Shimadzu RID-10A User Manual
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Shimadzu RID-10A User Manual

Shimadzu RID-10A User Manual

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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.
CHROMATOGRAPHIC & SPECTROPHOTOMETRIC
INSTRUMENTS DIVISION
KYOTO, 3 A P A N

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  • 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.
  • Page 2 Note that Shimadzu does not have any obligation concerning the effects resulting from the application of the contents of this manual. MS, MS-DOS, Microsoft and Visual Basic are registerd trademarks, and Windows is a...
  • Page 3 Follow the procedures described in the instruction manual. 3. Observe the warnings and cautions. 4 . Do not disassemble or modify the unit without approval from Shimadzu. Failing to do so may lead to a dangerous situation or damage of the unit.
  • Page 4 For safety of operation, this unit is provided with the mark at the portion where special cautions are required. parts where this m a r k is indicated, exercise special caution after When operating the reading m a n u a l . Replacement of fuses This unit uses the following fuse.
  • Page 5 VAOS I VAOS I...
  • Page 6 8. Solvent not usable HFIPA (Hexafluoroisopropyl alcohol) affects the materials used in the flow path and deteriorate the strength of the material. In the worst case, pipe may explode and high- pressure solvent scatters. As it is very dangerous, never 9.
  • Page 7 Liquid chromatography using flammable organic solvents as mobile phase requires proper care against fire, explosion, etc. Pakcularly, among various possible accidents, those caused by static electricity are difficult to anticipate, and tend to occur only with unexpected conditions which often make countermeasures insufficient. At a site where preparative liquid chromatography is practiced, a large amount of flammable substances may be used.
  • Page 8 If air drv Liquid is flowing at high speed small through a diameter tube. *Charge is easily accumulated if Insulated vessel (like polyethylene) Spark discharge Inflammable gas is stored in the head space of the vessel. Inflammable organic solvent is charged to a great extent.
  • Page 9 Preventive measure 2. Minimize the clearance of both inlet and outlet of vessel to prevent flame from entering the vessel. Cap with three holes for 18 liter and 4 liter cans (P/N 228-21 is available. Connect clip to metallic Minimize clearance by attaching a cap.
  • Page 10 Preventive measure 5. When it is impossible to use a conductive vessel, use caution in the following points. Set the vessel so that the pipe outlet will be placed below the liquid level in the vessel. Or, dip a grounded metal (ex. pipe connected to the main body of device) in the liquid.

  • Page 11: Table Of Contents

    General ......................Outline ......................Features ................Principle of Measurement .................... Chapter2 Parts List ................... Parts and Accessories Component Location and Function ....................Front View .............. Interior of Front Cover. Right Side ..................... Rear View Chapter4 Installation ..............Basic Installation Requirements ................
  • Page 12 .................. Component Validation ............Test Procedures of Stand-alone Unit ........9.1.2 Test Procedures Controlled from the SCL- 1 O A ..................System Validation ..........Test Procedure of Isocratic LC System Troubleshooting ..............Symptoms. Causes and Remedies 10-2 10.1 .................. List of Error Messages 10.2 10-4 Specifications...
  • Page 13 Chapter 1 General ..................... Outline Features ............... Principle of Measurement Flow Schematic RID-1OA...
  • Page 14 LC- 1 series. The RID-10A improves analysis productivity and convenience use like a UV detector. Its shortened stabilization time, the fact that it covers various applications from high sensitivity analysis to...
  • Page 15 Excellent stability Stabilization time after turning on the power has been shortened to reduce the waiting time for start of analysis. Excellent stability has been realized by employing the dual temperature control structure of the optical system and by improving the thermal design. 2.
  • Page 16 The optical system of this unit is shown in following illustration. The light radiated from the lamp passes through the lens slit and through the cell in the form of parallel rays, which is then reflected by the mirror and passed through the cell to form an image of the slit the photodiode.
  • Page 17 Principle of Measurement TOTAL Signal processing in mode P Signal processing is performed using the upper and lower parts of the photodiode as individual elements. Since the boundary between the upper and lower parts is slanted against a horizontal line, when an image of the slit moves horizontally, the balance of the light intensity in the upper/lower parts of the diode changes.
  • Page 18 The diagram shows flow lines in the RID-10A. flow flow switch is OFT, the solenoid valve is open at side When the The solvent passing through the sample cell flows into the outlet port, not into the reference cell. flow...
  • Page 19 Chapter 2 Parts List ................Parts and Accessories CONTENTS 2- 1...
  • Page 20 [Caution] When connecting the flow line and performing maintenance, be sure to use the parts described on this page or “1 2.1, Consumable P a r t s Normal function of the system is not and Repair when other parts are used. This equipment consists of the following components.

