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Shimadzu RID-10A, User Manual

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Shimadzu RID-10A User Manual Download Page 1

228-30179 

DIFFERENTIAL  REFRACTIVE  DETECTOR 

RID-1 OA 

FOR 

SHIMADZU 

HIGH-PERFORMANCE 

LIQUID  CHROMATOGRAPH 

USER’S  MANUAL 

Read  the  instruction manual  thoroughly  before  you  use  the  product.  Keep 

this 

instruction 

manual 

with care 

so 

that you can use it any time you need it. 

CORPORATION 

CHROMATOGRAPHIC 

INSTRUMENTS  DIVISION 

KYOTO, 

Summary of Contents for RID-10A

Page 1: ...CE LIQUID CHROMATOGRAPH USER S MANUAL Read the instruction manual thoroughly before you use the product Keep this instruction manualwith care so that you can use it any time you need it SHIMADZU CORPO...

Page 2: ...red in this publication despite the utmost care taken in its production will be corrected as soon as possible but not necessarily immediately upon detection Note that Shimadzu does not have any obliga...

Page 3: ...may lead to a dangerous situation or damage of the unit 5 For internal repair of the product contact your Shimadzu ServiceRepresentative 6 The pink color pages and the meshed parts are for our servic...

Page 4: ...ions are required the m a n u a l Replacementof fuses Thisunit uses the following fuse Be sure to replace the fuse of sametypeand capacity Rated voltage 100 24OV Part NO 072 01652 23 250V 5AT I CAUTIO...

Page 5: ...m VAOSI AOX 022 VAOSI A02I 96 000ZE 822 26 0002 822 VAOSI hpedea A001 16 000Zf 822 a3NlOS JaMOd ON lred...

Page 6: ...e the strength of the material In the worst case pipe may explode and high pressure solvent scatters As it is very dangerous never use HFIPA 9 Others The equipment should not be exposed to direct sunl...

Page 7: ...ke place through the following processes When liquid is fed at high speed through a small diameter tube like the pipe of a liquid chromatograph static electrical charge occurs by friction between soli...

Page 8: ...uantity of flammable solvent is held in a large vessel be sure to observe the preventivemeasures 1 2 and 3 Preventive measure 1 Use metallic conductive waste liquid vessel which is well grounded This...

Page 9: ...ith charged objects including the human body Charging prevention measures for human body a b Groundingof human body c Make working floorconductive Prevention of charging of shoes and clothes Suitable...

Page 10: ...id level in the vessel Or dip a grounded metal ex pipe connected to the main body of device in the liquid This method is not effectivefor liquid with small conductivity 10 I0s mor less Use a vessel of...

Page 11: ...4 7 4 5 Plumbing Connections 4 6 Connecting the Drain Tubefor SolventLeakage 4 13 1 1 Operation 5 1 Precautions for Operation 5 2 5 2 Fundamentals of Operation 5 3 5 3 Plumbing of the Flow Selection B...

Page 12: ...9 2 System Validation 9 9 9 2 1 Test Procedureof Isocratic LC System 9 9 1 1 Troubleshooting 10 1 10 2 Symptoms Causes and Remedies 10 2 List of Error Messages 10 4 1 Specifications 11 1 RID 1O A Spe...

Page 13: ...Chapter 1 General 1 1 Outline 1 2 1 2 Features 1 3 1 3 Principle of Measurement 1 4 1 4 Flow Schematic 1 6 1 1 RID 1OA...

Page 14: ...Its shortened stabilization time the fact that it covers various applications from high sensitivity analysis to sampling analysis preparation and more RID 1OA is much improved in convenience than conv...

Page 15: ...amic range of various applications from high sensitiveanalysisto large scalepreparation of high concentration samples 2 Various applications 3 Safety measure 4 Corresponding to the LC 1OA series The s...

Page 16: ...ur as shown in the figure below When selecting a piece of photodiode to use among these four the unit is able to provide measurements for both analytical and preparativework I n modes P and L In mode...

Page 17: ...hat of mode A In mode A when the slit image goes beyond the center line measurement becomes impossiblebecause the balance value stops varying while in mode P measurement is possible under these condit...

