample is sandwiched Syringe vi Buffer tube Syringe valve 5 1 3 2 4 Plunger wash Waste solution Wash port Sample Rack Wash fluid2 P Needle vl Injection valve From Pump To Column Injection port 5 4 3 2 1 6 Waste solution Degassing unit Loop vi Wash pump Wash fluid1 Degassing unit 3 way solenoid valve 2 20 ...

Page 817: ...jection volume the sample net volume to the flow path vl Lead volume forward part cut volume vr Rear volume rearward part cut volume va Air volume the air volume which sample is sandwiched Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Waste solution Wash port Sample Rack Wash fluid2 Wash fluid1 P vl Injection valve Needle From Pump To Column Injection port 5 4 3 2 1 6 Loop Waste solution ...

Page 818: ...n port with the wash pump to wash the flow path of the buffer tube and the injection valve Buffer tube Syringe valve Syringe Wash pump 5 1 3 2 4 Waste solution Wash port Sample Rack Wash fluid2 Wash fluid1 P Needle Injection valve From Pump To Column Injection port 5 4 3 2 1 6 Loop Waste solution Degassing unit Plunger wash Degassing unit 3 way solenoid valve 2 22 ...

Page 819: ...dle to the injection port with the wash pump to wash the flow path of the buffer tube and the injection valve Buffer tube Syringe valve Syringe 5 1 3 2 4 Plunger wash Waste solution Wash port Sample Rack Wash fluid2 Wash fluid1 P Needle Injection valve From Pump To Column Injection port 5 4 3 2 1 6 Loop Waste solution Degassing unit Wash pump Degassing unit 3 way solenoid valve 2 23 ...

Page 820: ...Switch the 3 way solenoid valve to the wash fluid1 side Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Needle Injection port 5 4 3 2 1 From Pump To Column 6 Waste solution Loop Waste solution Wash port Sample Rack Wash fluid2 P 3 way solenoid valve Degassing unit Wash fluid1 2 24 ...

Page 821: ...port 4 Deliver the wash fluid2 to the pump plunger with the wash pump specified time After washing it moves to the idle status Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Needle Injection port 5 4 3 2 1 From Pump To Column 6 Waste solution Loop Waste solution Wash port Sample Rack Wash fluid2 P 3 way solenoid valve Degassing unit Wash fluid1 2 25 ...

Page 822: ...eed volume The wash fluid volume to deliver a sample to the loop va Air volume The air volume of the lead and rear part of a sample 100 µL loop is used for the autosampler as a standard In general the feed volume is set as from 30 μl to 40 µL when using 10 μl of sample In All volume injection method the condition as va 0 μl of Air volume is recommended For a high accuracy gradient analysis wash fl...

Page 823: ...yringe via the 3 way solenoid valve the wash pump and the port3 of the syringe valve Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Needle Injection port 5 4 3 2 1 6 Loop Sample Rack Wash fluid2 P Waste solution Waste solution Wash port From Pump To Column Degassing unit 3 way solenoid valve Wash fluid1 2 27 ...

Page 824: ... needle has moved into the wash port the same as 2 3 3 Cut injection method procedure 9 And when fluid2 wash is set wash the injection port flow paths using the wash fluid2 the same as 2 3 3 Cut injection method procedure 10 Buffer tube Syringe valve Syringe Injection valve vd Dead volume the instrument inside parameter vi Injection volume the sample net volume to the flow path vf Feed volume the ...

Page 825: ...eter vi Injection volume the sample net volume to the flow path vf Feed volume the wash fluid volume to deliver a sample to the loop va Air volume the air volume which sample is sandwiched Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash vi Injection port 5 4 3 2 1 6 Loop Wash port Sample Rack P va 2 vi Needle va 2 Wash fluid1 Wash fluid2 From Pump To Column Waste solution Wa...

Page 826: ...t inside parameter vi Injection volume the sample net volume to the flow path vf Feed volume the wash fluid volume to deliver a sample to the loop va Air volume the air volume which sample is sandwiched Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash 5 4 3 2 1 6 Loop Sample Rack P va 2 Needle va 2 Injection port Waste solution Waste solution Wash port From Pump To Column Was...

Page 827: ...ort Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Injection port 5 4 3 2 1 6 Loop Sample Rack P Needle Waste solution Waste solution Wash port From Pump To Column Wash fluid1 Wash fluid2 Degassing unit 3 way solenoid valve 2 31 ...

Page 828: ...e in the loop Buffer tube Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Needle Injection valve Sample Rack P Needle Injection port 5 4 3 2 1 6 Loop Degassing unit Wash fluid1 Wash fluid2 Waste solution Waste solution Wash port From Pump To Column Degassing unit 3 way solenoid valve 2 32 ...

Page 829: ... Injection volume the sample net volume to the flow path vf Feed volume the wash fluid volume to deliver a sample to the loop va Air volume the air volume which sample is sandwiched Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Sample Rack P Needle Injection valve Injection port 5 4 3 2 1 6 Loop vf vf vi vd va Wash fluid1 Wash fluid2 From Pump To Column Waste solution Waste solution Wash ...

Page 830: ... the instrument inside parameter vi Injection volume the sample net volume to the flow path vf Feed volume the wash fluid volume to deliver a sample to the loop va Air volume the air volume which sample is sandwiched Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Wash solution Wash port Sample Rack Wash fluid2 Wash fluid1 P Needle Injection valve Injection port 5 4 3 2 1 6 Loop Wash soluti...

Page 831: ...capacity can t be used all 175 µL of Standard syringe vi vw va 165 µL vi Injection volume The sample net volume to the flow path vw Waste volume The disposal sample volume of the lead and rear part of the loop va Air volume The air volume of the lead and rear part of a sample One half of the waste volume vw 2 is calculated and delivered automatically to the lead and the rear part of the loop each ...

Page 832: ... syringe via the 3 way solenoid valve the wash pump and the port3 of the syringe valve Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Needle Injection port 5 4 3 2 1 6 Wash solution Loop Wash solution Wash port Pump Rack P Wash fluid2 Wash fluid1 From Pump To Column Degassing unit 3 way solenoid valve 2 36 ...

Page 833: ... needle has moved into the wash port the same as 2 3 3 Cut injection method procedure 9 And when fluid2 wash is set wash the injection port flow paths using the wash fluid2 the same as 2 3 3 Cut injection method procedure 10 Buffer tube Injection valve vd Dead volume the instrument inside parameter vi Injection volume the sample net volume to the flow path vw Waste volume the air volume of the lea...

Page 834: ...de parameter vi Injection volume the sample net volume to the flow path vw Waste volume the air volume of the lead and rear part of a sample va Air volume the air volume which sample is sandwiched Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash vw vi Injection port 5 4 3 2 1 6 Waste solution Loop Waste solution Wash port Sample Rack P Needle va 2 va 2 From Pump To Column Was...

Page 835: ...t inside parameter vi Injection volume the sample net volume to the flow path vw Waste volume the air volume of the lead and rear part of a sample va Air volume the air volume which sample is sandwiched Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Injection port 5 4 3 2 1 6 Waste solution Loop Wash port Sample Rack P Needle va 2 Wash fluid2 Wash fluid1 Waste solution From...

Page 836: ...ort Buffer tube Injection valve Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Injection port 5 4 3 2 1 6 Loop Sample Rack P Needle Wash fluid2 Wash fluid1 Waste solution Waste solution Wash port From Pump To Column Degassing unit 3 way solenoid valve 2 40 ...

Page 837: ...ase pressure in the loop Buffer tube Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Sample Rack P Needle Injection valve Injection port 5 4 3 2 1 6 Loop Wash fluid2 Wash fluid1 Waste solution Waste solution Wash port From Pump To Column Degassing unit 3 way solenoid valve 2 41 ...

Page 838: ...me the instrument inside parameter vi Injection volume the sample net volume to the flow path vw Waste volume the air volume of the lead and rear part of a sample va Air volume the air volume which sample is sandwiched Syringe vlave Syringe Wash pump 5 1 3 2 4 Plunger wash Sample Rack P Needle Injection valve Injection port 5 4 3 2 1 6 Loop vw 2 vw 2 Wash fluid2 Wash fluid1 Waste solution Waste so...

Page 839: ... Buffer tube Refer to 2 3 3 Sample Injection Procedure Cut Injection Method Procedure 9 to 12 for completion of the analysis after this operation Syringe valve Syringe Wash pump 5 1 3 2 4 Plunger wash Sample Rack P Needle Injection valve Injection port 5 4 3 2 1 6 Loop Wash fluid2 Wash fluid1 Waste solution Waste solution Wash port From Pump To Column Degassing unit 3 way solenoid valve 2 43 ...

Page 840: ...1 to 100 µL 5 Loop capacity 100 µL standard 200 µL accessory 5 10 20 µL option 6 Syringe speed 5 steps 7 Reproducibility of injection volume 1 2 0 2 RSD in 10 μL injection Cut injection method 0 25 RSD in 5 μL injection Cut injection method 0 9 RSD in 1 μL injection Cut injection method 1 0 RSD in 1 μL injection All volume injection method 0 2 RSD in 5 μL injection Full loop injection method 8 Car...

Page 841: ...0 MPa 17 Material of liquid contacting parts SUS316 Vespel fluororesin PP EPDM Perfluoroelastomer 18 Number of injections per sample 99 max 19 Maximum cycle time 999 9 min 20 External communication e Line 21 GLP function Maintenance logbook a Injection port seal b Injection valve seal c Syringe valve seal d Syringe e Wash pump operation time 22 External I O a WAIT OFF IN b START OUT c ALL END OUT ...

Page 842: ... 1 5 mL sample vial 855 2351 Septum Si TEF slit 080 3704 Screw cap In the other cases refer to 6 3 adjust the rack parameters refer to 3 3 according to the combination used for your practical application and check the reproducibility performance before proceeding to operation For good reproducibility avoid using a septum repeatedly to prevent a cause of a hole It causes a fluctuation of sample con...