  • Page 21: Rear View

    Chapter 3 Component Location and Function ....................Front View ............Interior of Front Cover, Right Side ....................Rear View RID-1OA...
  • Page 22 RID-1OA Function Description Performs parasnetex setting displays set values. The front cover is opened for mounting and dismounting of cell and Front cover flow piping. Front cover opening button Press this button to open the front cover. RID-1OA...
  • Page 23 I I I Description Function Refer to page Connects the tube column. from I D . Normally back pressure tube I m ) . Tube holder Secures the connected tube. Connection port for leak tube Connects the leak tube to this port.
  • Page 24 Function Description Refer to page REMOTE connector This the connector for SCL-IOA. External input and output texminals These terminals connect external equipment. 7-16 Grounding terminal is used for grounding. terminal Power supply cord connector The power supply cord is connected here. Fuse holder Two fuses are provided in this holder.

  • Page 25: Basic Installation Requirements

    Chapter Installation ............. Basic Installation Requirements ..............Example of System Layout ................................Electrical Connections ................Plumbing Connections ..........Connecting the Recorder and Integrator 4- 1 1 ........Connecting the Drain Tube for Solvent Leakage 4-13 RID-1OA...

  • Page 26: Example Of System Layout

    Basic Installation Requirements take full advantage of the RID-1OA’s performance capabilities and to ensure its operational stability over a long service life, verify that the selected installation site satisfies the following requirements. 1. Ventilation Ventilate the room where the high-perfomance liquid chromatograph is located since the solvent used is flammable andor toxic.
  • Page 27 Example of System Layout Example liquid chromatograph system layout using this equip- ment and space requirements are shown below. Detector ( R I 0 - 1 Q A ) Column oven (CTO-1OA) Manual injector (7725) Pump (LC-IOAD) Reservoir Chrornatopac (C-RGA) Degasser (D G U - 1 Option bpx S Each component of the LC-1OA has a little clearance at the bot-...
  • Page 28 RID-1OA may be stacked on the pump (LC-IOASLC-lOAD/ LC- 1 OAT/LC- 1 OAi) or the column oven (CTO- equipment can be stacked and locked for safety in case of an earthquake, etc. using the supplied locking plate. Refer to the figure below and remove the screws fastening the equipment cover.
  • Page 29 Check the following points before connecting power supply. Supply voltage and capacity 228-32000-91 120V 150VA 228-32000-92 228-32000-94 When the power supply is not stable or the capacity insufficient, satisfactory performance is not possible. Verify the total power supply for the system before preparing the power supply. OFF.
  • Page 30 umbing Connections This section describes proper connection in a typical flow line as shown in the figure below: Flow line in the system Refer to the column oven instruction manual for installation of the manual injector and column oven. When the column oven is used, an injector holder and a column holder are optionally available for installation of the manual injector and the column.
  • Page 31 Connections Plumbing Manual injector Injector holder 3. Connecting injector and column A typical connection of a manual injector and a column is shown below: Cut the pipe (1.6 x 0.3 supplied to the pump, to the necessary length for connecting the injector and the column. Attach a male nut and a ferrule to the ends of this pipe.

  • Page 32: Plumbing Connections

    Plumbing Connections SUS pipe PEEK pipe Cut perpendicularly with a cutter knife. Cut perpendicularly. Mail nut 1.6MN Ferrule 1.6F Ferrule 1.6F PEEK Mail nut 1.6MN PEEK To detector Rear of manual injector Connecting detector and column A typical connection between the RID-1OA and a column is described in this section.
  • Page 33 Plumbing Connections Tubing Manual injector Manual injector Main body port PEEK (Tighten by hand) hand) Male 5. Detector outlet side piping Prepare a waste liquid bottle. Connect the drain tube to the detector outlet. Select one from the drain tubes listed in the table below depending on the applied flow rate.
  • Page 34 Plumbing Connections Main body outlet port When piping for the detector inlet and outlet is completed, secure as shown the two piping tubes in the tube holder in the figure below. RID-1 OA Fit the tubes in the tube holder. When the front cover is dosed.
  • Page 35 RECORDER terminal of the 1. Connection with recorder Connect the and the recorder using the supplied signal cable. RID-1OA (1 OmV full scale recorder) the 6th terminal Recorder The 7th terminal of RID-1OA Recorder GND Green Grounding terminal Green When using a stranded wire, twist the end tightly, or tin it with solder.

