PerkinElmer 200A Series User Manual Download Page 97

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Operation

The recorder setting screen appears.

RECORD (RCD RANGE=1, RCD SPEED=2,
3

SPECT RCD=3)

Press numeric key 3 and then ENT to select SPECT RCD (spectral recording).

The output data spectrum No. setting screen appears.

RECORD SPECTRUM NO. (1 - 4)
1

Press a numeric key 1 to 4 and then ENT to set a spectrum No. to be output.

Initial (default) value: 1

The background spectrum No. setting screen now appears.

The background spectrum is used to compensate for absorption by the solvent

or cell. To ensure that an appropriately corrected spectrum is used in analysis,

a new background spectrum should be acquired whenever the solvent or
wavelength scan range is changed.

BACKGROUND SPECTRUM NO. (0 ~ 4)
0

Press a numeric key 0 to 4 and then ENT to select whether or not to correct the output

spectrum.

0: Spectrum selected at RECORD SPECTRUM NO. will be output as it

is.

1 - 4: Spectral data obtained by subtracting the specified background

data from the spectrum selected at RECORD SPECTRUM NO. will be

output.

Initial (default) value: 0

When the energy spectrum and spectrum type are

mismatched, the error message indicated below will appear. Press

the CL key and the 1st monitor screen will return.

Summary of Contents for 200A Series

Page 1: ...SERIES 200A FLUORESCENCE DETECTOR User s Guide LIQUID CHROMATOGRAPHY ...

Page 2: ...and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or tran...

Page 3: ...Burns 23 Direct Viewing of Xenon Lamp Could Cause Eye Damage 23 Heavy Instrument 23 Prevention of Instrument Tipover 23 Precautions on Use of Solvents 24 Disposal of Waste Solution 25 Accuracy and Precision of Measured Values 25 Possible Carryover 25 Before Turning on Xenon Lamp Again 25 General Operating Conditions 27 Environmental Conditions 28 Electrical Safety 29 EMC Compliance 30 Europe 30 Un...

Page 4: ...Use 109 Before Performing Analysis 110 Characteristics of Organic Solvents 112 Cautions on Static Electricity 116 Maintenance 117 Operational Check 119 Performance Check 120 Energy Check of Xe Lamp 120 Check of Wavelength Accuracy by Using Hg Lamp 120 Check of Sensitivity 120 Check and Calibration of Wavelength Accuracy 130 Check of Leak Sensor 132 Periodic Checks 134 Maintenance Inspection Method...

Page 5: ...Introduction ...

Page 6: ......

Page 7: ... intended for use by persons having a basic knowledge of chemical analysis procedures Keep in mind that improper use of analytical instruments chemicals or samples would result not only in wrong analytical data but also in consequences adverse to safety Please read this instruction manual carefully before attempting operation and acquaint yourself with the Series 200a FL detector for its correct u...

Page 8: ... the time of replacement Note that this warranty does not apply to the instrument after it is discarded or if modified by the user or resold without permission from the manufacturer consumable parts and any failure of lifetime expired parts The manufacturer assumes no liability for any damage to data or application software due to any possible fault or failure of this instrument 2 Warranty Period ...

Page 9: ...ue to computer virus infection l After disposal of this instrument after its resale without prior approval from the manufacturer consumable parts and failure of any part that has reached the end of its service life 4 Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES EITHER EXPRESS OR IMPLIED EXCEPT AS PROVIDED HEREIN INCLUDING WITHOUT LIMITATION THEREOF WARRANTIES AS TO MARKETABILITY MER...

Page 10: ...or a descriptions of Fluorometry and instrument specifications Chapter 4 Installation Information on installing and re installing your instrument should you ever need to move your system is provided Chapter 5 Operation This chapter provides information on operating the instrument Chapter 6 Maintenance Maintenance and cleaning procedures for the various components of your instrument are provided Ch...

Page 11: ... keys on the PC keyboard is used to show that you have to press two keys at the same time for example ALT F All eight digit numbers are PerkinElmer part numbers unless stated otherwise Notes cautions and warnings Three terms in the following standard formats are also used to highlight special circumstances and warnings NOTE A note indicates additional significant information that is provided with ...

Page 12: ...En recuadros éste se proporciona información sobre este tipo de circunstancias F Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoquer de graves détériorations de l instrument ou d autre matériel Les détails sur ces circonstances figurent dans un encadré semblable à celui ci I Caution Attenzione Con il termine CAUTION ATTENZIONE vengono ...

Page 13: ...ecuadros como éste se proporciona información sobre este tipo de circunstancias F Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages corporels à l utilisateur ou à d autres personnes Les détails sur ces circonstances sont données dans un encadré semblable à celui ci I Warning Pericolo Con il termine WARNING PERICOLO vengono segnalat...

Page 14: ...14 Series 200a User s Guide Warning Signs on the Instrument WARNING FOR CONTINUED PROTECTION REPLACE ONLY WITH SAME FUSE TYPE AND RATING Power On Off push button Alternating current ...

Page 15: ...Safety Practices ...

Page 16: ......

Page 17: ......

Page 18: ...nformation provided does not cover every safety procedure that should be practiced Ultimately maintenance of a safe laboratory environment is the responsibility of the analyst and the analyst s organization Please consult all manuals supplied with the Series 200a and accessories before you start working with the instrument Carefully read the safety information in this chapter and in the other manu...

Page 19: ...nt be sure to provide proper ventilation of the room Inadequate ventilation could endanger human health Keep in mind that the hazard warnings in the manuals 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 In Use If an abnormality such as unusual noise odor fuming or gas leakage occ...

Page 20: ...ent shelf Ignition of Flammable Chemicals This instrument is not explosion proof In unattended operation do not use organic solvents having an ignition point below 70 C Beware 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 follow...

Page 21: ... power cable to a grounded three prong power outlet Injury Due to Xenon Lamp Explosion Replace the xenon lamp with a new one before its cumulative turn on time exceeds the guaranteed useful lifetime With the lapse of the guaranteed useful lifetime the bulb wall darkens due to evaporation of electrode material and adhesion of scattered substances resulting in a decrease in heat dissipation This may...