Page 843: ...ut sample freezing 4 C Target temperature 10 C 40 C ambient temperature 25 C relative humidity 60 water temperature measured in central microplate without sample freezing 4 Temperature distribution 2 C Target temperature 4 C 40 C ambient temperature 25 C relative humidity 60 water temperature measured in central and 4 corner sample vials 1 5 mL 4 mL 1 mL without sample freezing 3 C Target temperat...

Page 844: ...untermeasure Overheat prevention system by the thermal protector 75 C 10 Power supply AC 100 V to 240 V 10 50 60 Hz 110 VA 1 An acceptable temperature range for the thermostat is from 1 to 45 C The actual temperature depends on ambient environment temperature and humidity so different specifications are set as temperature control ranges 2 48 ...

Page 845: ...splay monitor for a long time take a break for 10 to 15 minutes per hour for health of your eyes and body 3 1 Basic Operation 3 1 1 Power supply The power activation operation of the Chromaster 5210 autosampler is described here Window Door L Door R Power switch UI Pad LED Fig 3 1 Front Panel NOTE If the monitor display screen does not appear on the LCD within 3 minutes after turning on the power ...

Page 846: ... main frame 1 1 1 10 0 1 1 0 0 C STEP RACK VIAL VOL µL INJ TIME I Indication Description STEP A step in the running program RACK No of the sample rack under analysis VIAL No of the sample vial under analysis VOL μl Sample injection volume per injection INJ Number of actual injections into each sample vial per set number of injections TIME Analysis time Description of status indication at upper rig...

Page 847: ...s indicated when the thermostat is not under control The following screen appears when the thermostat is not connected or its use is not set d Monitor screen changeover i 1st Monitor Screen ii 2nd Monitor Screen THERMO UNIT IS NOT AVAILABLE I C STEP RACK VIAL VOL µL INJ TIME I ESC or or or 35 0 30 0 40 0 C TEMP RANGE I 1 1 1 10 0 1 1 0 0 C NOTE Even in the key locked status the monitor screens can...

Page 848: ...Input field c Numerical selection Selection item Parameter name UTILITY SEQ 1 RACK 2 WASH PARAM 3 1 OTHERS 4 Input field d Program setup screen STEP RACK VIALS VOL µL INJ TIME 1 1 1 120 10 0 1 5 0 Input Item Input field 2 Numerical input a A cursor is indicated on the first character in the input field Previous setup value is indicated in the input field Initial value will be indicated for the fir...

Page 849: ...een monitor screen Even if the ESC key is pressed during input the inputting parameter won t be renewed NOTE When turning on the power supply default numbers are indicated in the selection item When the CL key is pressed in the input field indication in the field is deleted and the cursor returns to the first character in the input field When the DEL key is pressed in the input field items are del...

Page 850: ...rear side on the rack holder and then slowly insert the rack toward the rear Fix the rack at the position where a pin engaging sound can be heard After mounting the sample rack on the rack holder take the following steps a and b Be sure to check that the sample rack is mounted at the correct position a Make sure that the sample rack does not move in an attempt of pushing it toward the rear side of...

Page 851: ...ng the sample rack to prevent splash of dew condensation water to the instrument in the following procedure a Lift the handle of the sample rack about 10 mm The locating pin of the sample rack is removed via the locating hole of the rack holder At this time avoid lifting the handle suddenly and highly At this time avoid lifting the handle suddenly and highly It may cause a malfunction of the instr...

Page 852: ...Pull out the sample rack while keeping it in parallel position t the rack holder o Sample rack Locating pin Handle Rack holder Fig 3 3 Handling of Thermostat Rack 3 8 ...

Page 853: ...e sample rack accidentally 2 Take care not to flaw the contacting surfaces of the sample rack and cooling rack holder The performance of the instrument could deteriorate if these surfaces are flawed 3 Put it in until a sample vial touches the bottom of a sample rack The target temperature control and the suction of a sample will be failed 3 9 ...

Page 854: ... 3 Setting of standard sample rack Orient the septum as shown below Cap with hole White silicone rubber Brown Teflon Septum Sample vial 1 5 mL 3 10 ...

Page 855: ...tions can be set Confidence report can be displayed and reset Keys can be locked THERMO STOP Halfway stop For displaying or resetting confidence report For locking keys LOCK OFF Measurement continues till end of sequential program ALL END IDLE IDLE ESC IDLE FUNC End of operation IDLE mechanism initialization IDLE key input awaited IDLE IDLE key input awaited ESC ENT or ESC ENT or ESC ENT or Moveme...

Page 856: ...rminated the idle status is set and the monitor screen appears STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 C Wait until the pump column detector etc are warmed up and the baseline becomes stable Press the WASH key to fill the syringe and wash port with detergent Place the vials containing samples in the rack and position the rack in the autosampler Press the START key to start a sequential...

Page 857: ...e end of initialization after power on PROG EDIT MODE MODIFY 0 NEW 1 0 Select MODIFY for editing the previous program or NEW for creating a new program 0 ENT or 1 ENT STEP RACK VIALS VOL µL INJ TIME 1 1 1 1 10 0 1 5 0 Input a rack code 1 ENT STEP RACK VIALS VOL µL INJ TIME 1 1 1 1 10 0 1 5 0 Input the first vial number 1 ENT STEP RACK VIALS VOL µL INJ TIME 1 1 1 1 10 0 1 5 0 Input the last vial nu...

Page 858: ...nitor screen reappears ESC STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 C b STEP deleting method Unnecessary steps in a sequential program can be deleted STEP RACK VIALS VOL µL INJ TIME 3 _1 1 1 10 0 1 5 0 Display the unnecessary step and press the DEL key STEP RACK VIALS VOL µL INJ TIME 1 1 1 10 0 1 5 0 Press the ENT key STEP RACK VIALS VOL µL INJ TIME 3 1 5 5 10 0 1 5 0 The old contents o...

Page 859: ...PROG key during execution of a sequential program the screen displays that program An asterisk is displayed under the initial character S of the STEP which has already been executed or under execution The previous and next steps can be displayed by and keys The ESC key is usable for return to the monitor screen Example When a 3 step program has been created STEP RACK VIALS VOL µL INJ TIME 3 1 3 3 ...

Page 860: ...y an asterisk appearing under the initial character S of STEP Program execution can be resumed by pressing the PAUSE key again STEP RACK VIAL VOL µL INJ TIME P PAUSE NOW SAMPLING P PAUSE WAIT 2 1 2 10 0 1 1 0 0 C ESC ESC ESC STEP RACK VIALS VOL µL INJ TIME 2 1 2 2 10 0 1 10 0 STEP RACK VIALS VOL µL INJ TIME 1 1 1 1 10 0 1 10 0 STEP RACK VIALS VOL µL INJ TIME 3 1 3 3 10 0 1 10 0 Program indication ...

Page 861: ...ng Use the UTLTY key to set it UTILTY STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 C UTILITY SEQ 1 RACK 2 WASH PARAM 3 1 OTHERS 4 Under this display a parameter is selectable and its contents are settable as you desire 3 17 ...

Page 862: ... by pressing the START key 2 ENT At the end of a sequential program the ALL END signal can be output This signal is usable for control of other module connected For output of the ALL END signal input 1 YES or 0 NO for avoiding the output 0 ENT UTILITY SEQ 1 RACK 2 WASH PARAM 3 1 OTHERS 4 SEQ PARAM START STEP 1 ALL END 2 1 OPERATION 3 INJ TIMING 4 START STEP 1 100 1 Monitor screen reappears ALL END...

Page 863: ...till output of the ALL END signal is settable For stopping the system with a short time lag due to washing in the pump a time period should be set here taking a necessary time lag into account 15 ENT Monitor screen reappears 3 ENT Select an operating condition 1 ENT For creating a new sequential program input the default rack code value at the first step 1 ENT OPERATION RACK SELECT 1 INJ METHOD 2 ...

Page 864: ...ut a rear volume 30 ENT 2 ENT Input a feed volume 30 ENT 3 ENT Input a waste volume 100 ENT 1 LEAD VOLUME 0 0 300 0 µL 30 0 REAR VOLUME 0 0 300 0 µL 30 0 Monitor screen reappears FEED VOLUME 0 0 500 0 µL 30 0 Monitor screen reappears WASTE VOLUME 0 0 600 0 µL 100 0 Monitor screen reappears to be continued 3 20 ...

Page 865: ...D 1 5 4 Set a syringe speed to discharge a sample according to the sample viscosity Set slow syringe speed for a high viscosity sample 4 ENT Relation between Syringe Capacity and Syringe Speed Syringe Capacity Speed 1 Speed 2 Speed 3 Speed 4 Speed 5 70 µL 0 4 µL s 1 µL s 4 µL s 10 µL s 35 µL s 175 µL 1 µL s 2 5 µL s 10 µL s 25 µL s 87 5 µL s 700 µL 1 µL s 4 µL s 10 µL s 20 µL s 87 5 µL s Monitor s...

Page 866: ...d the needle is apt to be broken due to a strong falling force Therefore before operation make sure vials etc are correctly set 2 ENT 3 ENT Select a syringe volume to be used 2 ENT 4 ENT Input an air volume 2 ENT NEEDLE DOWN SPEED SLOW 1 FAST 2 2 Monitor screen reappears SYRINGE VOL 70 µL 1 175 µL 2 700 µL 3 2 Monitor screen reappears AIR VOL 0 0 20 0 µL 2 0 Monitor screen reappears to be continue...

Page 867: ...ed Take care not to incur this condition Since synchronization is made with the cam position of the pump the time period to be taken before injection may be longer than that in ordinary analysis 2 Indicated below are the proper minimum flow rate ranges for the respective pumps in USE setting of this function In cases where a lower flow rate is selected do not specify SYNCHRONIZED WITH PUMP PASS Mo...