  • Page 36: Connecting The Recorder And Integrator

    Connecting the Recorder and Integrator 2. Connecting with Chrornatopac (integrator) INTEGRATOR Connect the Chromatopac to the terminals (TBl No. 3 and No. in the external inpuvoutput terminals at the rear of the RID- 1 OA. The connection procedure is similar to that in “1. Connecting with recorder.”...
  • Page 37 Each component in the LC-1OA series is designed so that solvent leakage is discharged from the liquid leak tube connection port either at the right side or the lower front side of the equipment. Connect the liquid leak tube if necessary. Connecting liquid tube in system...

  • Page 38: Fundamentals Of Operation

    Chapter 5 Operation ................ Precautions for Operation CONTENTS ..............Fundamentals of Operation ........... Plumbing of the Flow Selection Block 5-1 3 ..........Creating and Executing Time Programs 5- 1 6 ............Additional Functions (AUX-FUNC) 5-21 5- 1 RID-1OA...
  • Page 39 Caution Be sure to close the front cover during measurement. The baseline fluctuates when the front cover is opened or closed during high sensitivity analysis. Noise may be increased when the front door is kept open. Precautions to prevent clogging of the flow cell. Dusty or clogged flow cells are the most frequent causes trouble in any detector.
  • Page 40 OFF. ON and Power switch OFF state Power switch state When the power is tumed ON, the RID-10A operates follows: Turning power ON All of the dots in the display unit and all of the indicator lamps light. Control program version No. is displayed.
  • Page 41 When this message is displayed, the time program is initialized. When any other error message is displayed, turn the power and contact your Shimadzu Service Representative. Display unit The display unit consists of display screen and indicator lamps as shown below.
  • Page 42 Fundamentals Operation Edit keys Use these keys to input parameters and edit a time program (ten-key, etc.). shift shift Enter STD-func keys Auto zero key Press this key to perform zero adjustment. Returns the baseline to the zero position Zero shift key Press this key to move the zero position on the recorder.
  • Page 43 Fundamentals Operation (mode] These keys select the measurement mode. The measurement mode changes from A Analytical mode Preparativemode Large-scale preparative mode 5.3.2, the operation of each mode, refer to section Changing the Measurement Mode. These keys can be used to set time constant. Values from 1 to 10 can be set.
  • Page 44 Fundamentals of Operation Note When the liquid inside the flow lines is not sufficiently replaced with the mobile phase, the baseline takes longer to become stabilized and the drift becomes large. R flow ON/OFF several times at an interval of two minutes. Switching flow lines during solvent delivery at large flow rate in mode may damage the solenoid valve and the flow cell.
  • Page 45 Fundamentals of Operation When the above operation is repeated, the mode is changed form Mode L is only applicable when an optional flow selection block is installed. When the block is not installed, do not perform measurement in mode L. Refer to 5.3.1 for the mode setting when using the flow selection block.
  • Page 46 Fundamentals of Operation 7. Changing the range RECORDER When a recorder connected to the terminal, set the range at a value about 1.2 times as much as the expected maximum peak value. Maximum peak will be about 80% of the full scale ensuring that peaks remain on-scale.
  • Page 47 Fundamentals Operation (Exam p I e) 1, ATTEN When that range x lO-kUFS] Plot full scale When a Chromatopac is used as a recorder, connect it to the INTEGRATOR terminal and set the range at A?TEN on the Chromatopac side. is also necessary to make a rough range setting on the detector side since the dynamic range of the detector is extremely wide.
  • Page 48 5.2 Fundamentals of Operation 8. Zero adjustment of recorder Before starting analysis, adjust the zero position of the recorder as follows: Set the measuring range to 0 to short-circuit the recorder output. SHORT is displayed in the range display. (Refer to section 5.2.6, Setting the Range.) Adjust the pen position to 0 scale on the chart paper using the pen position recorder adjusting knob.
  • Page 49 of Operation RESPONSE Corresponding time constant of analog CR filter Minimum peak width value ( Letters in brackets are response at half-height 0.05 sec 0.1 sec ( F A S T ) 1.0 sec 4.8 sec 1. 5 sec 3.0 sec (SLOW) 13 sec 6.0 sec...
  • Page 50 When the RID-1OA is equipped with the flow selection block (option), measurement mode can be selected for high sensitivity analysis, preparative and large-scale preparative mode. Operation in the large scale preparative mode requires the optional block. Mounting of the flow selection block is performed by a service engineer.