Page 22: ... 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 explosion To prevent this replace the lamp with a new one immediately if its cathode has been consumed substantially If the nut on the lamp base and wiring part is loose the contact res...

Page 23: ...proceeding to lamp replacement turn off the power switch unplug the power cord and then wait for at least one hour until the lamp and its housing cool down sufficiently See Chapter 6 Maintenance Direct Viewing of Xenon Lamp Could Cause Eye Damage WARNING The xenon lamp radiates intense ultraviolet light when it is on If you look at the illuminating xenon lamp during coarse adjustment of its positi...

Page 24: ...ow a Turn on the leak sensor function when feeding a solvent b The leak sensor function may remain inactive in cases 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 c In routine inspection of the...

Page 25: ...ensure that the performance of the instrument is normal Possible Carryover When examining the results of measurements take into account the possibility of carryover Since fluorocarbon resin and quartz materials are used for the wetted parts of piping particular attention should be paid when analyzing the samples that are likely to be adsorbed by these materials Before Turning on Xenon Lamp Again A...

Page 26: ...he detector to cease operation If the detector is not to be used for more than one week then prior to storage wash the flow line with pure water or acetone and store in isopropanol or 50 solution of isopropanol and HPLC grade water Do not use any eluent which might corrode the material such as stainless steel that it comes in contact with Use of such eluent might cause a baseline drift and damage ...

Page 27: ...nce and repair of the opened operating instrument If any adjustment maintenance and repair of the opened instrument are necessary this must be done by a skilled person who is aware of the hazard involved Whenever it is likely that the Series 200a is unsafe make it inoperative The Series 200a may be unsafe if it shows visible damage has been subjected to prolonged storage in unfavourable conditions...

Page 28: ...l to 6 562 feet Mains fluctuations not exceeding 10 of the nominal voltage Safe Operating Conditions Indoor use Ambient temperature of 5o C to 40o C 41 F to 104 F Relative humidity 25 to 80 without condensation Altitude 0 m to 2000 m Storage Conditions Ambient temperature 20 C to 60 C 4 F to 140 F Relative humidity 25 to 80 without condensation Altitude in the range 0 m to 12 000 m sea level to 39...

Page 29: ...e conductor earth ground inside or outside the instrument or disconnection of the protective conductor terminal is likely to make the instrument dangerous Intentional interruption is prohibited When working with the instrument Connect the instrument to a correctly installed line power outlet that has a protective conductor connection earth ground Do not operate the instrument with any covers or in...

Page 30: ...ty and these standards may change as the European Union adds new requirements United States This product is classified as a digital device used exclusively as industrial commercial or medical test equipment It is exempt from the technical standards specified in Part 15 of the FCC Rules and Regulations based on Section 15 103 c ...

Page 31: ...ing the customer s environment Requirements for waste collection reuse recycling and recovery programs vary by regulatory authority at your location Contact your local responsible body e g your laboratory manager or authorized representative for information regarding applicable disposal regulations Contact PerkinElmer at the web site listed below for information specific to PerkinElmer products We...

Page 32: ...ts 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 PerkinElmer WARNING Beware of electric shock Can cause death or serious injury Provide proper grounding connection Removal of this cover from the instrument is permitted only to qualified se...

Page 33: ...Safety Practices 33 Figure 2 2 Overview of the warning labels on the front of the instrument ...

Page 34: ...34 Series 200a Fi User s Guide Figure 2 3 Detail of the warning labels on the front of the instrument ...

Page 35: ...System Description 35 System Description ...

Page 36: ...36 Series 200a Fi User s Guide ...

Page 37: ...olumn at a constant temperature and a detector section for detecting a signal of a separated component of the sample In addition a degasser for de aerating an eluent a gradient device for varying the mixing ratio of eluent with time and other optional devices are incorporated in the system Series 200 Autosampler Series 200a Fluorescence Detector Series 200 LC Pump Solvent Systems Kit 3 x 3 Column ...

Page 38: ... and Indicators Fig 3 2 Front View Power switch Turns power ON OFF UI pad option A keypad required for unit operation LEDs Four LED indicators are provided for indicating the following states Table 1 1 Doors upper and lower right left Three doors are provided Power Switch UI Pad LEDs LCD ...

Page 39: ... green Green Time program is in execution Keyboard on the UI Pad Option Fig 3 3 Keyboard on the UI Pad Option All data entry is made via the keyboard on the UI pad see Figure 3 3 or the chromatograph data station The role of each key is indicated below For additional information about each key see the detailed discussions in the Installation chapter 1 2 4 5 7 STOP PROG GLP UTLTY 3 CL ENT 6 DEL 8 9...

Page 40: ...the end of analysis and accesses display mode See Chapter 5 Operation 3 2 If the UTLTY key is depressed when the power switch is turned on digital communication channel via the E Line and LCD contrast can be set SET UP See Chapter 5 Operation 4 GLP Used for setting the key lock for checking lamp energy and wavelength accuracy and for accessing Xe lamp and Hg lamp logbook See Chapter 5 Operation 5 ...

Page 41: ...ectrum over a specified wavelength range and stores the spectrum in memory See Chapter 5 Operation 12 Marker Places a marker on the recording See Chapter 5 Operation 13 Clear 1 Used to remove the present data input on the display before the ENT key is pressed e g to erase incorrect data 2 Also used to reset system when an error condition is indicated 14 Escape Lock off 1 Used to return from data i...

Page 42: ...eries 200a Fi User s Guide The Rear Panel Fig 3 4 Rear Panel Explanation of each function is given in Table 3 3 1 E Line 4 Marker In option 5 Recorder option 6 Processor option 2 Lamp Off In 3 Auto Zero In ...

Page 43: ...n is activated by means of contact signal input The marker function is started when the short circuit signal of more than one second is input 5 RECORDER option Analog output for recorder 1 The absorbance value at each point of time 2 Stored spectral data The absorbance value data is output 6 PROCESSOR option Analog output for data processor integrator 1 The absorbance value at each point of time 2...