Page 868: ... 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 2 57 1 178 6 10 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 3 57 1 178 6 10 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 4 57 1 178 6 10 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 5 57 1 178 6 10 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 6 57 1 178 6 10 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 7 57 1 178 6 10 0 0 148 5 34 0 12 5 For 1 5ml 120 PCS STD 8 57 1 17...

Page 869: ...7 Pattern code 8 NOTE The coordinate position indicated in the fig 3 5 determines rack parameters for X1 X coordinate of first vial Y1 Y coordinate of first vial X2 X coordinate of last vial Y2 Y coordinate of last vial Select the pattern cord type of the rack parameter to change the order of the vial for analysis 3 25 ...

Page 870: ...rameter is to be set Select INPUT VALUE for numerical input or ROBOTIC for the robotic mode 1 ENT Input the X1 coordinate 57 1 ENT Input the X2 coordinate 178 6 ENT Input an Nx value 10 ENT Input the Y1 coordinate 0 0 ENT RACK CODE 1 16 1 OPERATION MODE INPUT VALUE 1 1 ROBOTIC 2 X1 0 0 180 0 mm 57 1 X2 0 0 180 0 mm 178 6 Nx 1 40 10 Y1 0 0 155 0 mm UTILITY SEQ 1 RACK 2 WASH PARAM 3 1 OTERS 4 0 0 to...

Page 871: ... 5 ENT 2 ENT Input an Nx value 10 ENT Input an Ny value 12 ENT Input a pattern code 5 ENT Y2 0 0 155 0 mm 148 5 Ny 1 40 12 Z 0 0 53 0 mm 34 0 PATTERN CODE 1 8 5 Monitor screen reappears Nx 1 40 10 Ny 1 40 12 PATTERN CODE 1 8 MOVING WAIT 5 to be continued 3 27 ...

Page 872: ...ent in the same procedure as in 2 v Press the ENT key to start adjustment of the last vial position NOTE For fine adjustment in a vial with Z movement be sure to perform X Y adjustments to make sure the needle can be inserted into the vial before Z movement into the vial The Z shift value in this operation will not be taken into the rack parameter Be sure to perform Z adjustment in the following a...

Page 873: ... iv Perform fine adjustment in the same procedure as in 2 and 3 v Press the ENT key to terminate NOTE For fine adjustment in a vial with Z movement be sure to perform X Y adjustments to make sure the needle can be inserted into the vial before Z movement into the vial The Z shift value in this adjustment will be taken into the rack parameter So be sure to perform Z For adjustment with the needle i...

Page 874: ...ct the needle 1 ENT Input a needle wash time with the wash fluid1 15 ENT Input a needle wash time with the wash fluid2 15 ENT 2 ENT Input a rinse port wash time ENT WASH PARAM MANUAL WTIME 1 1 INJ WTYPE 2 INJ WTIME 3 MANUAL WTIME NEEDLE 1 RINSE PORT 2 1 PUMP PLUNGER 3 NEEDLE WASH TIME SOLVENT1 1 999 s 15 Monitor screen reappears NEEDLE WASH TIME SOLVENT2 1 999 s 15 Monitor screen reappears RINSE P...

Page 875: ...INJ WTYPE Setting the washing conditions during execution of a sequential program INJ WTIME Setting the washing time during execution of a sequential program 2 ENT Select an execution of needle wash before an injection 0 ENT 1 ENT WASH PARAM MANUAL WTIME 1 2 INJ WTYPE 2 INJ WTIME 3 NEEDLE WASH BEFORE INJ YES 1 NO 0 0 WASHING SOLVENT SOLVENT 1 1 SOLVENT1 2 2 Select an execution of pump plunger wash...

Page 876: ...eedle 1 ENT Input a needle wash time with the wash fluid1 15 ENT Input a needle wash time with the wash fluid2 15 ENT 2 ENT Input a rinse port wash time 15 ENT WASH PARAM MANUAL WTIME 1 3 INJ WTYPE 2 INJ WTIME 3 INJ WASH TIME NEEDLE 1 RINSE PORT 2 1 PUMP PLUNGER 3 NEEDLE WASH TIME SOLVENT1 1 999 s 15 Monitor screen reappears NEEDLE WASH TIME SOLVENT2 1 999 s 15 UTILITY SEQ 1 RACK 2 WASH PARAM 3 3 ...

Page 877: ...NT 1 ENT PUMP PLUNGER WASH TIME 1 999 s 15 Monitor screen reappears OTHERS LEAK SENSOR 1 VIAL SENSOR 2 1 ERROR OUT 3 BUZZER 4 INJ LEAK SENSOR OFF 0 ON 1 0 UTILITY SEQ 1 RACK 2 WASH PARAM 3 4 OTHERS 4 Monitor screen reappears VIAL SENSOR OFF 0 ON 1 1 Monitor screen reappears Monitor screen reappears Monitor screen reappears continued to be continued 3 33 ...

Page 878: ... occurrence of an error or DISABLE for avoiding it In case of ENABLE ERROR OUT will be issued if a mechanism error or an error on thermostat control is detected Refer to 4 5 And ERROR OUT will be issued when liquid leak has occurred 0 ENT 1 ENT 4 ENT A sample can be injected in a volume determined by multiplying the injection volume set in a sequential program with the injection volume correction ...

Page 879: ...1 ENT Input the number of the part to be checked or reset 1 ENT Select 1 for logbook display or 2 for resetting the logbook 1 ENT This screen displays the number of needle insertions into the injection port after the latest replacement of the injection port seal and the date of the replacement ENT or ESC STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 GLP LOGBOOK 1 KEY LOCK 2 1 LOGBOOK REPORT ...

Page 880: ...of all the inputs up to year the logbook is reset 2010 ENT Monitor screen r 2 ENT Select 1 for logbook display or 2 for resetting the logbook 1 ENT This screen displays the number of injection valve switchings to the LOAD side after the latest replacement of the injection valve seal and the date of the replacement ENT or ESC eappears LOGBOOK REPORT 1 RESET 2 1 INJ VALVE SEAL LAST CHANGED DATE 23 t...

Page 881: ...ook 1 ENT This screen displays the number of syringe movements to the 0 μL position after its replacement and the date of the replacement ENT or ESC INJ VALVE SEAL CHANGE MM DD YYYY 1 12 1 1 2000 INJ VALVE SEAL CHANGE MM DD YYYY 1 31 6 1 2000 INJ VALVE SEAL CHANGE MM DD YYYY 2000 2100 6 2 2000 Monitor screen reappears LOGBOOK REPORT 1 RESET 2 1 SYRINGE LAST CHANGED DATE 23 times 1 1 2000 Monitor s...

Page 882: ... logbook 1 ENT This screen displays the number of syringe valve switchings to port 1 after the latest replacement of the syringe valve seal and the date of the replacement ENT or ESC SYRINGE CHANGE MM DD YYYY 1 12 1 1 2000 SYRINGE CHANGE MM DD YYYY 1 31 6 1 2000 SYRINGE CHANGE MM DD YYYY 2000 2100 6 2 2000 Monitor screen reappears LOGBOOK REPORT 1 RESET 2 1 S VALVE SEAL LAST CHANGED DATE 23 times ...

Page 883: ...f replacement 2 ENT S VALVE SEAL CHANGE MM DD YYYY 2000 2100 6 2 2000 Input the year of replacement Upon completion of all the inputs up to year the logbook is reset 2010 ENT Monitor screen reappears 5 ENT 1 ENT ENT or ESC LOGBOOK REPORT 1 RESET 2 1 Monitor screen reappears WASHING PUMP LAST CHANGED DATE 23 h 1 1 2000 continued to be continued 3 39 ...

Page 884: ...put the date of replacement 2 ENT WASHING PUMP CHANGE MM DD YYYY 2000 2100 6 2 2000 Input the year of replacement Upon completion of all the inputs up to year the logbook is reset 2010 ENT Monitor screen reappears 2 ENT KEY LOCK YES 1 NO 0 Select 1 for key lock to prevent mistyping Press ESC key to release it 1 ENT 0 Monitor screen reappears 3 40 ...

Page 885: ...E I 1 1 1 10 0 1 1 0 0 FUNC TUBE 1 MOVE 2 HEIGHT 3 SYR 4 1 VALVE 5 SVALVE 6 SPURGE 7 WPUMP 8 1 ENT TUBE RACK CODE VIAL NO 0 16 1 1 FUNC Input a rack code TUBE RACK CODE VIAL NO 1 500 1 1 1 ENT MOVING B WAIT 1 ENT IDLE PRESS FUNC KEY OR IDLE KEY W FUNC ESC ESC EESC Input a vial number The needle moves to the specified vial position For rack code input any other than 0 1 to 16 0 ENT MOVING B IDLE WA...

Page 886: ...edle replacement position The needle moves to the specified position Wash port and Injection port is ESC 2 ENT FUNC Monitor screen reappears MOVING B WAIT PRESS IDLE KEY W IDLE The mechanism position is initialized because the mechanism might be deviated due to needle replacement MOVING B IDLE WAIT MOVING B IDLE WAIT Monitor screen reappears 3 42 ...

Page 887: ...VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 FUNC FUNC TUBE 1 MOVE 2 HEIGHT 3 SYR 4 2 VALVE 5 SVALVE 6 SPURGE 7 WPUMP 8 2 ENT ESC MOVE X Y 0 0 180 29 7 0 0 MOVE X Y 0 0 155 0 14 5 0 0 e g 14 5 ENT MOVING B WAIT e g 0 ENT IDLE PRESS FUNC KEY OR IDLE KEY W FUNC ESC ESC Input an X coordinate value Input an Y coordinate value The needle moves to the specified coordinates Z is located at 0 uppermost point MOVI...

Page 888: ...G B WAIT 2 ENT IDLE PRESS FUNC KEY OR IDLE KEY W FUNC ESC ESC Input a desired height Input a needle moving speed 1 The needle will move at the low speed Select this speed for using a hard septum etc 2 The needle will move at the high speed Usually this speed is used However for moving the needle upward the needle will move at the high speed irrespective of the setting made here The needle moves to...