Page 18: ...he solenoid valve is open at side B The solvent passing through the sample cell flows into the outlet port after passing through the reference cell This is used to fill the sample cell and the referen...

Page 19: ...Chapter 2 Parts List c v 3 2 1 Parts and Accessories 2 2 1CONTENTS 1 2 1 RID 1OA...

Page 20: ...npacking confirm that all parts listed below are included in your shipment 0 RID IOA Main Body Power supply cord 120V 220 240V Opticalcable 0 StandardAccessories 071 60814 01 1 071 60814 06 070 92025...

Page 21: ...Chapter 3 Component Location and Function 3 1 Front View 3 2 3 2 Interior of Front Cover Right Side 3 3 3 3 Rear View 3 4 c 0 D 0 0 c 3 1 RID 1OA...

Page 22: ...ver is opened for mounting and dismounting of flow cell and piping I No I Description 7 Function 1 0 I controipanel I Performsparasnetexsettingand displays set values I I Front cover openingbutton 1 P...

Page 23: ...n 4 8 I I I I H I 1 I Cell outletport Tube holder Connectionport for leak tube NormallyCOM C S back pressure tube 03mmI D x I m 4 9 Securesthe connected tube Connectsthe leak tube to this port 4 13 So...

Page 24: ...16 REMOTEconnector Externalinput and output texminals Groundingterminal Power supply cord connector Fuse holder These terminals connect externalequipment This terminalis usedfor grounding The power su...

Page 25: ...allation Requirements 4 2 4 2 Example of SystemLayout 4 3 4 3 StackingModules 4 4 4 4 Electrical Connections 4 5 4 5 PlumbingConnections 4 6 4 6 Connectingthe Recorderand Integrator 4 11 4 7 Connectin...

Page 26: ...act with solvent 4 Corrosivegas and dust Avoid installation in a place exposed to corrosive gases or dust 5 Electromagneticnoise Avoid locations subject to intense magnetic or electromagnetic fields U...

Page 27: ...uirements are shown below Detector RI 0 1QA Column oven CTO 1OA Manual injector 7725 Pump LC IOAD Reservoir box Chrornatopac C RGA Degasser DGU 106 Option bpx S Caution Each component of the LC 1OA ha...

Page 28: ...equipment can be stacked and locked for safety in case of an earthquake etc using the suppliedlockingplate 1 Refer to the figure below and remove the screws fastening the equipmentcover 2 Attach the m...

Page 29: ...pplied with the unit to the power supply cord connector at the rear of the unit and plug the male connector into a power supply outlet The supplied power cord is a three conductor 3 prong type When co...

Page 30: ...ibedbelow Cut the SUS pipe 1 6 x 0 3 supplied as a liquid pump accessory to the necessary length for the pump outlet and injectorport 2 Installthe male nut and ferrule to both ends of the SUS pipe Att...

Page 31: ...column 2 Attach a male nut and a ferruleto the ends of this pipe 3 Connect the ends of the SUS pipe to the injector and the column respectively Attach the ferrule and the male nut supplied with the in...

Page 32: ...ube on the perpendicular When the tube is cut on a diagonal dead volume is generated which deteriorates separation When the flow selection block option is used refer to section 5 3 Piping of Flow Sele...

Page 33: ...of the FRC 1OA to the detector outlet directly Note that the maximum flow rate varies depending on the preparativehead of the FRC FRC 1OA inletpipe Insidediameter m x Length cm FRC 10A outlet pipe Ins...

Page 34: ...outlet port When piping for the detector inlet and outlet is completed secure the two piping tubes in the tube holder as shown in the figure below I 1 IRID 1OA I Fitthe tubes inthe tube holder When th...

Page 35: ...ecorder or the 6th terminal I mV full scale recorder The 7th terminal of RID 1OA Green Green Groundingterminal When using a stranded wire twist the end tightly or tin it with solder Using a small scre...

Page 36: ...voutput terminals at the rear of the RID 1OA The connection procedure is similar to that in 1 Connecting with recorder Connect the cable supplied with the Chromatopac to the Chromatopac side and conne...