Page 44: ...r Energy Level Diagram Radiationless transition Radiationless transition Absorption Excitation light Excited triplet state Excited state V Phosphorescence Fluorescence Ground state V 3 0 1 2 3 0 1 2 Light Light Excitation Stable condition Ground state Fluorescence or Phosphorescence Unstable condition Excited state ...

Page 45: ...d 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 absorb the same number of photons the fluorescence intensity of the compound with the larger fluorescence quantum yield will be grea...

Page 46: ...ompound exhibits a strong fluorescence signal it is likely that fluorescence can detect concentrations that are two orders of magnitude lower than absorbance A graphical description of why fluorescence can provide better sensitivity than absorbance is presented in Fig 3 6 In this figure the signal IS is used to represent the difference between the intensity of the incident beam Io and the intensit...

Page 47: ...n wavelength even if the absorption wavelengths of two components are the same a Absorptiometry b Fluorometry Fig 3 7 Spectroscopic Measurement of a Sample Containing Two Components Table 3 4 compares the analytical information obtained via absorptiometry and fluorometry Table 3 4 Comparison of Analytical Information Attainable with Absorptiometry and Fluorometry Absorptiometry Fluorometry Absorpt...

Page 48: ...may change The Raman Effect is moderately strong when water is the solvent but is considerably weaker for other solvents that are commonly used in HPLC Table 3 5 presents the position of the Raman peak for a variety of excitation wavelengths Fig 3 8 Raman Spectrum of Water Table 3 5 Raman Spectral Peak Position at Each Excitation Wavelength Excitation Wavelength Water Ethanol Cyclohexane Carbon Te...

Page 49: ... if the inner filter effect is reducing the fluorescence intensity it is suggested that the sample be diluted and the intensity measured again If the reduction in the fluorescence intensity matches the dilution the inner filter effect is not in effect Fig 3 9 Sample Having Extremely High Concentration Another potential error that may occur when fluorescence detection is used is the re absorption o...

Page 50: ...s indicated above In most cases the fluorescence of the compound of interest lies closer to the excitation than shown in Fig 3 10 and overlapping of peak of interest and the second order radiation is rarely a problem Typically the peak for the compound of interest might correspond to peak D and the analyst might have to correct for the Raman peak e g use a shorter excitation wavelength A Scatterin...

Page 51: ...n monochromator where it is dispersed by the monochromator The selected radiation strikes the measuring detector photomultiplier The monitor detector photodiode measures the intensity of the excitation beam as a function of time Photomultiplier high voltage circuit Xenon lamp starter Recorder or integrator Xenon lamp ballast Xenon lamp Sample fluorescence amplifier Electrical connection Monitor de...

Page 52: ...f a fused silica xenon lamp that produces intense radiation even in the short wavelength region As a safety measure against failure or stoppage of the cooling fan a thermal sensor works to extinguish the xenon lamp in about 15 minutes if the fan stops during analysis at a room temperature of 27 C or in about 20 minutes if the fan was stopped from the beginning in order to prevent failure or damage...

Page 53: ...interval of 30 nm or more is required 7 Wavelength setting By communication E line or keyboard 8 Wavelength accuracy 3 nm 9 Wavelength repeatability 0 5 nm 10 Recorder output option 10 mV full scale full scale range 1 to 1000 settable in increments of 1 11 Processor output option 1 V full scale 40 to 1000 mV 12 Response Changeable in 7 steps corresponding to time constants of 0 05 0 1 0 5 1 0 2 0 ...

Page 54: ...e 100 steps for a total of 9 files Programmable parameters Measurement wavelength Ex and Em Baseline processing PMT gain 20 External Output terminals option Analog output for processor 1 V full scale Analog output for recorder 10 mV full scale 21 External I O contact terminals Time Program Start Error Input Output Busy Output Auto Zero Input Lamp Off Input Marker Input 22 Flow cell capacity Standa...

Page 55: ...Installation 55 Installation ...

Page 56: ...56 Series 200a Fi User s Guide ...

Page 57: ...m on a sturdy and level desk or bench NOTE The customer must not attempt installation of the instrument at delivery To insure safe and correct use of the instrument its installation must be carried out your PerkinElmer service representative Before installation of this instrument the customer shall make preparations for satisfying the installation requirements in accordance with this manual If rel...

Page 58: ...on see Chapter 2 Installation WARNING Electric Shock due to Improper Grounding To prevent an electric shock hazard provide a proper grounding connection Be sure to use the grounded three prong power cord which is supplied with the instrument The use of a different type of power cord may result in an electric shock hazard Connect the three prong power cord to a grounded three prong power outlet Ins...

Page 59: ... of the laboratory room b Not exposed to drafts directly c Free from intense vibrations and shocks d Apart from a heat source such as a gas burner electric heater or oven e Apart from a strong magnetism source such as an electric welder high frequency electric furnace or pole transformer f Free from dust and dirt Contamination with dust and dirt could deteriorate the performance of the instrument ...

Page 60: ... 6 Maintenance 3 Use a Phillips screwdriver to remove the transport screw D E and Transport TY RAP F Fig 4 2 from the lamp house 4 Mount the xenon lamp and place it into the unit See Chapter 6 Maintenance 5 Adjust the position of the xenon lamp Please adjust VERTICAL first because the lamp position is shifted downward for fixation of the transport screw See Chapter 6 Maintenance Transport screw B ...

Page 61: ... Removal Xe Lamp Attachment Tubing Arrangements In the Series 200a provide inlet tubing to the pump and waste solution tubing through the right piping section of the drain reservoir Provide tubing from the pump to the autosampler column and detector through the center piping section of the drain reservoir Fig 4 3 Connecting Tubes ...

Page 62: ...monitor window DEL delete Deletes a cursor pointed step This key is effective only in program editing When the cursor is positioned on the TIME input part pressing the DEL key removes a step pointed by the cursor When the cursor is positioned on another input part pressing the DEL key removes an item pointed by the cursor Pressing the ESC key on a window where is indicated returns control to the m...

Page 63: ...llowing the last line of the current program Autosampler A new step is inserted U V arrows 1 Monitor window V key Goes to the next window U key Goes back to the previous window 2 Program editing V key The next line is presented Pressing this key at the last line causes the first line to appear in a circular fashion U key The previous line is presented Pressing this key at the first line causes the...