Page 889: ... SPEED 0 690 0 0 0 4 SYRINGE VOLUME µL SPEED 1 5 100 0 4 e g 100 ENT MOVING B WAIT e g 4 ENT PRESS FUNC KEY OR IDLE KEY W FUNC IDLE ESC ESC Input a desired volume up to which the syringe is to be moved Input a syringe speed The syringe moves to the specified volume position The syringe valve position will be switched over automatically according to the syringe movement MOVING B IDLE WAIT Monitor s...

Page 890: ... will be switched over automatically according to the syringe movement To the port3 aspiration movement To the port4 discharge movement NOTE When it is discharge movement wash fluid in the syringe will be discharged to the port4 side of the syringe valve In this case remove the closed cap in port4 of the syringe valve before the SYR command is carried out Without removing it reduces the lifetime o...

Page 891: ...0 FUNC FUNC TUBE 1 MOVE 2 HEIGHT 3 SYR 4 5 VALVE 5 SVALVE 6 SPURGE 7 WPUMP 8 5 ENT ESC VALVE INJECT 0 LOAD 1 1 MOVING B WAIT 1 ENT PRESS FUNC KEY OR IDLE KEY W FUNC ESC Select an injection valve position Injection valve position is now shifted IDLE MOVING B IDLE WAIT Monitor screen reappears 3 47 ...

Page 892: ... 3 SYR 4 6 VALVE 5 SVALVE 6 SPURGE 7 WPUMP 8 ESC 6 ENT SVALVE RINSE PORT 1 NEEDLE 2 1 SYRINGE 3 PUMP PLUNGER 4 MOVING B WAIT 1 ENT PRESS FUNC KEY OR IDLE KEY W IDLE FUNC ESC Select a port to which the syringe valve is to be switched The syringe valve is now switched to the specified port MOVING B IDLE WAIT Monitor screen reappears 3 48 ...

Page 893: ...he stop valve from port 7 of the syringe valve STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 FUNC FUNC TUBE 1 MOVE 2 HEIGHT 3 SYR 4 7 VALVE 5 SVALVE 6 SPURGE 7 WPUMP 8 7 ENT ESC MOVING B IDLE WAIT 3 ENT SYRINGE PURGE STROKES SPEED 1 20 3 5 PRESS FUNC KEY OR IDLE KEY W IDLE FUNC ESC SYRINGE PURGE STROKES SPEED 1 5 3 5 5 ENT ESC MOVING B IDLE WAIT Monitor screen reappears 3 49 ...

Page 894: ... key STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 FUNC FUNC TUBE 1 MOVE 2 HEIGHT 3 SYR 4 8 VALVE 5 SVALVE 6 SPURGE 7 WPUMP 8 8 ENT ESC WPUMP PURGE OFF 0 SOLV1 1 SOLV2 2 0 PRESS FUNC KEY OR IDLE KEY W IDLE FUNC ESC Select the purging state of a wash pump 0 OFF 1 Wash fluid1 is purged 2 Wash fluid2 is purged 1 ENT e g MOVING B IDLE WAIT Monitor screen reappears 3 50 ...

Page 895: ...NIT NO USE 0 USE 1 1 1 ENT SETUP ITEMS THERMO UNIT 1 CONTRAST 2 1 ENT Turn off power supply and turn it on again UTLTY SET UP POWER ON SETUP THERMO UNIT CONTRAST S NO A S NO USE 4 02AB 111 Turn on power supply with the UTLTY key held down Indicates a serial No product No Enter 0 for avoiding use of the thermostat and 1 for selecting its use When turning on power supply again the instrument starts ...

Page 896: ...HERMO UNIT 1 CONTRAST 2 2 ENT Turn off power supply and turn it on again UTLTY SET UP POWER ON SETUP THERMO UNIT CONTRAST S NO A S NO USE 4 02AB 111 Turn on power supply with the UTLTY key held down Indicates a serial No product No Enter a contrast level When turning on power supply again the instrument starts under the set conditions 3 52 ...

Page 897: ...he thermostat is not connected or its use is not set a Temperature setting A set temperature can be input THERMO 1 ENT Input a desired set temperature 10 ENT e g STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 THERMO UNIT SET TEMP 1 CALIBRATION 2 1 TOLERANCE 3 SERIAL NO 4 TEMPERATURE 1 45 C 10 Monitor screen reappears 3 53 ...

Page 898: ...easured with a calibrated thermometer is 10 5 C the difference correction value offset value is 0 5 So setting is required as follows THERMO 2 ENT Select on which side there is a difference plus side or minus side e g 1 ENT Set an offset value for correction e g 0 5 ENT ENT or ESC STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 THERMO UNIT SET TEMP 1 CALIBRATION 2 2 TOLERANCE 3 SERIAL NO 4 The...

Page 899: ...y And for temperature calibration on multiple thermostats be sure to correct all thermostats at the same temperature 3 In the thermostat its aluminum block is subjected to temperature control Therefore a temperature difference occurs between the set temperature and the liquid temperature in a sample vial If it is necessary to control the absolute liquid temperature you should measure the liquid te...

Page 900: ...n case the use of tolerance is selected by entering 1 YES the instrument remains in the standby status does not launch a sequential program until the present temperature of the thermostat enters a range of the set temperature tolerance STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 THERMO THERMO UNIT SET TEMP 1 CALIBRATION 2 3 TOLERANCE 3 SERIAL NO 4 3 ENT USE TOLERANCE YES 1 NO 0 0 ENT 1 1 E...

Page 901: ...rial No product No of the thermostat can be indicated STEP RACK VIAL VOL µL INJ TIME I 1 1 1 10 0 1 1 0 0 THERMO THERMO UNIT SET TEMP 1 CALIBRATION 2 4 TOLERANCE 3 SERIAL NO 4 4 ENT THERMO UNIT PROGRAM NO S NO 00 02A 111 ENT or ESC Monitor screen reappears 3 57 ...

Page 902: ...e STOP key to suspend operation during an analysis The analysis will be suspended and autosampler will wait for the IDLE key press 4 The other units such as the pump are suspended NOTE If a solvent containing salt is used for a mobile phase it causes damages such as the surface of the valve seal and the flow path clogging Additionally it is resulting in deterioration of performance or shorter serv...

Page 903: ...peration immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemicals If a flammable chem...

Page 904: ...y For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper protective clothes e g safety goggles so that a solvent will not come into direct contact with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor 3 60 ...

Page 905: ... of pipings of pump and separation column use stainless steel SUS316 solvents or reagents that may corrode stainless steel may be restricted Especially solvents or solutions which contain halogen ions such as HCl KCl NaCl NH4Cl are typical reagents Reagents which may be restricted are shown in Table 3 2 use the table as a rough standard c Degas the mobile phase before use without fail It is recomm...

Page 906: ...ace or tip resulting in degradation in performance or shorter service life e Avoid using an alkaline solvent pH 8 or higher for washing as it may deteriorate the glass surface of the inside of the syringe resulting in degradation in performance or shorter service life f When the all loop injection method is applied a wash fluid in a buffer tube and a sample are introduced to the flow path together...

Page 907: ...d necessarily wash all the flow paths with distilled water completely without fail Do not use reagents that corrode SUS316 though they are not shown in the table above High viscosity solvent won t be delivered so please be careful Table 3 3 Isocratic Analysis One Fluid Wash standard for Cut injection method Full loop injection method Two Fluids Wash for All volume injection method Low carry over a...

Page 908: ...or wash fluid b Special membrane c Vacuum container d Solenoid valve e Pressure sensor f Control circuit board g Vacuum pump h Liquid delivery pump The liquid which needs to be degassed passes through the special synthetic resin membrane placed in the vacuum container in the degassing unit The gas dissolved in liquid has a small molecular size and its mobility and affinity to the resin membrane ar...

Page 909: ... 1 Example of Filtering of Mobile Phase by Using Membrane Filter Removing dust and degassing can be performed simultaneously by filtration with a 0 45 μm membrane filter Membrane filter Removing Dust from Mobile Phase by the Membrane filter NOTE Remove dust from mobile phase by using a 0 45 μm membrane filter Do not use filter paper because it generates dust 3 65 ...

Page 910: ...ormality is found stop operation immediately Leakage of solvent or waste solution Leakage of solvent inside the instrument When using flammable chemicals be careful about possible ignition due to static electricity To prevent the build up of static electricity use a conductive container for waste solution and provide proper grounding connection to it WARNING Explosion of Vapor from Flammable Chemi...

Page 911: ...y For details of the properties of each solvent and how to handle it refer to the relevant Material Safety Data Sheets MSDS Be sure to handle each solvent properly a Wear proper protective clothes e g safety goggles so that a solvent will not come into direct contact with the skin b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor 3 67 ...

Page 912: ...8 1 378 1 496 1 389 1 525 1 501 1 424 1 353 1 442 1 443 1 424 1 394 1 408 1 445 1 381 1 400 1 359 1 422 1 370 1 362 1 410 1 586 1 387 1 394 1 344 1 510 1 38 1 361 1 329 1 427 1 372 1 333 210 210 210 210 210 210 210 380 265 225 220 290 220 225 285 225 280 220 290 245 245 330 220 230 330 380 220 260 260 210 275 380 210 305 220 210 210 210 210 40 21 7 46 1 20 17 8 30 12 8 9 4 o 17 2 m 25 p 25 27 8 32...

Page 913: ...nts whose boiling point is 55 C or higher Solvents of low boiling point are not only dangerous but also generate bubbles when sucked by pump so that normal pumping will be impossible 3 When performing high sensitivity analysis with UV detector use solvents which absorb especially small amount of UV light Since special grade reagents such as methanol and acetonitrile generally used absorb the short...

Page 914: ...ctive container for waste solution and provide proper grounding connection to it Since flammable organic solvents are used for the High Speed Liquid Chromatograph be careful about heat and fire Since thin tubings are used for the liquid chromatograph static electricity is easily generated If charged liquid is collected into an insulated waste container for example and an electric discharge occurs ...