Page 37: ...ct the straight type joint to the liquid leak tube at the bottom of the equipment and insert it into the drain bottle L type leak tuhe Liqiud leak tube U Connecting port of liquid leak tube Straight t...

Page 38: ...5 1 Precautions for Operation 5 2 5 2 Fundamentalsof Operation 5 3 5 3 Plumbing of the Flow SelectionBlock 5 13 5 5 Additional Functions AUX FUNC 5 21 1CONTENTS 1 5 4 Creating and Executing Time Progr...

Page 39: ...ls are the most frequent causes of trouble in any detector After analyzing a high concen tration sample thoroughly flush it from the flow cell using a large amount of mobile phase Buffer solution crys...

Page 40: ...lance adjustment is moved to the set position and the instrument seeks the home position M 101 rsnge mode f S E E K I N G H O M E The position is adjusted so that the optical balance is at the optimum...

Page 41: ...FF and contact your Shimadzu Service Representative temp cont The display unit consists of display screen and indicator lamps as shown below Lights when the power is being supplied to the temperature...

Page 42: ...n on the recorder It is moved upward by pressing A side and downward by pressing V side Press this key to add Mark to the data being recorded in the recorder by pressing this key Mark is not valid in...

Page 43: ...key to clear the display and alarms when an error is displayed Equipment failure errors cannot be cleared with this key Deletes a line in the time program Advances to the next item in the display scr...

Page 44: ...avoid trouble caused by bubbles refer to the following When the pump sucks bubbles degas the solvent with the ultrasonic cleaner If dirt on the suction filter is the cause clean the filter with the ul...

Page 45: ...ed When the index is 500 x 10 FUU or less use mode A Note that the settingof mode P has wider measurement range while it has the larger baselinenoise The range value will default to 100 when the mode...

Page 46: ...having refractive index up to about 100times as much as the setting range can be recorded Set the measurement range at a value about 1 80 of the expected maximum peak refractive index Normally the re...

Page 47: ...value in the parameter AUX RANGE Relation between AUX RANGE value and INTEGRATOR terminal output are listed in the table below INTEGRATOR terminal output Remarks 1x O R I U N 1 x 1 0 3 RIUN Compatibl...

Page 48: ...0 scale on the chart paper 5 Press zeroshiftAV1 to move the baseline to a desired position and start analysis 6 Press the key to return the baseline to the previous position 9 Settingthe RESPONSE In...

Page 49: ...idth at half height increases It is recommended that response be set at a value such that for a given half height width the peak height drops no more than 10 The relation between response time peak ha...

Page 50: ...Mode Setting Application Analytical A For general analysis The flow lines are the same as that of the RID 10A without the flow selection block This mode is compatible with the FUD 6A P For measuring...

Page 51: ...x lo00 FRC 1OA accessory FRClOA outlettubing 0 D x 1 D x Length rnrn 3 2 X 1 6 X lo00 FRC 1O A accessory 3 2 X 1 6 X lo00 Note When a fractioncollectorFRC 1OA is used use the followingtubing I I 150 I...

Page 52: ...2 Do not tubing Tubingconnectioninthe largescale preparativemode set the instrument to mode L with analytical and preparative connection Similarly do not set the instrument to mode A t 0 or P in larg...

Page 53: ...ls of Operation 1 10 1EVNT 1 EVEhToutputON OFF 0 1 2 12 Refer to section 5 5 Additional Functions 1POL 1 olaritysetting STOP IO I Ends a program Not applicable Positive polarity Negative polarity RNGA...

Page 54: ...e shows that the time program is set for 10steps and there are 22remaining steps 2 PressLEnter 1to display the following I I I 6 Commandname 0 Setvalue Elapsed time fiom time program start minute 3 Pr...

Page 55: ...ess Enter balance lo4 range mode 1 0 0 0 Z E R O I I I I I I I I Each time Ifunc is pressed commands are displayedsequentially Press IEnter when the objectivecommand is displayed to set the command ba...

Page 56: ...lay the step to be deleted 2 Press lshlftland 1 2 0 0 0 R A N G A 2 1 The first step in the program is deleted and the second step is displayed When the second step is not set the following is display...