Page 64: ...ii To define an input numeric value press the ENT key The cursor will then move to the next item If an erroneous numeric value is input the cursor is brought back to the top of the input part with the input numeric value displayed In this state you are prompted to enter a correct numeric value Pressing the ESC key brings you back to the initial window monitor window If the ESC key is pressed durin...

Page 65: ...p are the only replacement parts and consumables for this instrument It is suggested that you stock a few fuses and lamps in the laboratory to minimize down time Replacement Parts Part No Description 0999 1667 Fuse 5 Amp 250 V Slo Blow N292 2082 Xenon lamp 150 W ...

Page 66: ...66 Series 200a Fi User s Guide ...

Page 67: ...Operation 67 Operation ...

Page 68: ...68 Series 200a Fi User s Guide ...

Page 69: ...oubleshooting 1 Turn ON the power switch of the detector 2 Liquid Crystal Display LCD presents the initial screen which changes to the initializing screen after a few seconds At the same time a test for self diagnosis initialization is carried out The current channel setting LED and the Xe LAMP LED will light in green Initial screen Series 200a FL Detector Initializing screen WL DRIVE LAMP INITIAL...

Page 70: ...d program number is the currently selected one However when the time program is not used is indicated c In lamp indication Xe stands for the lit status of the xenon lamp and OFF stands for the extinguished status d Fluorescence intensity FL is indicated within a range from 1000 0 to 1000 0 If the intensity is outside this range is indicated e Status indicators should be read as follows I Initial s...

Page 71: ...ESC escape key for return to the 1st monitor screen then re edit the value 3 Canceling the setup conditions press ESC key for return to the 1st monitor screen followed by re setup 4 Accessing the next window without change or entering values press ENT key or V key Accessing the previous or next window press U key or V key 5 If the time program is not in use spectral output can be performed at any ...

Page 72: ...y held down 2 The following display will be presented Setup initial screen SETUP DETECTOR CONTRAST Serial No CH1 4 Press the ENT key 3 The following display will be presented Setup items selecting screen SETUP ITEMS DETECTOR 1 CONTRAST 2 1 EXCHANGE STANDARD 3 Select DETECTOR Press numeric key 1 and then ENT key 4 The following display will be presented Channel selecting screen DETECTOR CH1 1 CH2 2...

Page 73: ...t a contrast brightness level of the LCD screen 1 Turn on the power switch with the SET UP UTLTY key held down 2 The following display will be presented Setup initial screen SETUP DETECTOR CONTRAST Serial No CH1 4 Press the ENT key 3 The following display will be presented Setup items selecting screen SETUP ITEMS DETECTOR 1 CONTRAST 2 2 EXCHANGE STANDARD 3 Select CONTRAST Press numeric key 2 and t...

Page 74: ... of the Xe lamp is longer than the standard lifetime upon turning on the lamp an error message is indicated to notify that the time point of lamp replacement is reached 1 Turn on the power switch with the SET UP UTLTY key held down 2 The following display will be presented Setup initial screen SETUP DETECTOR CONTRAST Serial No CH1 4 Press the ENT key 3 The following display will be presented Setup...

Page 75: ... input the correct value listed below Part No Part Name Guaranteed Life Limit Allowable Input N292 2082 150 W Xe lamp 150 hours 500 hours 500 or less Default value 500 This detector unit has been shipped with N292 2082 lamp attached 5 The setting of a standard Xe lamp lifetime is now completed and the following display will be presented Setup initial screen SETUP DETECTOR CONTRAST Serial No CH1 3 ...

Page 76: ... 1st monitor screen is reset to zero and output signal becomes zero The 1st monitor screen TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 Xe Setting value range 0 to 1000 If the range is exceeded an error message is displayed Setting the Wavelength Setting items Ex Excitation wavelength Em Emission wavelength 1 Press the WL key 2 The following display will be presented Excitation wavelength Ex is set...

Page 77: ...or screen returns Pressing the U key enables you to return to the excitation wavelength setting without changing the emission wavelength 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 Setting the Utility The following conditions can be set by the UTILITY key OFFSET ...

Page 78: ...imit for an integrator or data processor is approximately 10 mV If the baseline decreases below this level it becomes impossible to integrate the peaks in the chromatogram see Fig 5 2 a In such a case the offset function is used to adjust the shifted baseline to the allowable input signal range of the data processor see the following figure b Fig 5 2 Example of Offsetting d Offset setting is now c...

Page 79: ...key 1 to 7 usually input 3 and then ENT key Default value 4 d Constant setting is now completed and the 1st monitor screen returns 3 Setting the USE PROG selection or avoidance of time program It is selectable whether or not to use automatic change of measurement parameters in response to measurement time time program a Press the UTLTY key b The following display will be presented Utility initial ...

Page 80: ...ey b 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 ENT key c The following display will be presented PMT voltage setting screen PMT VOLT SUPER HIGH 1 HIGH 2 MID 3 3 LOW 4 SUPER LOW 5 Set a photomultiplier voltage Press numeric key 1 to 5 usually input 3 and then ENT key ...

Page 81: ... be presented Em bandwidth selecting screen Em BANDWIDTH STANDARD 1 WIDE 2 1 Set an Em bandwidth value Press numeric key 1 or 2 usually input 1 and then ENT key Default value 1 v Em bandwidth setting is now completed and the 1st monitor screen returns b Setting the ERROR OUT It is selectable whether to enable or disable the error signal output When enabled the following errors can be indicated Xen...

Page 82: ... key 0 or 1 and then ENT key Default value 1 v Error out setting is now completed and the 1st monitor screen returns c Setting the LEAK SENSOR Whether to use the liquid leak sensor or not is settable i Press the UTLTY key ii 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 EN...

Page 83: ...ented 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 ENT key iii The following display will be presented Others setting screen OTHERS Em BANDWIDTH 1 ERROR OUT 2 4 LEAK SENSOR 3 LAMP 4 Select LAMP Press numeric key 4 and then ENT key iv The following display will be presented Xe lamp selecting screen Xe LAMP ON OF...