Page 915: ...ning solution as in the case mentioned above The internal capacity per flow path of the degassing unit including its tubing connection is approx 12 mL For complete displacement it is therefore required to feed approx 30 mL of solvent per flow path When performing displacement using the pump set a flow rate to 5 mL min or less to prevent formation of air bubbles 2 Periodically replace mobile phase ...

Page 916: ...he connection tubing with a new one thoroughly and then proceed to analytical operation 3 5 2 Sample Pretreatment 1 Filter samples without fail if they may contain fine dust Dust can clog column and deteriorate it 2 Remove foreign matter from samples without fail Foreign matter can lower the reliability of data e g generating abnormal peaks etc a Example of Filtering Samples Dust in sample can be ...

Page 917: ...emoving foreign matter 3 5 3 Preparatory Operations of Autosampler Proper 1 Check that the autosampler is correctly connected to the pump and detector before turning on the power 2 Check that the drain tube is correctly connected to the waste solution bottle The waste bottle must be positioned at a level lower than the autosampler 3 Prepare other components to be connected to the autosampler refer...

Page 918: ...air bubbles in the pipe from the wash pump to the syringe valve 9 Press the FUNC key of the autosampler and select SPURGE to fill the syringe with wash fluid Then make sure that there are no air bubbles in the syringe and port4 of the syringe valve discharges waste solution 10 Press the WASH key of the autosampler and select NEEDLE side to fill the needle and the injection port with wash fluid1 Wh...

Page 919: ...g for changeover from amino acid analysis to liposoluble vitamin analysis 2 Storage of Column When leaving the column unused for a long time fill it with a solvent and seal its outlet and inlet a Run a solvent through the column continuously at a flow rate of 0 2 mL min 0 02 mL min for a semi micro type of column b Remove the outlet tubing and attach the sealing plug to outlet c Stop the pump d Re...

Page 920: ...er Aspirator Absorbance Wavelength 4 Cleaning of Micro syringe a After and before sampling wipe off the needle of a micro syringe b Before aspiring a wash fluid wipe off the needle and wash the inside of the syringe repeatedly i e seven times or more c After injection wash the syringe immediately 5 Fastening of Connection Tube If the Teflon tube is overtightened its inside diameter is made smaller...

Page 921: ...Finger tighten the Teflon tube Column Setscrew made of SUS Fasten the SUS pipe 6 Handling of Detector When the autosampler is to be left unused for a long time wash the inside of the detector short circuit the outlet and inlet and seal the detector with proper liquid filled in it 7 Replacement of Consumable The replacement time of each consumable differs depending on the condition of use Be sure t...

Page 922: ...ly If the mobile phase and the washing solution are not deaerated sufficiently the full performance of this instrument may not be attained NOTE Set the washing solution bottle at a position higher than the autosampler If it is placed at a position lower than the autosampler a negative pressure may be produced in the piping to form air bubbles in the syringe disabling achievement of the full perfor...

Page 923: ...the combination used for your practical application refer to 3 2 and check the reproducibility performance before proceeding to operation NOTE For good reproducibility avoid using a septum repeatedly to prevent a cause of a hole It causes a fluctuation of sample concentration in sample vial NOTE Be sure to use the sample vials caps and septa recommended by Hitachi High Technologies refer to 6 3 If...

Page 924: ...on bottle must be at a lower position than the autosampler 4 Prepare other units to be connected to the autosampler as described in the respective instruction manuals 5 Put the drain tube from the detector into the exclusive detector waste liquid bottle If this tube is put into other waste solution bottle such as for Chromaster 5210 autosampler baseline fluctuation may be caused due to unstable ba...

Page 925: ...fluid When two wash fluids are used replace the wash fluid2 side with fresh one Then make sure that there are no air bubbles in the pipe from the wash pump to the syringe valve 10 Press the FUNC key of the autosampler and select SPURGE to fill the syringe with wash fluid Then make sure that there are no air bubbles in the syringe and port4 of the syringe valve discharges waste solution 11 Press th...

Page 926: ...mL min 15 Set the detector wavelength to 265 nm Set the detector time constant to 0 1 s 16 Set the following conditions in the data processing unit SAMPLE PERIOD 100 ms STOP TIME 3 min 4 1 3 Reproducibility Check Check the reproducibility of the injection volume in the following procedure 1 Press the PROG key and set the following conditions STEP RACK VIALS VOL µL INJ TIME 1 1 1 1 10 0 6 3 0 Press...

Page 927: ...during analysis 6 Upon completion of analysis the operation of the system stops with the initial screen displayed Instead of the initial screen the ALL END screen will appear if ALL END is set In this case the initial screen appears when you press the IDLE key 7 Data Check Determine the Relative Standard Deviation RSD of peak area by the following calculations Mean value n xi x n 1 i Standard devi...

Page 928: ...producibility with high precision required NOTE Before starting an analysis select the NEEDLE side by pressing the WASH key of the autosampler to fill the needle the injection port and the buffer tube with deaerated wash fluid1 or wash fluid2 when it is used Otherwise the deaeration state of the wash fluid in the flow path will be changing gradually so reproducibility just after the analysis start...

Page 929: ...roducibility of the system 1 When using an aqueous detergent At the end of measurement wash the flow path with distilled water If contamination is heavy fill the syringe with detergent and leave it overnight After cleaning the syringe rinse it with distilled water If the instrument will not be used for a week or loner wash the flow path adequately with distilled water and keep the syringe filled w...

Page 930: ... results may be degraded and or carry over may increase 2 Clean the immersion filter for detergent periodically Refer to 5 11 If the filter is clogged the detergent will not flow and performance may become poor 4 2 4 Waste solution tube The waste tubes in the system are made of materials having a high chemical resistance EPDM ethylene propylene diene monomer For these tubes however be careful abou...

Page 931: ... detect high volatile solvents Always check leakages to prevent a serious situation iii Daily visual check for leakages is required iv The periodic check for the leak sensor performance is required 2 Cleaning of the leak sensor Preparation A hexagon wrench P N N315003 Size B2 5 a Loosen the leak sensor set screw with the hexagon wrench Remove the leak sensor from the drain tray b Wipe up droplets ...

Page 932: ... b Ventilate the laboratory room adequately to prevent accidental inhalation of harmful solvent vapor Refer to the following procedure and perform operation check and cleaning for drain tray 1 Loosen the leak sensor set screw with the hexagon wrench Remove the leak sensor from the drain tray NOTE Avoid damage of the tip part of the leak sensor It may cause errors 2 Pull out the drain tray from the...

Page 933: ...sh port After wash port cleaning adjust it to the correct location 1 Turn on power supply to the autosampler Fig 4 3 Front View 2 Using the MOVE command on the UI pad move the needle so that the wash port can be removed easily FUNC 2 ENTER 1 8 0 ENTER 1 5 5 ENTER 4 12 ...

Page 934: ...remove the wash port Other screws should not be loosened 4 Replace it with a new wash port Or carry out ultrasonic cleaning 5 Fix the wash port temporarily 6 Detach the lid from the wash port 7 Using the MOVE command move the needle to the design position of the wash port X 29 7 mm Y 0 mm FUNC 2 ENTER 2 9 7 ENTER 0 ENTER 4 13 ...

Page 935: ... 8 Using the HEIGHT command lower the needle by about 5 mm FUNC 3 ENTER 5 ENTER 1 ENTER Retaining screw 1 Retaining screw 1 Retaining screw 2 Fig 4 5 Height Adjustment of Needle 4 14 ...

Page 936: ... to the procedure 2 to readjust the wash port and fix it temporarily 10 When the wash port is located just below the needle move the needle once again refer to 2 and fix the washing port 11 After adjustment press the IDLE key to set the needle to its home position Mount the needle cover in place 4 15 ...

Page 937: ...etergent in the flow path is not deaerated sufficiently a Repeat the WASH operation several times to get rid of air Fill the flow path with the deaerated detergent refer to 3 4 2 b The injection port leaks b Check the lock nut and retighten if loose Or replace the port seal c The syringe valve leaks c Check that the fixing screws are tightened properly not tightened unevenly Or replace the valve s...

Page 938: ...se the slit septum refer to 4 1 1 p In present use septum has a hole p Replace it with a new one q The front door refer to 2 1 is open during an analysis q Close the front door during an analysis r The wash pump leaks r Check the wash pump setscrew and retighten if loose Make sure the tip of tube is not deformed or the ferrule is not crushed s Air bubbles in the wash pump s Fill it with deaerated ...

Page 939: ...mn performance is poor j Wash or replace the column 4 Carryover occurs k The vial detection lever is contaminated due to sample vial k Attach a cap to the sample vial Wash the vial detection lever a An insufficient sample volume is used a Increase the sample volume b The injection port leaks b Check the lock nut and retighten if loose Or replace the seal c The flow path has clogged c Replace the t...

Page 940: ...t step No which is not contained in a sequential program is set 2 Setting of a start step No which is not contained in a sequential program was attempted by the UTILITY function 9 CHECK TOTAL VOL An injection volume that cannot be handled with the mounted syringe is set Check and correct the set parameter value 10 START KEY IS NOT ACCEPTABLEDOOR IS OPEN When starting analysis pressing the START ke...

Page 941: ...nologies Corporation sales representative 15 STOPPED BY EXTERNAL ERROR An error has occurred in other unit connected Eliminate the cause of the error to release the error status 16 SEQ PROGRAM BUFFER OVERFLOW Communication is abnormal Contact your nearest service office of Hitachi High Technologies Corporation sales representative 1 The sample rack or sample vial is blocking movement 1 Set the sam...

Page 942: ...gh Technologies Corporation sales representative 1 The syringe valve seal has worn out 1 Replace the seal 2 The inside of syringe valve is dried up 2 Fill the valve with fluid and retry operation 21 ERROR SVALVE 3 The electric system malfunctions 3 Contact your nearest service office of Hitachi High Technologies Corporation sales representative 1 The injection valve seal has worn out 1 Renew the s...

