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Showa Denko Shodex RI-101 Service And Maintenance Manual

Refractive index detector
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Shodex RI-101
Refractive Index Detector
Service and Maintenance Manual
High Sensitive Refractive Index Detector
for High Performance Liquid Chromatography
Publication No. ______________

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  • Page 1 Shodex RI-101 Refractive Index Detector Service and Maintenance Manual High Sensitive Refractive Index Detector for High Performance Liquid Chromatography Publication No. ______________...
  • Page 2 ©Copyright SHOWA DENKO K.K. 2000 All rights reserved. Reproduction, adaptation, or translation without prior written permission is prohibited, except as allowed under the copyright laws Part No. XXXXX First Edition: May 2001 Printed in Japan Important Notice The information contained in this manual is subject to change without notice.
  • Page 3 The following is a Federal Communication Commission advisory: WARNING This equipment generates, uses, and can radiate radio frequency energy and if not installed and used in accordance with the instruction manual may cause interference to radio communications. It has been tested and found to comply with the limits for Class A computing device pursuant to Subpart J of Part 15 of FCC rules, which are designed...
  • Page 4 It is important that you operate and service described below. equipment in accordance with this manual and any additional information that may be provided by Showa Denko from time to time. Alerts you to potentially hazardous situations WARNING that could result in serious injury, and how to...
  • Page 5 SHOWA DENKO warrants its products against defects in materials and workmanship for the period of twelve (12) months from the date of shipment out SHOWA DENKO will, at its option, repair or replace of its factory. products that are proved to be defective.

  • Page 6: Table Of Contents

    INDEX SECTION 1. INTRODUCTION ............1 1-1. Principle of refractive index detection...............1 1-2. Specifications .....................3 SECTION 2. UNPACKING AND INSTALLATION ..4 2-1. Installation Site Requirements................4 2-2. Power Requirements ..................4 2-3. Unpacking and Inspection..................4 2-4. Standard Accessories ..................5 2-5. Loosing the locking screws ................6 2-6.
  • Page 7 SECTION 4. GETTING STARTED ..........24 Just in Case ! 4-1....................24 4-2. Start Up......................24 4-2-1. Unattended Start Up..................24 4-2-2. Manual Start ....................25 SECTION 5. MAINTENANCE ............26 5-1. Cell Cleaning.....................26 5-1-1. Preparations ....................26 5-1-2. Cleaning......................26 5-2. Validation (Primarily for Customer Use)............29 5-3.
  • Page 8 8-2-4. Solenoid Valve....................55 8-2-5. Main Board and A/D-D/A Board..............56 8-2-6. Pre-Amp Board...................57 8-2-7. Output Board....................57 8-2-8. Front Panel Assembly and its components..........58 8-2-9. Leak Sensor....................59 Appendix 1. Shodex RI-101 Components and Subassemblies ......60 Appendix 2. Miscibility Chart of Solvents ............61...

  • Page 9: Section 1. Introduction

    Shodex RI-101 is a deflection or Snell type refractive index detector. Snell's law states that a parallel light beam, when passing through a dielectric interface separating two media of different refractive index at an angle of incidence greater than zero, will be refracted as a function of the magnitude of difference of the refractive indices of the two media.
  • Page 10 During operation, Shodex RI-101’s reference and sample cells are filled with mobile phase. The reference cell is then isolated from the flow path and mobile phase flows through the sample cell only. As long as no difference exists between the refractive indices of the media of the two cells, there is no refraction of the light passing through them.

  • Page 11: Specifications

    1-2. Specifications l Construction Deflection type l Refractive Index Range 1.00 to 1.75 l Range 512 micro-RIU l Linearity 600 micro-RIU l Noise =/<2.5 nRIU( Response : 1.5 seconds ) l Response Time 0.1, 0.25, 0.5, 1.0, 1.5, 2, 3, 6 sec. l Polarity Positive/Negative l Auto Zero...

  • Page 12: Section 2. Unpacking And Installation

    Section 2. Unpacking and Installation 2-1. Installation Site Requirements To install Shodex RI-101, please make sure that any of followings shall be kept away from it to prevent interference on your analysis. Refractive Index Detector, in general, is very sensitive to the change in ambient temperature and airflow that results a drift of baseline.