  • Page 51: Plumbing Of The Flow Selection Block

    Plumbing of the Flow Selection Block Drain tube Use the following types of drain tube for large-scale preparative mode. The longer and/or smaller I.D. tubing than the specified one causes high back pressure beyond the value in the specifications of the detector, which may lead to damage of the detector. Max flow rate Drain tubing For extension...
  • Page 52 Plumbing the Flow Selection Block Column Fig. 2 Tubing connection in the largescale preparative mode set the instrument to mode L with analytical preparative tubing connection. Similarly, do not set the instrument to mode A or P in large-scale preparative tubing connection. 5-15...
  • Page 53 Command list Commands which can be used for a time progam are listed below. Command Description Setting range Remarks ZERO Execution of zero adjustment Not applicable MARK Marking on output for recorder Not applicable RNGA Designation of output range for recorder (mode A) Unit: x106RIUFS, Designation of output range for recorder (mode P) Recorder is short-circuited when...
  • Page 54 Creating and Executing Time Programs display screen 2. Explanation of The edit mode is used to create a time program. Press screen similar to the one below will be displayed. Number of steps already set Number of remaining steps The above example shows that the time program is set for 10 steps and there are 22 remaining steps.
  • Page 55 Creating and Executing Time Programs Flow setting Flow in setting a time program is shown below Press l s h l f t j a n d m . mode U S E D L E F T If no program Press is input (even range...
  • Page 56 Creating and Executing Time Programs It is unnecessary to set the time order of steps as they are automatically rearranged. STOP command at the end of a program unless the Set a program is to be operated continuously. When selecting a function, the previous function is displayed pressing Deleting a step Display the step to be deleted and press...
  • Page 57 Creating and Executing Time Programs 6. LOOP command program can be repeated any number of times using a LOOP command. TIME VALUE ZERO MARK LOOP According to the above setting, steps (1) and (2) are repeated 3 times at an interval of 30 minutes. When parameter is changed while executing a time program, the changed value is valid only until the end of the program.
  • Page 58 I Functions (A UX- FU N C) Add i ti The following Additional Functions are equipped with the RID- 1 OA. Command Function TOTAL EN Indicates the total quantity of light irradiated on the photodiode. Displays the quantity of light irradiated on each of the right and the side of CELL left...
  • Page 59 Additional Functions TEMP CELL mode ( C E L L T E M P (Cell temperature setting) Sets the cell temperature at the measuring unit. OFF. When the flow rate is larger than 3 d m i n , turn this When the flow rate is less than 3 set the temperature to the room temperature...
  • Page 60 T I M E (Monitors the lamp lit time) Displays the integration time of the lamp lighting. (unit hour) The life of a lamp is 20,000 hours. When the lamp life is close to the end, contact your Shimadzu Service Representative. 5-23...
  • Page 61 Additional Functions balance range mode CLOSE KEY C L O S E K E Y (Prohibition of key input) This function locks keypad, preventing entry, and is invoked by pressing (=]when the above display is shown. To restore simultaneously. keypad function, press ADRS range mode...
  • Page 62 Functions Additional range SPAN L 1 . 0 0 S P A N (Span factor i n mode L) Inputs the span value of large-scale preparative mode. Large-scale preparative mode is applicable when the flow selection block option is installed. 5-25 RID-1OA...