Page 943: ... is not connected 2 Power supply of the thermostat is cut off after initialization 1 Check proper connection of the power cord and clear the message 2 Check proper connection of the power cord and turn on power supply again 6 THERMO UNIT IS NOT CONNECTED The thermostat is set in the USE status though the autosampler is not equipped with this unit Set the thermostat in the NO USE status 7 ABNORMAL ...

Page 944: ...h a margin in quantity depending on the actual operating conditions NOTE Please replace service parts and consumables in this instruction manual by the specified cycle It may causes malfunction of the instrument without replacing them Table 5 1 Consumables Part No Name Form Specification Location Estimated Life Standard Life 080 3595 Sample vial 500 pcs Sample vial 855 2351 Septum 100 pcs slit Sam...

Page 945: ... 20 000 injections 893 0817 Syringe 70 µL Syringe valve Two years Syringe option 20 000 plunger reciproca tions φ12 φ34 φ12 92 5 1 2 Spare Parts It is desired to prepare the items listed below for running the system for a long time Each item should be prepared in an adequate quantity depending on the operation time Table 5 2 Spare Parts Part No Name Form Location Remarks 810 1337 Solvent filter Wa...

Page 946: ... firmly it may become loose during operation of the instrument to cause such a fault as liquid leakage or unpredictable stop of analysis SUS pipe installation To connect a new pipe Ferrule not yet caulked To reconnect an existent pipe Ferrule already caulked Angle of re tightening 270 to 360 30 to 60 SUS ferrule SUS pipe SUS setscrew NOTE In a case where the setscrew is made of resin just finger t...

Page 947: ...er P N 893 2115 1 Loosen the injection port with your hand And remove it from the injection valve Injection port Injection valve Fig 5 1 Removal of Injection Port 2 Insert a seal remover into the injection port And remove an injection port seal Injection port seal Injection port Insert a seal remover into the injection port Remove an injection port seal Seal remover Fig 5 2 Removal of Injection Po...

Page 948: ...on port seal to the injection port side when attach it 2 Tighten the injection port with your hand until it is finger tight 3 Avoid using tools to prevent the injection port seal from deformation 4 After replacing the injection port seal press the WASH key to carry out injection port cleaning NOTES 1 After replacement of the injection port seal U make sure liquid is not leaking through the seal 2 ...

Page 949: ...ng the UI pad move the needle to the replacement position Refer to 3 2 2 Analyzing Operation 5 Functions a TUBE for details FUNC 1 ENTER 0 ENTER 2 ENTER 3 Using a wrench 5 16 inch to remove the flange needle while holding the screw on the needle joint side with wrench 12 mm Needle joint Flange needle Fig 5 4 Removal of the Flange Needle 5 6 ...

Page 950: ...de with wrench 12 mm 7 Check a setscrew If it is loosening tighten the setscrew while holding the screw on the needle joint side with wrench 12 mm Setscrew Fig 5 5 Setscrew Check 8 After replacing the flange needle press the IDLE key on the UI pad to set the needle to its home position 9 After replacing the needle press the WASH key to wash the needle NOTE After replacement of the flange needle ch...

Page 951: ...d a syringe valve Syringe Beaker Distilled water Wash fluid Syringe 175 µL P N 893 0815 Syringe 70 µL P N 893 0817 option 1 Remove the sealing screw connected to the port 4 of the syringe valve Plunger setscrews Syringe valve Sealing screw Hook Syringe Syringe mount Fig 5 6 Syringe Valve 5 8 ...

Page 952: ...OTE When 70 µL optional syringe is used using the SYR command aspirate 70 µL of wash fluid 4 Using the SVALVE command select port 1 RINSE PORT FUNC 6 ENTER 4 ENTER Refer to 3 2 2 Analyzing Operation 5 Functions f SVALVE 5 Loosen the plunger setscrew with your hand to remove the syringe from the hook 6 Turn the top end threaded metal part of the syringe counterclockwise with your hand to separate t...

Page 953: ...at the time of syringe mounting will be purged through port 4 PUMP PLUNGER 10 Secure the plunger setscrew with your hand to fasten the plunger groove with the hook 11 Press the SPURGE key to replace fluid with wash fluid of the syringe Refer to 3 2 2 Analyzing Operation 5 Functions g SPURGE for details Or refer to 5 6 Discharge of Air Bubbles from Syringe to avoid air bubbles 12 Press the IDLE key...

Page 954: ...e to be reset by pressing the IDLE key 5 When fitting the plunger groove of syringe into the hook make sure the plunger setscrew is secured If it is loose the instrument will not provide the original performance 6 When filling the syringe with a liquid take care not to forcedly press the tip precision part of the plunger against the top wall of the syringe Otherwise the tip may deform to cause a r...

Page 955: ...between a syringe and a syringe valve 1 Remove the sealing screw from port5 of the syringe valve Syringe valve Sealing screw Fig 5 10 Syringe Valve 2 Connect the hypodermic syringe furnished plastic injector to port4 Hypodermic syringe Fig 5 11Connecting the Hypodermic Syringe or Tube 5 12 ...

Page 956: ...r you have completed eliminating air bubbles 5 Attach the sealing screw on the port4 of the syringe valve NOTES 1 If it is difficult to eliminate air bubbles from the syringe disconnect the syringe once for details refer to 5 5 Syringe Replacement With 2 propanol wash the inside of the syringe and then try to eliminate air bubbles 2 When filling the syringe with a liquid take care not to forcedly ...

Page 957: ... of the cell for a moment and then release it immediately Fig 5 12 Discharge of Air Bubbles from Syringe with Hypodermic Syringe 6 The hypodermic syringe can be stored in the wall of the autosampler using the provided pipe holder Fit in the pipe holder on the wall of the autosampler whichever you choose right or left side wall Fig 5 13 Setting the Pipe Holder 5 14 ...

Page 958: ... 7 Fit in the body of the hypodermic syringe to the pipe holder Put the tube from syringe valve port 4 to the downside and the piston to the upper side Fig 5 14 Fitting the Hypodermic syringe 5 15 ...

Page 959: ...h 1 4 inch disconnect the tubes and pipes from the injection valve port 1 to 5 Port 1 from the pump Port 2 to the column Port 5 drain tube Port 3 and 6 Loop Drain pipe Loop Injection valve Screw cap Fig 5 15 Disconnecting Tubes and Pipes from the Injection Valve NOTE Avoid loosing the screw cap Otherwise it may cause a reduction in service life or performance 2 Loosen three stator setscrews using ...

Page 960: ... setscrews Secure these setscrews in turn and by equal increments 6 In the reverse order of removal connect the tubes and pipes to the injection valve Refer to 5 2 7 After replacement of the injection valve seal check that there are no liquid leaks NOTES 1 While the inside of the valve is dry avoid moving the valve unless otherwise necessary Otherwise the plunger seal will sear out abnormally 2 If...

Page 961: ...r hand Port 1 Tube SV1 Port 2 Buffer tube Port 3 Tube SV3 Port 4 Sealing screw Port 4 Tube SV5 Screw cap Syringe valve Fig 5 17 Disconnection of Tubes and Pipes from Syringe Valve NOTE Avoid loosing the screw cap Otherwise it may cause a reduction in service life or performance 2 Loosen three stator setscrews using a hexagon wrench 9 64 inch and demount the injection valve stator 3 Pull out a stat...

Page 962: ...he stator setscrews Secure these setscrews in turn and by equal increments 6 In the reverse order of removal connect the tubes and pipes to the syringe valve 7 After replacement of the syringe valve seal check that there are no liquid leaks NOTES 1 While the inside of the valve is dry avoid moving the valve unless otherwise necessary Otherwise the plunger seal will sear out abnormally 2 If the val...

Page 963: ... a new one according to the same procedure Using the WPUMP command deliver wash fluid2 for about 3 minutes to replace the fluid of the flow path between the solvent filter and the wash port with the wash fluid2 FUNC 8 ENTER 1 ENTER 3 Check that there are no air bubbles in the tube between the wash pump and the syringe valve And check that operational noise of the washing pump is reduced NOTE If th...

Page 964: ...repared Hypodermic syringe A tube between a hypodermic syringe and a syringe valve Syringe Beaker Distilled water Wash fluid 1 Remove a setscrew from the port1 of the syringe valve with your hand Syringe valve Setscrew Syringe valve Fig 5 17 Syringe Valve 5 21 ...

Page 965: ...TER Refer to 3 2 2 Analyzing Operation 5 Functions h WPUMP for details NOTES To suspend delivering of the wash pump select OFF in the WPUMP PURGE screen or press the IDLE key Delivering fluid is not suspended automatically 4 After the fluid delivering by the wash pump press the hypodermic syringe plastic injector with your finger to apply proper pressure Then air bubbles can be removed with ease H...

Page 966: ...o be prepared Beaker Wash fluid 2 propanol Ultrasonic cleaner Distilled water 1 Loosen the cap of the wash fluid bottle Inlet tube Cap Wash fluid bottle 2 Pull out the inlet tube from the wash fluid bottle 3 Loose the setscrew with your hand and separate the solvent filter from the inlet tube Pull out Inlet tube Solvent filter 5 23 ...

Page 967: ...x 5 to 6 minutes Solvent filter Beaker Wash fluid Distilled water Ultrasonic cleaner 5 Then replace the wash fluid with distilled water and perform additional ultrasonic cleaning for approx 5 to 6 minutes 6 After removing water completely attach the solvent filter to the inlet tube Insert Inlet tube Solvent filter 5 24 ...

Page 968: ...eding to fuse replacement 1 Item to be Prepared New fuse P N J821336 Be sure to use a new time lag fuse meeting the specified 2 Pre check Before fuse replacement make sure that the power switch of the instrument is off and that the power cord is disconnected from it 3 Fuse Replacement Procedure a Remove the fuse holder while holding the tabs on both sides Tabs Fuse holder C941322 b Replace the exi...