Page 84: ...amp CHECK Xe lamp energy check NOTE The logbook data entry is reset when a numeric value representing year is input followed by pressing the ENT key Even when the same year as desired is already indicated it must be reentered without fail 1 Display of Xe lamp LOGBOOK data Total ON period of the Xe lamp and its standard lifetime in parentheses under Xe LAMP the number of switching on times and the ...

Page 85: ...book display is now completed and the 1st monitor screen returns 2 Resetting of Xe lamp LOGBOOK data Total ON period of the Xe lamp the number of switching on times and the date of the last lamp change can be set again a Press the GLP key b The following display will be presented GLP initial screen GLP LOGBOOK 1 KEY LOCK 2 1 WL CHECK 3 Xe CHECK 4 Select LOGBOOK Press numeric key 1 and then ENT key...

Page 86: ...ursor moves to YYYY iii Input a year for YYYY Xe lamp change date setting screen year Xe LAMP CHANGE MM DD YYYY 2000 2100 7 25 2005 Press numeric keys 2 0 0 0 to 2 1 0 0 and then ENT key Even when the same year as desired is indicated it must be reentered again f Logbook setting is now completed and the 1st monitor screen returns When a xenon lamp change date is set the total ON period of the Xe l...

Page 87: ...he number of switching on times and the date of the last lamp change will be indicated Logbook report screen Hg LAMP SWITCHING LAST CHANGED DATE 12h 56 times 7 25 2005 Press the ENT or ESC key f Logbook display is now completed and the 1st monitor screen returns 4 Resetting of Hg lamp LOGBOOK data Total ON period of the Hg lamp the number of switching on times and the date of the last lamp change ...

Page 88: ...mp change in the following procedure i Input a month for MM cursor appears under MM Hg lamp change date setting screen month Hg LAMP CHANGE MM DD YYYY 1 12 _7 25 2005 Press numeric key 1 to 12 and then ENT key The cursor moves to DD ii Input a day for DD Hg lamp change date setting screen day Xe LAMP CHANGE MM DD YYYY 1 31 7 25 2005 Press numeric key 1 to 31 and then ENT key The cursor moves to YY...

Page 89: ...screen KEY LOCK YES 1 NO 0 1 Set selection 1 or disable 0 of KEY LOCK Press numeric key 1 or 0 usually input 1 and then ENT key Default value 0 Even with the keys locked the monitor screen can be changed with U and V keys Key lock can be released by pressing LOCK OFF ESC key It is also released when power is turned on again or when an error occurs d Key lock setting is now completed and the 1st mo...

Page 90: ...ENT If the error is within 3 nm GOOD will appear and if the error exceeds 3 nm FAIL will appear on the display If ESC key is pressed prior to ENT key or if this status continues for 5 minutes or longer the system will return automatically to the 1st monitor screen e The result of emission wavelength Em check will now be displayed Em side check result Em SIDE ACCURACY 254 nm GOOD 1nm Press ENT or E...

Page 91: ...yed automatically Xe lamp energy check result Xe ENERGY 1200 Press the ENT or ESC key If 5 minutes or more elapses without pressing ENT or ESC key the system will return automatically to the 1st monitor screen e 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 ...

Page 92: ...surement and Recording of Spectrum for Excitation Ex 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 1 Press numeric key 1 and then ENT to select FL Ex Now proceed to the scan range setting screen for setting a scan range and enter a start wavelength cursor will appear at WL1 c Enter a start wavelength minimum value...

Page 93: ...e lamp goes off press the ENT key and the 1st monitor screen will return f The scan monitor screen appears and spectral acquisition within the set range is carried out Scan monitor screen spectral acquisition under way SCANNING SPECTRUM NO 1 MODE FL Ex Ex nm Em 350 nm Pressing ESC key during spectral acquisition will cancel the process Spectral data will not be memorized The memorize spectrum No s...

Page 94: ...ial default value 250 If setting will not be changed press V key to proceed to WL2 setting The cursor now moves to WL2 d Now enter an end wavelength maximum value at WL2 Scan range setting screen indicate WL2 SCANNING WL RANG WL1 WL2 nm FL Em 300 900 250 700 Press numeric keys 3 0 0 to 9 0 0 and then ENT Input value Value of less than 900 within WL1 50 to WL1 400 Setting range 300 to 900 nm Initia...

Page 95: ...ecorder Output speed of recorder Output spectrum data NOTE With an emission spectrum scattered excitation light Raman scattering due to solvent emission 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...

Page 96: ... 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 RANGE 1 RCD SPEED 2 2 SPECT RCD 3 Press numeric key 2 and then ENT to select RCD SPEED recorder speed c The recorder speed setting screen appears Recorder speed setting screen RCD SPEED 40 nm min 1 60 nm min 2 Press numeric...

Page 97: ...lvent or cell To ensure that an appropriately corrected spectrum is used in analysis a new background spectrum should be acquired whenever the solvent or wavelength scan range is changed Background spectrum No setting screen BACKGROUND SPECTRUM NO 0 4 0 Press a numeric key 0 to 4 and then ENT to select whether or not to correct the output spectrum 0 Spectrum selected at RECORD SPECTRUM NO will be ...

Page 98: ...ill cancel the process The output spectrum No set before will be indicated at RCD NO g When the spectrum output is finished the 1st monitor screen will return automatically Operation of Marker 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 MA...

Page 99: ...or the final step NOTE Set an interval of at least 0 3 minute between steps of the time program NOTE It is recommended that the wavelength set here for 0 0 minute be identical to the measurement wavelength set in section 4 4 2 For instance if 500 is set here for Ex with 250 set for Ex of the measurement wavelength then a time loss will occur when Ex shifts from 250 to 500 at the start of the time ...

Page 100: ...en TIME indicated TIME Ex Em BASE PMT _ 0 0 1 Press numeric keys 0 0 and then ENT key Be sure to enter 0 0 for TIME Initial default value 0 0 The program No currently set is indicated at the bottom right of the screen The cursor now moves to Ex II 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 ENT key Settin...

Page 101: ...HOLD is executed Baseline is held so that it doesn t fluctuate HOLD function is released by executing AUTO ZERO Initial default value 1 V 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 ENT key VI When the setting for the first step is completed return to the TIME setting on step setting screen If some ...