  • Page 63: System Performance Check

    Chapter 6 Initial Performance Test ..............System Performance Check 6- 1...
  • Page 64 This chapter contains an explanation of the operation check for the simple system in the figure below. Detector (RID-1OA) Column oven (CTO-1OA) Manual injector (7725) Pump (LC-IOAD) Reservoir box Option box S R I D - 1 O A LC- 1 O A D Helium gas Manual...
  • Page 65 6.1 System Performance Check Press [ZERO Enter on the Chromatopac to center the Den Position. Press m on the ChromatoDac to d o t the output. (10) Wait till the baseline becomes stable. Good example Stable There are examples Increases w i t h the time.
  • Page 66 System Performance Check (Example of chromatogram) CALCULATION REPORT HEIGHT 7.379 1 .. F r u c t o s e 9.349 551971 27933 Grucose 11.661 862498 Sucrose 15.324 533931 t ose 22.591 761268 Raf f i nose TOTAL RID-1OA...
  • Page 67 Chapter 7 Control from the External Equipment ........Connection with System Controller ..............Control from the SCL-IOA ........Connecting External Input and Output Terminals 7-10 RID-1OA...
  • Page 68 Preparation Using the supplied optical cable, connect the REMOTE connector at the rear panel of the RID-1OA and the REMOTE connector of the SCL- 1 O A REMOTE r 6 1 remote not bend the control optical cable at less than angle.
  • Page 69 Refer to the SCL-1OA System Controller Instruction Manual for basic operation of the system controller. Power and CONFIG screen Turn ON the SCL power switch to display the CONFIG screen. When the detectors and the are properly connected, is displayed at the right side of both (when two detectors are connected).
  • Page 70 Control from the SCL-1OA (menu) Main menu screen Press in the CONFTG screen to display the main menu screen. Press to access the main menu from any screen M E N U A N A L Y S I S F I L E P A R A M E T E R S P R O G R A M...
  • Page 71 Control from screen 4. DET CONTROL Press menu screen select the m a i n DETECTOR CONTROL screen. The detector parameters, which cannot be input on the screen, can be input on the CONTROL screen. These detector parameters control the operation of the detector from the (described in section 5.2,...
  • Page 72 7.2 Control from the SCL-1OA Using function key select the detector where parameters are to be set. This is only necessary when two detectors (e.g., A and B) are connected. When a detector B is selected and only one detector is connected, DETECTOR NOT CONNECTED is disulaved.
  • Page 73 Control from Sends marker signal to the recorder connected to the detector A. detector B. Sends marker signal to the recorder connected to Toggles between the detector or B for parameter display. Disables acceptance of any key input except for (lock release).
  • Page 74 7.2 Control from Move the cursor to a desired device name in the following line using F U N C T I O N F O R ( P U M P D E T . B O T H E R ) Commands corresponding to the selected module are displayed in example for the command table is shown the command table.
  • Page 75 Control from the SCL-1OA Outputs the time program on display to the printer connected to the Chromatopac the time program in the file being displayed. Erases all Copies the file being displayed to a different file. Moves the cursor at the device name in the command table to the left.
  • Page 76 external input and output terminals are T.B. T.B. 2. 1 and T.B.l External equipment input terminal External terminal recorder T.B.2 EVENT parameter in AUX. FUNC. Signal output terminal connected to output terminal Signal output terminal connected to 6 (+lmV F.S.) output terminal recorder.

  • Page 77: Connecting External Input And Output Terminals

    Connecting External Input and Output Terminals Appendix T. B. 2 Explanation EVENT2 Relay contact It is turned ON/OFF according to the EVENT Event output terminal 2 program or the set value of parameter in START Time program is started shorting this terminal input terminal with COM terminal.

  • Page 78: Chapter 8 Maintenance 8.1 Cleaning The Flow Lines

    Chapter 8 Maintenance ................. Cleaning the Flow Lines ..................Span Adjustment ................Replacement of Fuse ................. Periodical Cleaning RID-1OA...
  • Page 79 Dirty cells and piping may cause phenomena such as an unstable baseline or a large baseline noise due to pulsation of the solvent delivery pump. In this case, clean the flow lines with the following procedures. be prepared Syringe Adapter Water Acetone nitric acid...

  • Page 80: Span Adjustment

    Span adjustment should be performed over each mode of A, P and When a Chromatopac is used, refer to 8.2.1, and when an LC workstation is used, refer to 8.2.2. Inject the standard solution whose refractive index is known, and adjust the detector output so that the signal intensity can be verfied.
  • Page 81 Span Adjustment Set the detector that the plot full scale of the Chromatopac becomes 128 1 0-6 AUXRANGE of the detector Flow distilled water from the inlet port using the syringe and the adapter. Make M o w on(*) to purge the reference side flow lines with water.
  • Page 82 Span Adjustment (Example) When the measured refractive index is 102.4 R and the old span factor is 0.90, the new span factor is: 0.90 0.88 New SPAN-A Input the new span factor obtained by the above formula into SPAN-A. (12) Inject distilled water from the inlet port and finish the span adjustment.
  • Page 83 Span Adjustment Change display ATTEN so that the vertical axis of the chromatogram on the analysis screen becomes more than 100 pRru. (Example) When AUX RANGE setting is 2, set ATTEN Supply distilled water from the inlet port using the syringe and adapter.
  • Page 84 This unit uses two pieces of the following fuses. Be sure to replace the fuses of the same type and capacity. Rated voltage: 100-240 VAC P a r t 072-01 652-23 Replace the blown fuse according to the following procedure: T u r n OFF.