Page 969: ...hermostat This unit is capable of cooling 120 sample vials 1 5 mL each within a temperature range from room temperature 21 C to room temperature 25 C or a setting range Rack holder Sample rack Fig 6 1 The Thermostat Table 6 1 Thermostat Part No Part Name Remarks Thermostat Sample rack for the thermostat is equipped 1 5 mL x 120 vials P N 892 0240 6 1 ...

Page 970: ...rks 892 0230 Sample rack for 1 5 mL x 120 vials Equipped as standard 892 0232 Sample rack for 4 mL x 72 vials 892 0234 Sample rack for 1 mL x 195 vials 892 0236 Sample rack for Microplate 96 or 384 holes x 2 plates Deep well plates are unsuitable 6 2 2 For Thermostat Used when a thermostat is installed Table 6 3 Sample Racks for Cooling Part No Part Name Remarks 892 0240 Sample rack for 1 5 mL x 1...

Page 971: ...pplication indicated in Table 6 4 to 6 11 and check the reproducibility performance before proceeding to operation NOTE For good reproducibility avoid using a septum repeatedly to prevent a cause of a hole It causes a fluctuation of sample concentration in sample vial NOTE Be sure to use the sample vials caps and septa recommended by Hitachi High Technologies indicated in Table 6 4 to 6 11 If othe...

Page 972: ...TFE 500 pcs contained Manufactured by Chromacol Ltd Without slit Septum type 8 TST1 080 3711 Septum Si PTFE 500 pcs contained Manufactured by Chromacol Ltd Without slit Septum type 8 ST14 080 3704 Screw cap black 500 pcs contained Manufactured by Chromacol Ltd Cap type 8 SC 890 3674 0 6 mL sample vial 500 pcs contained Manufactured by Chromacol Ltd Vial type 06 PESV φ12 32 mm polyethylene 892 0230...

Page 973: ...anufactured by Chromacol Ltd Without slit Septum type 8 TST1 080 3711 Septum Si PTFE 500 pcs contained Manufactured by Chromacol Ltd Without slit Septum type 8 ST14 080 3704 Screw cap black 500 pcs contained Manufactured by Chromacol Ltd Cap type 8 SC 080 3230 Support sleeve 50 pcs contained Manufactured by Chromacol Ltd Type TTS 312 Teflon The support sleeve is required for use on the sample rack...

Page 974: ...al 500 pcs contained Manufactured by Chromacol Ltd Vial type 4 SV φ15 46 mm 892 0232 892 0242 080 3701 4 mL sample vial brown 500 pcs contained Manufactured by Chromacol Ltd Vial type 4 SV A φ15 46 mm 080 1863 Septum Si PTFE 100 pcs contained With slit 080 3702 Screw cap black 500 pcs contained Manufactured by Chromacol Ltd Cap type 12 SC 6 6 ...

Page 975: ...230 892 0240 With blue mark 080 3768 1 5 mL crimp top sample vial 500 pcs contained Manufactured by Chromacol Ltd Vial type 2 CV G φ12 32 mm low alkaline glass With yellow mark 080 3598 1 5 mL crimp top sample vial blown 500 pcs contained Manufactured by Chromacol Ltd Vial type 2 CV A φ12 32 mm 080 3712 Crimp cap with septum 500 pcs contained Manufactured by Chromacol Ltd Cap type 11 AC TST1 with ...

Page 976: ... cap with septum 500 pcs contained Manufactured by Chromacol Ltd Cap type 11 AC TST1 with PTFE Si PTFE three layer septum Without slit on septum 080 3230 Support sleeve 50 pcs contained Manufactured by Chromacol Ltd Type TTS 312 Teflon The support sleeve is required for use on the sample rack When these vials are used for the sample rack 892 0240 cooling performance will be degraded The rack param...

Page 977: ...ated crimper tool To remove the cap use the decapper Part No Name Remarks 080 3232 Crimper CR 8 For sealing of 080 3226 080 3233 Crimper CR 11 For sealing of 080 3227 Crimper Decapper Part No Name Remarks 080 3258 Decapper DCR 8 For removal of 080 3226 080 3259 Decapper DCR 11 For removal of 080 3227 6 9 ...

Page 978: ...neckless sample vial brown 200 pcs contained Manufactured by National Scientific Company C4015 99 φ8 40 mm With polyethylene cap 890 3662 1 mL neckless sample vial transparent 200 pcs contained Manufactured by National Scientific Company C4015 9VO Without polyethylene cap 890 3665 1 mL neckless sample vial brown 200 pcs contained Manufactured by National Scientific Company C4015 99VO Without polye...

Page 979: ...set of 100 vials Manufactured by FUJIMOTO SCIENCE φ12 32 mm 892 0230 892 0240 With silicone rubber cap 805 2236 Neckless sample vial transparent set of 100 vials Manufactured by FUJIMOTO SCIENCE φ12 32 mm Without silicone rubber cap 080 1954 Silicone rubber cap set of 100 Manufactured by FUJIMOTO SCIENCE with 0 2 mm membrane 6 11 ...

Page 980: ... Pack 11190933 11150650 φ12 32 mm polypropylene With snap cap having septum Si PTFE with slit 890 3669 0 3 mL snap top sample vial 100 pcs contained La Pha Pack 11190933 φ12 32 mm polypropylene Sample vial only 890 3670 Snap cap with septum Si PTFE 100 pcs contained La Pha Pack 11150637 without slit 890 3671 Snap cap with septum Si PTFE 100 pcs contained La Pha Pack 11150650 with slit 890 3687 0 3...

Page 981: ...by Whatman Ltd 7704 0105 Silicone NOTE The plate seal in Table 6 13 is used exclusively for aqueous samples For organic solvent samples use each microplate by sealing it with the exclusive thermal fusing type sealer or the like NOTE Use microplate seals to prevent sample evaporation contamination fluid splash and increase constant temperature efficiency the well plate when the microplate is used O...

Page 982: ... 6 14 Optional Syringes Part No Part Name Remarks 892 0250 70 µL syringe kit Syringe 6 5 Degassing Unit 2ch degassing unit for the Chromaster 5210 Autosampler is indicated in the Table 6 15 Refer to the instruction manual of the optional 2ch degassing unit for details Table 6 15 2ch Degassing unit Part No Part Name Remarks 892 0260 2ch Degassing unit Tubes are equipped 6 14 ...

Page 983: ... Cable connection Cabling APPENDIX1 16 APPENDIX1 18 Cleaning 4 9 Consumables 5 1 D DEL delete 2 6 3 14 Dimensions 2 45 Drain tray 2 3 E ESC escape 2 6 3 11 ENT enter 2 6 3 11 External communication 2 45 e Line 2 4 2 45 APPENDIX1 18 F Fixing bracket APPENDIX1 12 Flow path 2 7 3 75 Frequency APPENDIX1 4 Function 2 1 G GLP 2 6 3 11 Grounding APPENDIX1 5 Grounding terminal 2 4 7 1 ...

Page 984: ...NDIX1 16 M Main switch 2 1 Maintenance 4 1 N Needle 2 4 2 8 Needle down speed Needle lowering speed 3 22 Needle replacement 5 6 Number of injection per samples 2 45 O Operation flow 3 11 Operation keys 2 5 P Packing list APPENDIX1 11 PAUSE 2 6 APPENDIX3 1 Performance specification check 4 1 Periodic maintenance 4 8 Power capacity APPENDIX1 4 Power cord APPENDIX1 15 Power supply voltage APPENDIX1 3...

Page 985: ...STEP 3 18 STEP 3 2 STOP 2 6 Sample injection method 2 9 2 44 Sample injection volume 3 2 Sample rack 2 2 3 6 6 2 Sample vial 3 2 5 1 6 3 Spare parts 5 2 Specifications 2 44 Suspend operation 3 58 Syringe 5 2 5 8 5 12 Syringe capacity 2 44 Syringe replacement 5 8 Syringe speed 3 21 4 5 Syringe valve 2 2 5 8 T Thermostat APPENDIX1 8 Tubing APPENDIX1 20 U UI pad 2 1 2 5 3 1 UTLTY Utility 2 6 APPENDIX...

Page 986: ...W WASH 2 6 4 4 5 5 Wash port 2 3 2 7 4 12 Washing condition 3 30 Waste solution tube 3 73 4 8 44 9 Weight 2 46 Wiring cover Cable cover 2 4 APPENDIX1 28 7 4 ...

Page 987: ...ench NOTE It is not permitted for the customer to carry out installation at the time of delivery For ensuring safety and high accuracy in operation of the instrument installation of the instrument shall be carried out by qualified service personnel trained by the manufacturer or its authorized maintenance service agent Before installation however the customer shall make adequate preparations for i...

Page 988: ... filled with gas of an organic solvent particularly benzine and paint thinner which dissolves coating 4 Other General Precautions on Instrument a Shall not be exposed to direct sunlight Otherwise performance degradation or coating discoloration might be caused Avoid a place near windows as far as possible b Shall not be exposed to draft c Shall be free from strong vibration or shock which can be f...

Page 989: ...all be free from a sudden change of power supply voltage Otherwise noise might be caused h Power supply to motor driven equipment such as stirrer and vibrator without a noise suppressor shall not be turned ON OFF frequently on the same power supply line as that of this instrument APPENDIX 1 3 ...

Page 990: ...otal system shown comprises Chromaster organizer Chromaster 5110 pump Chromaster 5210 autosampler Chromaster 5310 column oven and Chromaster 5410 5420 5430 5450 detector Check the necessary power supply requiretemnts and prepare a power supply meeting the specified requirements taking into account your actual system configuration and the OA equipment to be used in combination Power outlet Power su...

Page 991: ...pe of power cable may result in an electric shock hazard Connect the 3P power cable to a grounded 3P power outlet as a rule b If a grounded 3P power outlet is not available use a 3P table tap with a grounding wire or a 3P 2P adapter In this case please be sure to provide proper grounding connection For grounding connection use a screw having a diameter of M4 or larger and a turn count of 3 or more...