Page 57: ...utes When parameter is changed while executing a time program the changed value is valid only until the end of the program On completion of the time program the parameter is reset to the value set bef...

Page 58: ...KEY 1 1 1 _ _ _ 1 Sets addressof the RID1OA for control via system controller SPAN A SPANP SPAN L Inputs the span value of the analysismode Inputs the span value of the preparative mode Inputs the spa...

Page 59: ...reat the measuring unit When the flow rate is larger than 3 d m i n turn this OFF When the flow rate is less than 3 mL min set the temperature to the room temperature 12 c balpma m 103 range mode A C...

Page 60: ...ror of theRIDlOA U s e f u lforcommunicatingto externalequipment Both functions describedabove areenabled MONIT TIME Monitors program elapsed time LAMPTIME Monitors the lamp lit time r 0 Q d c L When...

Page 61: ...ting port No when this equipment is connected to the system controller SCL IOA for use Input the addressnumber then press Enter For port No see section 7 1 Connection with System Controller SCL 1OA L...

Page 62: ...L Span factor i n mode L baiance F I I I range mode S P A N L 1 0 0 Inputs the spanvalue of large scalepreparative mode Large scalepreparative mode is applicable when the flow selection block option...

Page 63: ...c Chapter 6 Initial Performance Test 1 6 1 System Performance Check 6 2 6 1 RID 1OA...

Page 64: ...the input cable of the Chromatopac to the INTEGRATORoutput terminal of this equipment using the signal cable supplied to this equipment through the terminal block suppliedto the Chromatopac Turn ON t...

Page 65: ...to 8 on the Chromatopac Chromatopac full scalebecomes equivalent to about 256 x 10 6RIU 12 Press 5 and on the Chromatopac plotting 14 Inject sampleto the injector 15 Press of the Chromatopac simultane...

Page 66: ...4 f hia t tose lj 324 CALCULATION REPORT CH PKNO TIME AREA 1 7 379 s40909 s 9 349 551971 9 11 661 862498 10 15 324 533931 12 22 591 761268 TOTAL 3553579 HEIGHT 33027 27933 30889 14479 12786 139055 I F...

Page 67: ...Chapter 7 Control from the External Equipment 7 1 Connection with System ControllerSCL 1OA 7 2 7 3 ConnectingExternalInput and OutputTerminals 7 10 7 2 Controlfrom the SCL IOA 7 3 I 7 1 RID 1OA...

Page 68: ...REMOTE connector of the SCL 1O A r RlPlOA SIL FRC REMOTE 1 17 1 21 1 37 1 47 r5 1 r 6 1 r l r 8 7 4 Do not bend the remote control optical cable at less than a 120 I angle 2 Set a value for ADRS in A...

Page 69: ...stored in the SCL and are required only once unless the systemconfiguration is changed Modulename S Y S T E M C O N F I G U R A T I O N L I N K E D L I N K E D L I N K E D L I N K E D F R C L I N K E...

Page 70: ...P D E T A I S O R A N G E 1 0 0 0 0 A F L O W 0 0 0 0 m l m i n P O L 1 8 F L O W 0 0 0 0 m l m i n C E L L T 4 0 0 Detector Sub controller J I _ _ _ _ D E T 6 C F L O W 0 0 0 0 ml min A P R E S 0 k g...

Page 71: ...e detector Example If the F Iparameter is set to 1 the LED for polarity on the detectoris lit and the polarity is reversed D E T E C T O R C O N T R O L F I L E 0 _ _ _ _ DET A R I D R A N G E 1 0 0 0...

Page 72: ...steps after accessing the help line with the f u c key To set the parameters for two detectors refer to item 2 above Parameters which can be set in the DET CONTROL screen arelisted in the table below...

Page 73: ...set in this screen commands for the detector aswell as other instrumentsare included e g solvent delivery u n i t etc T I M E P R O G R A M F I L E 0 B GE 3 0 0 S T E P S L E F T I T I M E I F U N C I...

Page 74: ...E R I I 0 O Ol 500 0 0 1 0 01 1 100 1 1 500 0 1 5ooo 1 100 Commands corresponding to the selected module are displayed in the command table An example for the command table is shown below 3 1 R E S P...