  • Page 85: Periodical Cleaning

    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.

  • Page 86: Component Validation

    Chapter 9 Performance Verification ................Component Validation CONTENTS ..........9.1 .I Test Procedure of Stand-alone Unit ......... 9.1.2 Test Procedure Controlled from the SCL- 1 OA ..................System Validation ..........9.2.1 Test Procedure of Isocratic LC System RID-1OA...
  • Page 87 Overview Each unit of the RID-10A system has been inspected stringently at the factory during the production process. The inspection procedures t h i s manual have been the inspection activities that are bothactually necessary and can be practically executed by the user. That is, this manual is intended to...

  • Page 88: Test Procedures Of Stand-Alone Unit

    7 years of use 8 hours a day. It is recommended that the lamp be replaced before the expected end of life to avoid the inconvenience of instrument failure. To replace the lamp, contact your Shimadzu representative or service engineer. 2. Checking the lamp intensity Content of inspection This test checks whether the light source intensity is sufficient.
  • Page 89 Component Validation Checking the span Content of inspection This test checks whether the refractive index value accurately measured and displayed by testing the standard sample whose index is already known. The test requires the following reagents and equipment. Distilled water Standard sample (Glycerin solution) Refer to the section 8.2 Span Adjustment.
  • Page 90 7 years of use 8 hours a day. It is recommended that the lamp be replaced before the expected end of life to avoid the inconvenience of instrument failure. To replace the lamp, contact your Shimadzu representative or service engineer.
  • Page 91 Component Validation 2. Checking the lamp intensity Content of inspection This test checks whether the light source intensity is sufficient. Test procedure Fill the cell with distilled water. Select the [6. MONITOR] on the main menu of the SCL-IOA to open the monitor screen. (Example of MONITOR screen] 40.0 7566...
  • Page 92 Component Validation Select the [6. MONITOR] on the main menu of the SCL-1OA to open the monitor screen. (Example of MONITOR screen] 40.0 7566 BALANCE Record the value of ACT-TMP as the actual temperature. TEMP. Acceptance criteria ACT TEMP value is within 0.1 "C of CELL TEMP The CELL...
  • Page 93 Component Validation Use the syringe and adapter deliver distilled water to the inlet port. During delivery, press t h e m and keys to flow the water to the reference flow lines. After the inside of the sample celvreference cell is replaced with distilled water, turn M o w by pressing the keys again.

  • Page 94: Outline

    Outline For the holistic validation of HPLC system, chromatographic analysis is performed under the analytical conditions specified by the manufacturer. The system status can be judged based on the obtained results. This is because the failure of the LC system may depend on the analytical conditions.