  • Page 13: Standard Accessories

    CAUTION Shodex RI-101 weighs 13 kgs (27 lbs). Use proper lifting techniques to avoid potential injuries. To remove the detector from the box, hold the bottom of the cabinet. Never attempt to lift by front panel or terminals. CAUTION Shodex RI-101 is packed with a number of accessories.

  • Page 14: Loosing The Locking Screws

    (2) locking screws (5mm Allen bolts). As you are installing Shodex RI-101, please make sure to loosen these screws. Move Shodex RI-101 to the side of a bench to make the locking screws accessible while supporting it to prevent it from falling.

  • Page 15: Replacing Fuse

    WARNING: SHOCK HAZARD Electrically conducting spills occur when conductive HPLC solvents are spilled on or in the instrument. Ground the instrument properly to protect the operator from electrical shock. Proper grounding also protects the instrument from power line noise. Verify that the instrument is properly grounded through the power line ground terminal.

  • Page 16: Tubing Connections

    2-6-3. Tubing Connections Connection to the Inlet CAUTION Shodex RI-101 must be the last component in your LC system. No detector or backpressure regulator can follow it. Do not use narrow-bore tubing for the outlet Hook up the narrow-bore stainless steel tubing of the Standard Accessory (0.25 mm ID, 1M long) with the inlet(IN) port of front panel.
  • Page 17 Integrator Connection Using the output signal cable supplied in the Standard Accessory, connect one end to the integrator, white lead to integrator negative (–) and red lead to integrator positive (+). Connect the third lead to the GROUND (FG). Red lead White lead Other Cable Connection For the following cable connection, please use duplex lead wire.

  • Page 18: Solvent Recommendations

    2-7. Solvent Recommendations General Recommendations Grade of Solvents HPLC grade solvents are recommended for better instrument performance and chromatographic data. Solvent Filtering All solvents, including deionized water, should be filtered by in-line solvent filter. Solvent Degassing Solvents should be properly degassed prior to use. Solvents that are not properly degassed may cause bubble formation in pump heads and in the detector cells potentially causing pressure flow problems and a noisy chromatographic baseline.
  • Page 19 If a solvent listed below is in use, flush out all the flow path sufficiently with an inert solvent that is compatible with your chromatographic system. Buffers, acids, and other highly ionic aqueous solutions should be flushed out with large amounts of water (5-10 times the volume of liquid from pump head to detector outlet If you neglect this flushing, the pump, injector, and column may become corroded and badly damaged.

  • Page 20: Characteristics Of Commonly Used Mobile Phase

    Characteristics of commonly used mobile phase (Those in bold should not be employed) Polarity Viscosity Refractive Flash Fire Point Vapor Boiling Gravity P20deg-C Index Cut-off Point Density Point (deg-C) Upper Lower (nm) (deg-C) (deg-C) Fluoroalkanes -0.25 1.25 0.00 0.23 1.358 <-40 308.9 n-Pentane...

  • Page 21: Front View

    Section 3. Functional Keys and Displays 3-1. Front View (6) (7) (10) (11) (12) (13) (14) (1)Power Switch (2)Solvent Leak Indicator (3)Power Indicator (LED) (4)Liquid Crystal Display (LCD Screen) (5)Start Up Sequence Key (6)Purge Key (7)Auto Zero Key (8)Marker Key (9)Arrow Keys (10)Cancel Key (11)Enter Key...

  • Page 22: Functional Keys And Displays

    3-2. Functional Keys and Displays (1)Power Switch Press this key once to turn on or off the unit. (2)Leak LED Illuminated when solvent leak is detected. (3)Power LED Illuminated when power is on. (4)LCD Display Liquid Crystal Display (5)Start Up Sequence Key Press S.Seq key once to call Start-Up Sequence.

  • Page 23: Rear View

    3-3. Rear View (10) (11) (12) (1)External Signal In (Marker) (2)External Signal In (Auto Zero) (3)External Signal In (Purge On) (4)Signal Out (Error) (5)Signal Out (Solvent Leak) (6)Signal Out (Ready) (7)Integrator Our (8)Ground for signal cable (9)Recorder Out (10)RS-232C Port (11)Ground Terminal (12)Power Inlet...