Page 75: ...file being displayed Copiesthe file being displayed to a different file Moves the cursor at the device name in the command table to the left Moves the cursor at the device name in the command table t...

Page 76: ...l recorder Signal output terminal connected to ili T B l External o equipment input terminal p I 1 7 II 1OmV full scale I L 1 recorder 1 i 1mV recorder External terminal T B 2 u T B 1 of EVENTparamete...

Page 77: ...at the end It is unnecessary for supplied remote cable When the core wire is solid insert it into the hole of a terminal while pressing the button above the hole using a small screwdriver When the wir...

Page 78: ...Chapter 8 Maintenance 8 1 Cleaning the Flow Lines 8 2 8 2 SpanAdjustment 8 3 8 3 Replacement of Fuse 8 7 Q 8 4 Periodical Cleaning 8 8 0 f 0 r C Q c C I 8 1 RID 1OA...

Page 79: ...e substance Be extremelycareful when handling mitric acid Deliver acetone from the inlet port using the syringe and adapter During supply turn the M o w on to deliver solvent to the reference side The...

Page 80: ...L I Refractive index standard sample glycerinsolution0 872 g L Dissolve 43 6 g of glycerin USP grade or equivalent in the 1L of water and dilute this solution 50 times for the refractive index standar...

Page 81: ...the inlet port The baseline will move up ward by 80 of the full scale Record the base line level in caseof standard solution Read the difference between the base line levels of the distilled water and...

Page 82: ...follow the procedures from 4 above Input the span value obtained at each mode into SPAN P and SPAN L each RIU and the 0 90 x 100 102 4 0 88 t New SPAN A 8 2 2 When span adjustmenti sperformedusing the...

Page 83: ...e cursor to read the difference between the levels of the distilled water and the standard sample 10 When the refractive index of the standard sample is R x 1Od RIU the span factor is calculated by th...

Page 84: ...O 072 01652 23 Replace the blown fuse accordingto the following procedure 1 2 3 T u r nthe power switch OFF Disconnect the power cord from the power supply connector Catch the fuse holder cover with a...

Page 85: ...Periodical Cleaning If the cover or the panel of the unit is stained wipe out dirt or dust with soft cloth or a piece of paper If necessary use a non ionic detergent 8 8 RID 1OA...

Page 86: ...ication 9 1 Component Validation 9 2 9 1 I Test Procedureof Stand aloneUnit 9 3 9 1 2 Test ProcedureControlled from the SCL 1OA 9 5 9 2 System Validation 9 9 9 2 1 Test Procedureof IsocraticLC System...

Page 87: ...6 to 12 month Adjust the frequency of the inspection based on the actual operating conditionsof the LC system When the LC unit is operated continuously day and night the intervals between inspections...

Page 88: ...urce intensity is sufficient Test procedure 1 Fill the cell with distilledwater 2 Press the key severaltimes to display TOTAL EN 3 Record the light intensity value AcceDtance criteria TOTAL EN is more...

Page 89: ...he syringe and adapter to deliver distilled water to the 2 3 inlet port During delivery press the and R flow keys to flow the water to the reference flow lines After the inside of the sample celvrefer...

Page 90: ...d from the SCL IOA 1 Checkingthe lamp littime Content of inspection Thistest checks the lamp lit time Test procedure 1 Selectthe 6 MONITOR on the main menu of the SCL 10A to open the monitor screen Ex...

Page 91: ...y value AcceDtance criteria TOTAL EN is more t h a n6 000 3 When the value does not fall within reference value first clean the flow cell Refer to the section 8 1 Cleaning the Flow Lines Then increase...

Page 92: ...rd sample whose index is already known The test requires the followingreagents and equipment Distilledwater Standardsample Glycerin solution 0 Syringe Data processor Refer to the section 8 2 Span Adju...

Page 93: ...the full scale Record the baseline level when the cell is filled with standard solution When the Chromatopac is used press the E key to record the baseline 8 Read the difference of the baseline level...