  • Page 95: System Validation

    System Validation Sample Anthracene in acetonitrile [Method for sample preparation] Place 2OOmg of anthracene in the volumetric flask of to it. Water (HPLC grade or equivalent) Isopropyl alcohol Check the connection of the units. Refer to the instruction manuals for details of the connection of each unit. Before installing the column, observe tubing connection of the LC system.
  • Page 96 System Validation 3. Procedure Outline of procedure is described below: Set the flow rate of the pump to l d m i n and column oven temperature to Start pump flow and temperature control. Then, confirm that the solvent comes out from the outlet tubing of the detector and no leak of solvent is observed at the connection.
  • Page 97 9.2 System Validation Parameter Setting for Inspection described below. [LC parameters] Initial condition LC Time program FLOW 7.00 STOP Auto injector [SIL-10NlOAil SAMPLING SYRINGE SPEED EXCESS VOLUME (Use default value for others.) Detector [RID-1OA 2 (1 RESPONSE 5. Acceptancecriteria acceptance criteria for the %RSD are shown below. 0.5% or less Retention time Peak area...
  • Page 98 Chapter 10 Troubleshooting ..............Symptoms, 10.1 CONTENTS ..................List of Error M e s s a ~ e s 10.2 10-4 10-1...
  • Page 99 Symptoms, Causes and Remedies When an abnormality occurs in equipment, follow the proce- below for checking unit. dures Symptom Possible cause Remedy OVER is displayed on the display for Recorder terminals the refractive index. the negative end. No signal w i l l be output Recorder baseline does not change.
  • Page 100 10.1 Symptoms, causes, Remedies Symptom of malfunctions Possible cause Confirmation of cause Countermeasures Degas the mobile spiking phase. Bubbles flowing Sawtooth baseline through cell With the flow cell tubing connected, remove the methanol to Bubbles trapped cell, and check under rinse the cell flow conditions, then at every stroke of...
  • Page 101 It is displayed when the temperature of the measuring point rises to 63°C over. If this error is displayed, turn off the power of the unit and contact your Shimadzu Service Representative. balance range mode 2. Set value loss error...
  • Page 102 Chapter Specifications RID- 10A Specifications 1 1-2 CONTENTS 11-1 RID-1OA...
  • Page 103 Specifications RID-1 OA method Measuring Deflection Refractive index range (RIU) 1-1 -75 Measurement range (RIU) 0.01-500 x (Analysis mode) 1-5000 Linearity (RIU) % 1 5 x 10" (Analysis mode) Maximum operating flow rate (mumin.) 20 (with option installed 150) Baseline noise (RIU) 0.25 1 x Io'md below (filled with water, time constant 1.5 sec., room temperature Withstand pressure ( m a )
  • Page 104 Erratum in the instruction manual There is an erratum in the description of time constant setting for noise specification in section 1 I-Z(specification). Err a tum Correction Time constant 1.5 sec 3 sec Time constant...

  • Page 105: Consumables And Repair Parts

    Parts I’ ..............Consumables and Repair Parts 12.1 12-2 ....................12.2 12-4 12-1 RID-1OA...
  • Page 106 1. Consumables Life: 20,000 hours (equals to more 228-32445-91 years by 8 hours operation per day), compati- ble with RID-6A 2. Repair parts Description Remarks Part Number Panel, RID- 228-23009-98 Panel Switch, RID 228-23673-02 Power Switch 228-33968-9 1 228-23527-9 PCB, PCB-CPU90 ROM, RID-1OA (CPU90) 228-33806-91...
  • Page 107 12.1 Consumables and Repair Parts Part Description Remarks for flow lines Parts Solenoid valve 228-341 14-91 T u b e (for solenoid valve IN) 228-33816-01 T u b e (for solenoid valve OUT) Flow cell 228-32004 Gasket (for flow cell) 228-32057 228- 16447 Port,...
  • Page 108 Parts Optional Description Part Number Remarks Flow selection block including a block, tubing and flow diagram 228-34102-91 1) required when 20mUmin or larger flow volume is applied. (MAX 150 mUmin) 2) required for parallel flow configuration. Relief valve for protection of cell andor solenoid valve in 228-33615-9 case over pressure at high flow rate is applied, for example in preparative work.

  • Page 109: Solvent Characteristics

    Chapter 13 Reference Solvent Characteristics 13.1 13-2 13-1...
  • Page 110 Solvent Characteristics Boiling Point Viscosity Dielectric Solvent "7< ~ c p , <45' Cutoff Solvent Constant 0.25 e Source (Particular 21onm 1.267 <-2 1.88 P' and Dielect FC-75 (Fluorescent to LC) 1.276 1.86 FC-43 solvent) 210 orunder) 1.291 proportion to intensity) 1.389 0.47...
  • Page 111 13.1 Solvent Characteristics Water Boiling Point Viscosity Dielectric Solvent "7< .5cp, c 4 5 Source Cutoff Solvent Constant em 17.4 Acetophenone 1.532 1.64 18.3 Methylethyl ketone''' 0.51 Cyclohexanone 1.450 34.8 1.550 25.2 10.9 1.536 miscible Dioxane 1.420 Tetramethyl urea 23.0 10.7 Quinoline 1.625...
  • Page 112 13.1 Solvent Characteristics indicates solvents most suitable for LC, having convenient boiling points "C cp) and low viscosity (2 0.5 cp). indicates solvents with very low viscosity and boiling point. "LC" indicates that the solvents are commercially available specifically for LC from following companies: Burdick Jackson, Baker Chemical, Mallinkrodt Chemical, Fischer Scientific, Waters Associates and Manufacturing Chemists, (Note: In Japan, they are also commercially available from...

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