  • Page 24: Side View

    3-4. Side View Drain Port In case of internal solvent leak, solvent will be expelled from this port. Connect Teflon® tubing (6mm OD, 4mm ID). Lead the tubing to a safe waste disposal container always.

  • Page 25: Home Screen (Indicators And On-Screen Buttons)

    3-5. HOME Screen (Indicators and On-Screen Buttons) (10) (11) (12) (13) (1)Optical Balance This indicates current state of optical axis balance by the position of blue color box. Normally, the position of blue box should be in the center. If it isn’t, press o key to do "Auto-Zero".
  • Page 26 (8)Tab Showing available menus to choose. Following is a list of tab that you can choose. Choose desired tab by [-->] or [<--] key. Then, press [up arrow] or [down arrow] key to go into the screen. HOME PARAMETERS (Parameter Setting) OPERATING: Operating Condition S.

  • Page 27: Parameters Screen (Start Up Sequence)

    3-6. PARAMETERS Screen (Start Up Sequence) (1)Mode Choose one of built-in sequences (Fine, Standard, Coarse) from the menu or make your own (Custom). Move cursor by [up arrow] or [down arrow] key to “Mode”. Press [-->] or [<--] key to choose the mode. (2)Purge Cycle This will repeat on/off of purge solenoid valve to remove air bubbles trapped in the flow cell.
  • Page 28 (7)Drift Set the target drift value here. (8)Noise Set the target noise value here. (9)? Help To exit from this screen, press Enter key to save those changes that you have made. Press Cancel key to cancel those changes. Both case, the cursor will move back to the tab.

  • Page 29: Parameters Screen (Operating Parameters)

    3-7. PARAMETERS Screen (Operating Parameters) (1)TYPE “Analytical” analytical type: Flow Rate: Do not Exceed 10ml/min! “Semi-micro” semi-micro type: Flow Rate: Do not Exceed 1ml/min! “Preparative” preparative type:Flow Rate:Do not Exceed 150ml/min! (2)Recorder Range Recorder range setting. Choose the field by arrow] or [down arrow] key and edit by [-->] or [<--] key.

  • Page 30: Error Messages

    3-8. Error Messages To alert you about the situation that is hazardous or may cause a deterioration of your analysis, Shodex RI-101 flashes following six different error messages. Beep When any invalid command or editing is made, Detector beeps once for 0.5 second.
  • Page 31 “Optical Balance Error. If you have this error as you are turning on Shodex RI-101, please contact our local representatives in your area. (5)Optical Balance Error This indicates that Auto-Zero isn’t successful to get optical zero point.

  • Page 32: Section 4. Getting Started

    Section 4. Getting Started Just in Case ! 4-1. Prior to operation, check the following one more time. Locking screws are loosened Mobile phase solvent is freshly made and degassed well All wetted parts are chemically compatible to the mobile phase solvent Mobile phase flushed through the entire flow path;...

  • Page 33: Manual Start

    As soon as drift and noise met the target values during Measuring Time, the sequence is completed and READY sign comes up on the status bar. Shodex RI-101 is ready for the analysis. 4-2-2. Manual Start Set the parameter on operating parameter-setting screen (Refer to 4-7).

  • Page 34: Section 5. Maintenance

    To introduce cleaning solution into Shodex RI-101 by solvent delivery pump, connect a tubing line directly from the pump to Shodex RI-101 inlet port bypassing the column. Some cleaning solutions should be injected, however, directly into the flow cells by...
  • Page 35 [Binding of Proteins, Salts or Sugars] Connect detector with contamination free solvent delivery pump. Press Purge key to turn on the valve. Pump deionized water at 1ml/min flow rate and leave it overnight. You may want to wash the flow path with 0.1M NaOH priory if you know there is a potential of proteins binding.
  • Page 36 The sample and reference cells should be filled with water or air (blown dry) before proceeding. Filled the syringe with cleaning solution and connect to the inlet port of the Shodex RI-101. Carefully inject the cleaning solution. For safety, make sure that outlet tubing is led to drain bottle.

  • Page 37: Validation (Primarily For Customer Use)

    5-2. Validation (Primarily for Customer Use) From time to time, you are recommended to validate your HPLC system to keep an accuracy and credibility of your analysis. Shodex RI-101 has a very unique and user-friendly feature for this cumbersome mission.