Page 992: ...unded 3P power outlet 15 A Ground resistance 100 Ω or less Grounding electrode underground section Grounding construction for 100 Ω or less Grounded 3P table tap Chromaster 5210 autosampler Connector Rear panel 300 mm 2 mm 10 mm Organizer or AC adapter option Appended Fig 1 1 Grounding Method APPENDIX 1 6 ...

Page 993: ...iameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Chromaster 5210 autosampler Connector Rear panel 300 mm 2 mm 10 mm Organizer or AC adapter option Appended Fig 1 2 Connection when Only 2P Power Outlet is Available ii 2 With 2P power outlet having a grounding terminal Power outlet with grounding terminal Grounding terminal 2P 3P adapter Grounding wire green Screw diameter M4 or larg...

Page 994: ...ground section 750 mm or more below ground Copper plate 300 mm 2 mm 10 mm Chromaster 5210 autosampler Rear panel Grounded 3P power outlet 15 A Grounded 3P table tap Power cord attached to instrument Connector Grounding construction for 100 Ω or less Ground resistance 100 Ω or less Grounding electrode underground section Grounded 3P power outlet 15 A Organizer or AC adapter option Thermostat Append...

Page 995: ...m 2 mm 10 mm Chromaster 5210 autosampler Rear panel Grounding electrode underground section Grounded 2P power outlet 15 A Grounded 3P table tap Power cord attached to instrument Connecto Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Grounding terminal Grounding construction for 100 Ω or less Ground resistance 100 Ω or less Grounded 2P power outlet 15 ...

Page 996: ...ion when Only 2P Power Outlet is Available Chromaster 5210 autosampler Rear panel 3P 2P adapter Grounding wire green Screw diameter M4 or larger Turn count 3 or more Wire thickness 1 25 mm Grounding terminal Power outlet with grounding terminal Connecto Power cord attached to the instrument Organizer or r r AC adapter option Thermostat ii 2 With power outlet with grounding terminal APPENDIX 1 10 ...

Page 997: ...ay become inadequate For installation prepare a level and sturdy bench which withstands a load of 150 kg or more The system conceived here is an example in which Chromaster organizer Chromaster 5110 pump Chromaster 5210 autosampler Chromaster 5310 column oven and Chromaster 5410 5420 5430 5450 detector are stacked Confirm the necessary space taking the actual system configuration and OA equipment ...

Page 998: ...instrument shall be carried out by qualified service personnel trained by the manufacturer or its authorized maintenance service agent Appendix 1 5 1 Removal of Transport Screws Remove the fixing brackets using a Phillips screwdriver NOTE Please do not miss and store the removed fixing brackets carefully for they may be used for transportation in case of relocation of the instrument if any APPENDI...

Page 999: ...Retaining screws Fixing bracket Appended Fig 1 5 Removal of Fixing Brackets APPENDIX 1 13 ...

Page 1000: ...ube Attach the waste solution tube to the waste solution tube mounting port Waste solution mounting port a Before attachment Drain tube A1 I joint Drain tube T joint b After attachment Appended Fig 1 6 Mounting of Waste Solution Tube APPENDIX 1 14 ...

Page 1001: ...master 5310 column oven and Chromaster fluorescence detector the power cord needs to be connected to the column oven unit If a single organizer is inadequate due to use of 2 detectors for example an AC adapter option that matches the detector concerned needs to be used Connect the power cable from the organizer or AC adapter to the power connector at the rear left of the detector Power connector e...

Page 1002: ...le 1 P N 892 6909 attached to organizer Connector cable 2 P N 892 6910 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 4 P N 892 6912 attached to organizer AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster 5210 autosampler a...

Page 1003: ...e Used Connector cable 1 P N 892 6909 attached to organizer Connector cable 3 P N 892 6911 attached to organizer Connector cable 5 P N 892 6914 separately available Connector cable 6 P N 892 6913 separately available AC power cable Use the power cable attached to each module unit Plug the power cables from the organizer and column oven into AC power outlets For the Chromaster 5110 pump Chromaster ...

Page 1004: ...to be connected are OFF 1 Isocratic System Low pressure Gradient System Chromaster organizer Chromaster 5410 5420 5430 5450detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump e Line cable 1 e Line cable 2 Appended Fig 1 10 e Line Cable Connection Appended Table 1 3 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e ...

Page 1005: ...hromaster 5210 autosampler Interface control board e Line cable 1 e Line cable 2 Chromaster organizer Chromaster 5110 pump Appended Fig 1 11 e Line Cable Connection Appended Table 1 4 Cables to be Used e Line cable 1 50 cm P N 890 6105 attached to each unit e Line cable 2 80 cm P N 890 6107 attached to autosampler fluorescence detector and interface control board APPENDIX 1 19 ...

Page 1006: ...sampler to the column is passed Central hole Through this hole the tube from the pump to the autosampler and that from the column to the detector are passed NOTE Please ensure that the detergent vial is located higher than that the autosampler main unit If it is located lower than the autosampler main unit it is possible that the instrument is prevented from achieving sufficient performance due to...

Page 1007: ...Chromaster 5410 5420 5430 5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Chromaster 5110 pump Degassing unit Drain Injection valve Column Syringe valve Appended Fig 1 12 Tubing Diagram of Isocratic System stacked in one block APPENDIX 1 21 ...

Page 1008: ...m stacked in two blocks Connect the inlet tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the inlet of pump Connect the purge valve of pump to port 4 of the injection valve in the autosampler Connect port 5 of the injection valve to the inlet of column To the outlet of column connect the inlet tube of detector cell Connect the deterg...

Page 1009: ...420 5430 detector Chromaster 5310 column oven Chromaster 5210 autosampler Wash pump Low pressure gradient unit proportioning valve Chromaster 5110 pump Drain Degassing unit Syringe valve Injection valve Appended Fig 1 14 Tubing Diagram of Low Pressure Gradient System stacked in one block APPENDIX 1 23 ...

Page 1010: ...et tube from the mobile phase container to the IN port of degassing unit Connect the OUT port of degassing unit and the IN port of proportioning valve Connect the OUT port of the proportioning valve in the low pressure gradient unit to the 4 way joint Then connect the purge valve of pump to port 4 of the injection valve in the autosampler Also connect port 5 of the injection valve to the inlet of ...

Page 1011: ... Pump Mobile phase 1 for analysis Degassing unit channel A Pump Mobile phase 2 for analysis Degassing unit channel B Pump Mobile phase 3 for analysis Degassing unit channel C Pump Mobile phase 4 for analysis Degassing unit channel D Autosampler Detergent 1 for analysis Degassing unit channel E Autosampler Detergent 2 for analysis Degassing unit channel F APPENDIX 1 25 ...

Page 1012: ...agram for Drain when stacking module units in one block Appended Table 1 3 Drain Tubes to be Used Drain tube A2 P N 893 2874 attached to organizer Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 P N 893 2872 attached to organizer Drain tube 4 P N 893 2873 attached to organizer Drain tube P N 080 3090 attached to autosampler T joint P N 810 1362 attached to organizer T joint N1 P N 8...

Page 1013: ...ng module units in two blocks Appended Table 1 6 Drain Tubes to be Used Drain tube B1 P N 893 2875 attached to organizer Drain tube A1 1 2 P N 893 2872 attached to autosampler Drain tube A1 3 P N 893 2872 attached to organizer Drain tube 1 P N 080 3090 attached to autosampler Drain tube 2 P N 080 3090 separately available T joint P N 810 1362 attached to organizer T joint N1 P N 890 3493 attached ...

Page 1014: ...ing between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over When installing the instrument fasten between the module units On the rear of each module unit a cabling cover is attached The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers Fastening plate Fastening screw Appen...

Page 1015: ...high accuracy in operation of the instrument installation of the instrument shall be carried out by qualified service personnel trained by the manufacturer or its authorized maintenance service agent 1 Turn off the power supply for the instrument 2 Shift the arm to the retaining position for transport by hand and attach the fixing brackets APPENDIX 1 29 ...

Page 1016: ......

Page 1017: ... via 3 pin connector Their names and functions vary with the unit A name that indicates the function is given at each connector Example of output contact signal EVENT of pump Example of input contact signal LAMP OFF IN of detector Appendix 2 2 Contact Signals Entering e Line Connectors Each unit has two e Line connectors at the rear of the main frame and the respective signals of these connectors ...

Page 1018: ...e DIO cable 890 6145 3 pin connector e DIO cable 890 6145 e Line connector To L 2000 series unit 2 Connection with D 2500 For connection use the e DIO cable 890 6146 START COM EXTERNAL H L BUSY BUSY START G L H e Line connector D 2500 To Chromaster series unit Connect the L and G terminals of the START line of e DIO cable 890 6146 to the COM terminal of D 2500 APPENDIX 2 2 ...

Page 1019: ...nals These are contact signal output terminals for control of an external unit using contact signals The output circuit is as shown in Appended Fig 1 20 The rating of contacts used is 12 V 0 1 A Make sure the load connected does not exceed this rating e Line cable Other unit Chromaster series unit A Chromaster series unit B Appended Fig 2 1 e Line Cable Connection Appended Fig 2 2 e Line Contact C...

Page 1020: ...er series Activated upon shorting contacts of external unit External unit Appended Fig 2 3 Contact Signal Input Circuit 30 V max 1 2 3 0 1 A max Chromaster series External unit Appended Fig 2 4 Contact Signal Output Circuit APPENDIX 2 4 ...

Page 1021: ...n interrupt analysis is performed Start A series of analysis is started Stop time Time set which is required for analyzing a sample and obtaining chromatogram After a lapse of such time a series of analysis for the next sample is started Septum Sheet used as the lid for a vial Loop injection method A sample injection method in which a sample is once after stored in a loop temporarily introduced in...

Page 1022: ...Sample rack A component part on which a sample is set Logbook A historical record of instrument operation APPENDIX 3 2 ...

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