Page 102: ... 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 ENT key The cursor next moves to BASE iv Set the BASE baseline processing to be changed Step setting screen BASE indicated TIME Ex Em BASE PMT 10 0 400 500 2 1 Press a numeric key 1 or 2 usually 2 and then ENT key Enter 2 so as to match the baseline in the present step with th...

Page 103: ...are completed return to the 1st monitor screen g Addition of steps Press the INSERT key to add a step to the program during step input The step setting screen will appear so make the addition in the same procedure as described above However the addition must be made within the time entered at the final step 2 Start of Time Program Press the START key to start the time program Status indication on ...

Page 104: ...ram at program No 1 Ten minutes after the start 1 photomultiplier voltage is changed from MID 3 to LOW 4 excitation wavelength from 250 to 400 nm emission wavelength from 350 to 500 nm and hold baseline function is applied and then measurement is completed after 20 minutes 2 250 350 400 500 ON ON 3 4 0 0 10 0 20 0 START STOP Ex nm Em nm Base line Auto zero HOLD TIME minutes ...

Page 105: ...IT MODE MODIFY 0 NEW 1 0 Press 1 key and then ENT TIME Ex Em BASE PMT 0 0 250 350 1 2 1 Press 0 key and then ENT Press 2 5 0 keys and then ENT Press 3 5 0 keys and then ENT Press 1 key and then ENT Press 3 key and then ENT TIME Ex Em BASE PMT 0 0 250 350 1 3 1 Press 1 0 keys and then ENT Press 2 7 0 keys and then ENT Press 3 7 0 keys and then ENT Press 2 key and then ENT ...

Page 106: ... finished TIME Ex Em FL PROG LAMP I 0 0 250 350 0 0 1 Xe Press the START key The time program starts and measurement is initiated b Check of time program Take the following procedure for checking the program that was set in the above Press PROG key SET PROGE NO 1 9 1 Press 1 key and then ENT EDIT MODE MODIFY 0 NEW 1 0 Press 0 key and then ENT Step at startup is indicated TIME Ex Em BASE PMT 0 0 25...

Page 107: ... to access the next step TIME Ex Em BASE PMT 10 0 270 370 1 3 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 ...

Page 108: ...ector s power switch 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 conditions that were in place when power was turned off will be restored ...

Page 109: ...hing the Flow Cell After Use Make sure to flush the flow cell with distilled water after using any buffers or salts in the mobile phase Failure to carry out flushing may lead to clogging and or breakage of the flow cell ...

Page 110: ... is found stop operation immediately o Leakage of solvent or waste solution o Leakage of solvent inside the instrument 3 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 Chemica...

Page 111: ...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 depending on the manufacturing lot and the manufacturer Be careful especially when performing high sensitivity analysis 3 Degas the mobile phase before use It is recommended to use a degasse...

Page 112: ... 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 Do not use reagents that corrode SUS316 though they are not shown...

Page 113: ...nection 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 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 an...

Page 114: ... 6 7 11 3 3 8 37 8 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...

Page 115: ...ile 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 us...

Page 116: ...icity use a 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 tubes 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 di...

Page 117: ...Maintenance 117 Maintenance ...

Page 118: ...118 Series 200a Fl User s Guide ...

Page 119: ... for operation see chapter Operation 2 Turn ON the power switch of the detector 3 Check that measurement conditions time constant output range etc can be properly set 4 Check if wavelength operation is accomplished normally by pressing the WL key 5 Check the auto zero operation by pressing the A Z key ...

Page 120: ...by using the bright line at 254 nm of the Hg lamp see chapter 5 Operation GOOD will appear on the display when the wavelength error is within 3 nm or FAIL will appear when the error exceeds 3 nm NOTE Wavelength calibration is necessary when FAIL appears See the procedure for the calibration later in this chapter Check of Sensitivity The S N ratio of the Raman spectrum of water is used to measure t...

Page 121: ...chapter 5 Operation Measure in the following sequence Excitation Ex wavelength 350 nm Time constant response 2 seconds Photomultiplier voltage MID 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 wavelength i Press the WL key and the wavelength setting screen appears Set an excitation Ex...

Page 122: ...etting screen appears Press numeric key 5 to select 2 0 s and then ENT iii The 1st monitor screen appears iv Press UTLTY key and the utility setting screen reappears Press numeric key 4 and then ENT to select photomultiplier voltage v The pmt voltage setting screen appears Press numeric key 3 and then ENT to select MID vi The 1st monitor screen reappears vii Press UTLTY key and the utility setting...

Page 123: ...ndwidth 1 STANDARD emission spectrum bandwidth 15 nm 2 WIDE emission spectrum bandwidth 30 nm x The 1st monitor screen returns d Setting of spectrum measurement i Press the SPECT key The scan mode setting screen appears Press numeric key 2 and then ENT to select FL Em ii Set a scanning range 1 Enter a starting wavelength minimum value for WL1 Press 3 5 0 and ENT to set WL1 2 Enter an end wavelengt...

Page 124: ...r screen returns automatically e Setting of recorder full scale range speed and memory No i Press the RECORD key and the recorder setting screen appears Press numeric key 1 and then ENT to select RCD RANGE ii The recorder full scale setting screen appears Recorder full scale setting screen Press numeric keys 1 0 0 0 and then ENT to set the RCD RANGE iii The 1st monitor screen returns iv Press the ...

Page 125: ...ENT to select SPECT RCD viii The output data spectrum No setting screen now appears Press a numeric key 1 to 4 and then ENT to select a RECORD SPECTRUM NO Set the same number as was entered when making the setting for spectrum measurement ix The background spectrum No setting screen appears Press numeric key 0 and then ENT to set BACKGROUND SPECTRUM NO x The output ready monitor screen now appears...

Page 126: ...of Raman Signal Intensity FIG 6 2 Measuring the Raman Signal Intensity Determine the voltage value corresponding to S in the figure When using the recorder calculation can be made using the length L in mm of S on the chart L Length of S mm X ATT setting of data processor used in measurement 4 Measurement of Noise With the excitation wavelength left at 350 nm set the emission wavelength at 397 nm o...