Page 94: ...other hand if the results do not meet the acceptance criteria for holistic validation it implies that there is a problem in the LC system itself and modular validation should be performed for diagnosi...

Page 95: ...dependent on the operation status of the system General guideline is shown below To flush the flow line with solvents connect the inlet and outlet tubing of the column directly using a proper union C...

Page 96: ...00 T DBL o STOP TM 7 ATIEN 4 SPEED 5 Set the parameters of the data processor Monitor the baseline When a stable baseline is obtained press the zero point adjustment key of the detector Then inject lO...

Page 97: ...Time program FLOW 1 7 00 STOP 0VEN T 4 0 P MAX 200 Auto injector SIL 10NlOAil SAMPLING SYRINGESPEED 2 EXCESS VOLUME 50 Use default value forothers Detector RID 1OA AUX RANGE 2 1 x 10 m v RESPONSE 5 a...

Page 98: ...Chapter 10 Troubleshooting J 10 1 Symptoms Causes and Remedies 10 2 10 2 List of Error Messa es 10 4 1CONTENTS I L 10 1 RID 1OA...

Page 99: ...rminals are saturated in the negative end No signal w i l lbe output 1 Range is set to 0 2 Lamp does not light 3 OVERcondicionexist seeoVERsymptom AUX RANGEsettingis inappropriate 1 The solution in th...

Page 100: ...g mobile phase liquid supply stained 1 Drift Noise is Confirmation of cause Countermeasures With the flow cell tubing connected remove the cell and check it under flow conditions then check for bubble...

Page 101: ...is displayed when the home position sensor of the motor for driving the xerography does not properly work If this error is displayed turn the power of the unit off and contact your Shimadzu Service Re...

Page 102: ...Chapter I 1 Specifications 11 1 RID 10A Specifications 11 2 I CONTENTS I 11 1 RID 1OA...

Page 103: ...1 x Io md below filled with water time constant 1 5 sec room temperature Cell temperature setting Zero adjustment 30 60 C by 0 1T step OFF Optical balance optical zero Auto zero baseline shiftingFine...

Page 104: ...Erratum Time constant 1 5sec Erratum in the instruction manual Correction Time constant 3 sec There is an erratum in the description of time constant setting for noise specification in section 1I Z sp...

Page 105: ...Parts I 12 1 Consumablesand Repair Parts 12 2 12 2 Optional Parts 12 4 12 1 RID 1OA...

Page 106: ...parts for electric system I I 228 31627 91 228 31837 91 228 32578 91 Leak Sensor Battery 228 33743 91 228 25249 91 Heater Assy forinner block Heater Assy for outerblock 228 33738 91 228 33738 92 Phot...

Page 107: ...olenoid valve OUT 228 33816 01 228 33816 02 Flow cell Gasket for flow cell I Port INside I I 228 16447 I 228 32004 228 32057 I Port OUTside I I 228 16447 01 I Nu to mount port Washer to mount port 228...

Page 108: ...volume is applied MAX 150mUmin 2 required for parallel flow configuration for protection of cell andor solenoid valve in case over pressure at high flow rate is applied for example in preparative wor...

Page 109: ...Chapter 13 Reference I i L 13 1 Solvent Characteristics 13 2 I 13 1 RID 1OA...

Page 110: ...18 280 205 233 228 210 240 212 256 205 245 1 389 1 385 1 372 1 355 1 423 1 404 1 400 1 624 1 375 1 457 1 397 1 398 1 421 1 365 1 494 1 493 1 521 1557 1580 1SO5 1 350 1 498 1510 1 427 1 46 1S38 1 421 1...

Page 111: ...ol Formamide Water LC LC LC LC LC Gc LC LC Gc LC LC LC LC LC LC LC 329 215 265 380 330 210 210 190 268 268 268 285 205 380 1 532 202 1 376 80 1 450 156 1 550 211 1 536 191 1 420 101 1 449 175 1 625 23...

Page 112: ...rmaceutical Co Ltd Nakarai Pharmaceutical Co Ltd and Kanto Chemical Co Ltd GC indicates that the solvent is used as a stationary phase for gas chromatography and can be purchased from companies sellin...

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