Page 127: ...late the noise level on the chart by the method given in Fig 6 3 The noise level in the case of using the recorder is obtained from the noise width in mm as follows X ATT setting of data processor used in measurement 6 S N Ratio Calculation for Raman Spectrum of Water Perform calculation according to the S and N obtained in the preceding subsections 3 and 5 a Excitation spectrum bandwidth 15 nm b ...

Page 128: ...tance may mix in with the distilled water ii Check for bubbles If water is directly injected into an empty flow cell small bubbles may remain in the cell 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 shi...

Page 129: ...um obtained with the time program Fig 6 4 Calculate the Raman Peak of Water When using the recorder calculation can be made using the length L in mm of S on the chart L length of S mm 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 th...

Page 130: ...the bright line at 254 nm of the built in 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 b Check of wavelength accuracy Check the wavelength accuracy by using the bright line at 254 n...

Page 131: ...s numeric keys 9 9 and then ENT ii The excitation wavelength calibration mode screen appears The present offset value is indicated at Ex WL ADJUST Indicated at the bottom right of the screen is the wavelength check result deviation of wavelength indication range of 10 to 10 Wavelength calibration is conducted by entering a new offset value value to which the deviation is added Press numeric keys f...

Page 132: ...h calibration is conducted by entering a new offset value value to which the deviation is added Press numeric keys from 1 to 20 and then ENT Input range for offset value 1 to 20 Calculation of new offset value New offset value present offset value wavelength deviation Example 12 10 2 iii The 1st monitor screen now appears Check of Leak Sensor 1 Operational Check of Leak Sensor a Drip water onto th...

Page 133: ... function is activated you should be careful not to overlook liquid leakage for avoiding a serious situation 3 As a routine checkup visually check for any liquid leak before measurement 4 As a periodic checkup make sure the leak sensor works normally 2 Cleaning of Leak Sensor When separating the drain receiver from the instrument for cleaning of the leak sensor etc keep the leading end of sensor i...

Page 134: ...tensity check Daily Press A Z key and check if FL indication is zeroed Lifetime of lamp Monthly 1 Check lamp for service life by energy check or by cumulative lamp turn on time 2 Check if baseline drifts considerably or if baseline fluctuates or noise becomes high Leak sensor Monthly 1 drip water onto the leak sensor and confirm the occurrence of an error 2 After confirmation wipe off the water Wa...

Page 135: ...e useful life of the lamp is considered to have ended The lamp life can be judged by the energy level or by baseline fluctuation fluctuation of data and or noise Wavelength Accuracy Check Using Hg Lamp Check the wavelength accuracy by means of the bright line of the Hg lamp at 254 nm see chapter 4 Operation GOOD will be indicated on the display when wavelength error is within 3 nm FAIL will be ind...

Page 136: ...ng flammable chemicals be careful about possible ignition due to static electricity Particularly when using non conductive chemicals employ a conductive vessel made of metal or the like and provide grounding connection correctly 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 ...

Page 137: ...he cell it must be cleaned with an appropriate solution If an aqueous solvent has been used distilled water should be used for washing And if an organic solvent has been used then isopropyl alcohol should be used for washing Connect the syringe to the tip of the drain tube and inject the washing solution into the cell for cleaning see the next figure NOTE This flow cell unit uses apart similar to ...

Page 138: ...the end of the drain tube with your fingers for a few seconds to increase the pressure inside the cell then release your fingers quickly Repeat this procedure a few more times until all the air bubbles have been removed Fig 6 8 Removing Air Bubbles NOTE Applying too much pressure may damage the flow cell Set the pressure limiter of the pump at 1 0 MPa max before removing air bubbles Disassembly an...

Page 139: ... Flow Cell a Wash the flow cell in running water If the contamination cannot be removed with running water then use an ultrasonic cleaner 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 ...

Page 140: ... to disassembly flow a liquid through the unit and make sure there 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 6 11 A mistake in the orientation may preclude obtaining the proper performance from the instrument NOTE Tighten the setscr...

Page 141: ...e there is no more leakage NOTE It is important that the OUTLET tube of the flow cell be checked first for clogging If the upper nipple is found to be loose and is retightened with the wrench without checking the OUTLET tube then the flow cell may be damaged or broken NOTE If leakage is found in the sample compartment or on the optical base inside it wipe up the liquid thoroughly and then clean wi...

Page 142: ...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 repl...

Page 143: ...ltage of 30 kV which could cause an electric shock to result in serious or fatal injury Before removing the light source cover for replacement of the light source lamp be sure to turn off the power switch WARNING Injury 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...

Page 144: ...or between lamp house and main body and loosen the lamp house retaining screw Fig 6 14 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 Retaining screws Connector Flow cell unit Retaining screw for flow cell Grip Retaining screw Lamp house ...

Page 145: ...is high pressure gas still remains in the xenon lamp after it is demounted for replacement For disposal of the 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 impa...

Page 146: ...ng the retaining nut for the xenon lamp be careful not to apply excessive force to its glass bulb part Never hold and turn the glass bulb part for loosening tightening g Loosen the cathode nut and remove the cathode lead plate see the following figure Fig 6 17 Detachment of Xenon Lamp h Mounting of new xenon lamp ...

Page 147: ...ly 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 WARNING Injury due to Xenon Lamp Explosion at mounting 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 ...

Page 148: ...148 Series 200a Fl User s Guide Fig 6 18 The Xenon Lamp Fig 6 19 Orientation of Lamp Bulb Protrusion ...

Page 149: ...rce cover and turn ON the power check that the lamp comes on Now proceed to positional adjustment of the Xe lamp 3 Positional Adjustment of Xe Lamp WARNING Direct Gazing at Illuminating Xenon Lamp Could Cause Eye Damage The xenon lamp radiates intense ultraviolet light when it is on If you look at the illuminating xenon lamp during coarse adjustment of its position your eyes could be damaged Do no...

Page 150: ...apter 5 Operation i Turn ON the power switch and the 1st monitor screen appears ii In the present status pull out the flow cell unit see Fig 6 14 will be indicated at FL on the 1st monitor screen iii Press the WL key and the wavelength setting screen appears Set an excitation Ex wavelength Press numeric keys 5 5 0 and then ENT to set the Ex iv Emission Em wavelength will not be set here Leave the ...

Page 151: ...xcitation beam rainbow color becomes brightest The coarse adjustment of the light source position is thus completed Please adjust VERTICAL first in installation because the lamp position is shifted downward for fixation of the transport screw Fig 6 21 Observation of Ex Beam b Fine adjustment Following the coarse adjustment set the excitation Ex wavelength at 350 nm make a fine adjustment while obs...

Page 152: ...onitor screen appears vi In the present status turn the FOCUS HORIZONTAL and VERTICAL adjusting screws gradually in a repetitive manner while watching the MONITOR Ex value on the screen until this value is maximum When a maximum value is reached the fine adjustment of the lamp position is completed vii Press or ESC key and the 1st monitor screen will return 4 Entry of Lamp Replacement Date When th...

Page 153: ...unplug the power cord before proceeding to fuse replacement 1 Item to prepare 2 new fuses 2 Items to Check Prior to fuse replacement make sure the power switch of the instrument is OFF and the power cord is unplugged 3 Replacement of Fuse a Hold the tabs on both sides of the fuse holder and detach the holder Fig 6 22 Fuse Replacement b Replace the blown fuse s with new one s then reinsert the fuse...

Page 154: ...154 Series 200a Fl User s Guide ...

Page 155: ...Troubleshooting ...

Page 156: ...156 ...

Page 157: ... and unplug the power cable Then wait at least two hours for the lamp to cool down Upon detaching the light source cover the xenon lamp is automatically turned off by a safety mechanism Avoid releasing this safety mechanism WARNING Directly Gazing at Illuminated Xenon Lamp Could Cause Eye Damage The xenon lamp radiates intense ultraviolet light when it is on Do not look at the xenon lamp directly ...

Page 158: ...work The display does not present the 1st monitor screen FL indication Check the monitor screen Return to the 1st monitor screen FL indication Refer to Section 4 1 The time program does not start The instrument is not ready to operate Check the monitor screen Press the ESC key The READY status will be presented Excessive noise The flow cell is contaminated Visual check Clean the flow cell Refer to...

Page 159: ...ing from the column Stop feeding liquid from the pump Wait until elution is completed or replace the column with a new one There is a significant change in the ambient temperature ____________ Control the temperature variation The mobile phase is not sufficiently pure Check the mobile phase solvent Purify the mobile phase or replace it with one of a higher quality Poor S N ratio Flow cell contamin...

Page 160: ...is test initialization 1 Cannot be released by key operation 2 Turn on power again 3 Contact our nearest service center Ex Em SIDE ACCURACY 254 nm NOT DETECTED Wavelength error exceeds 10 nm during wavelength accuracy check Contact our nearest service center LAMP OFF BY OVERHEAT PRESS CL KEY TO CLEAR MESSAGE Abnormal temperature detected 1 Press CL key and 1st monitor screen returns 2 Contact our ...

Page 161: ...A ARE MISMATCHED PRESS CL KEY TO CLEAR MESSAGE Scan mode incorrect Em band pass incorrect fixed wavelength incorrect background WL range doesn t include entire spectrum WL range background spectrum mode incorrect or energy spectrum incorrect 1 Press CL key and 1st monitor screen returns 2 Select correct parameters DATA BUFFER OVERFLOW PRESS CL KEY TO CLEAR MESSAGE During data acquisition data tran...

Page 162: ...162 Series 200a Fl User s Guide ...

Page 163: ...Appendix 163 Appendix ...

Page 164: ...164 Series 200a Fl User s Guide ...

Page 165: ...that are used in common for each unit These signals are respectively formed from the START IN OUT ERROR IN OUT and BUSY IN OUT lines 2 Individual Contact Signals Used by Each Unit These 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 e g output contact signal EVENT of pump e...

Page 166: ...is turned off Diffusion plate This quartz plate is used for diffusion of excitation beam Drain port Equipped for allowing solution leaked from the flow cell joint to flow to an external waste bottle E Line Digital network line dedicated for analytical system Emission Fluorescence intensity Unit of measure of fluorescence relative intensity Emission Fluorescence wavelength A particular wavelength o...

Page 167: ... for holding the light source lamp This part becomes extremely hot when the lamp is lit Be careful not to incur burns by touching it Lamp off in The external contact signal can be input for turning off the light source lamp Lamp turn on count Indicates the number of times the light source lamp has been turned on Lamp turn on cumulative time Indicates a cumulative total time of lamp turn on periods...

Page 168: ...ht 3rd order light etc In fluorescence analysis particular attention should be paid to scattered light 2nd order light A spectral peak a kind of scattered light which appears at a wavelength of 2 times the level of excitation intensity In a common arrangement a filter is used to remove or cut off the 2nd order scattered light Stokes law This law states that the wavelength of a fluorescent emission...

Page 169: ...Appendix 169 Utility Used to set up operating conditions of the instrument Xenon lamp The xenon lamp is used for fluorescence measurement ...

Page 170: ...170 Series 200a Fl User s Guide ...

Page 171: ...Chemicals explosion 19 safety warnings 19 Flow Cell check 136 cleaning 138 disassembly 138 flushing 109 leakage 140 storage 141 washing 136 Fluorometry advantages 45 descriptions 44 Fuse replacment 153 G General Operating Conditions 26 Glossary 166 GLP Function setting 84 H HG Lamp wavelength accuracy 135 Hg Lamp Wavelength Check maintenance 120 I Installation conditions 58 space 58 L Labels warni...

Page 172: ...mation 18 electrical safety 28 environmental conditions 27 Sensitvity Check maintenance 120 Shutdown 108 Solvents precautions 23 safety warnings 22 Spare Parts 65 Spectrum Measurement 91 Spectrum Output Factors 95 Static Electricity cautions 116 Storage flow cell 141 T Terminology 166 Time Program setting 98 Troubleshooting Messages 158 Tubing Arrangements 61 U UI Pad 62 Unpacking 57 Utility Setti...

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PerkinElmer 200A Series, User Manual

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