  • Page 38: Maintenance Screen (Service Use Only)

    5-3. Maintenance Screen (Service Use Only) &note To activate the maintenance screen, you have to do a special key entry. Do not make customer possible to do unless it is only needed. 1. Select “Home” screen. 2. Press keys [up arrow] , [down arrow] Enter simultaneously.

  • Page 39: Span Adjustment Screen (Service Use Only)

    Dissolve in the 100 ml deionized, filtered, degassed water and dilute to flask’s mark. &note Use freshly made sucrose solution always. Equilibrate Shodex RI-101 by pumping deionized water through both reference and sample cells. Use the same deionized water as that used to prepare the sucrose standard solution.

  • Page 40: Span Validation (Primarily For Customer Use)

    100 ml deionized, filtered, degassed water and dilute to flask’s mark. &note Use freshly made sucrose solution always. Equilibrate Shodex RI-101 by pumping deionized water through both reference and sample cells. Use the same deionized water as that used to prepare the sucrose standard solution.

  • Page 42: Section 7. Troubleshooting

    You will begin by adding the pump to Shodex RI-101 first and you will add the column last. If another type of detector is available, it is a good idea to use it before Shodex RI-101 to aid in troubleshooting as reference.

  • Page 43: Troubleshooting (Q And A)

    7-4. Troubleshooting (Q and A) Problem Possible Cause Solution Solvent Leak Loosely connection at Inlet and Check if there is any solvent leak Outlet ports. Broken Cell Remove cabinet cover and check if you see a liquid drained out of Damaged Solenoid Valve optical block.
  • Page 44 Problem Possible Cause Solution Null Glass Stepping Motor (Motor-Lock) or Remove cabinet cover and check Motor Malfunction if the motor shaft rotates or not Home Position as the unit is powered on. The (Continued) shaft extends out of optical block (right hand side of front end of optical block).
  • Page 45 Problem Possible Cause Solution Noise Bubble in the pump. Purge pump heads. Use only premixed/degassed mobile phase. Bubble in the detector. Elevate drain reservoir above the level of the flow cells to create slight backpressure. Premix and degas mobile phase well. Dirty flow cell(s).
  • Page 46 Problem Possible Cause Solution Contaminated or non-HPLC grade Prepare fresh mobile phase solvents. (premixed/degassed) Vapor pressure of mobile phase is Reduce turn temperature too high for operating temperature control off. causing bubble formation Modify method to exclude or reference cell. decrease concentration troublesome solvent.

  • Page 47: Troubleshooting (Diagnosis Flow Chart)

    7-5. Troubleshooting (Diagnosis Flow Chart) All Displays Are Off Is there any loosen Secure connection! connection in line? Replace Fuse! Blown Fuse? Refer to Manual for proper rating Unexpected failure! Is the power switch Showa Please Call working? Denko to assist! Replace Power Switch Assembly.
  • Page 48 Low Light Intensity Broken Cell? Refer to Double check leak 8-2-1 Flow Cell Assembly tray for any leak? of Service Manual. No Leak Purge On and Pump sufficient volume of mobile phase. 1ml/min for 10min Bad Solenoid. Replace it! Clicking Sound of Refer to 8-2-4 Solenoid Valve Solenoid Valve? of Service Manual.
  • Page 49 Contamination is removed. Is alarm off? Choose Maintenance Screen Lamp is dead. Replace It. Check A+B voltage. Refer to 8-2-2 Source Lamp Is it Zero Volt? of Service Manual. Choose Lamp Output and change one step to increase or to decrease Weak Lamp.
  • Page 50 1ml/min for 10min Auto Zero Optical Balance Error is on again? Choose Maintenance Screen. Check Motor Step Number. Motor Step Number Unexpected failure! Call Showa Denko 0 or 400? to assist! Carry out Optical Adjustment. Refer to 8-2-3 of Manual...
  • Page 51 Unexpected failure! Call Is alarm off? Showa Denko to assist!
  • Page 52 Remove cabinet cover and power on the unit. Shaft stops as it goes Motor Shaft Moving? into block all the way? Unexpected failure! Call Showa Denko to assist! Can you rotate the Broken Motor. Replace the motor. shaft manually? Loosen Connector?
  • Page 53 Excessive Drift Pump thoroughly degassed mobile phase. (Use of on-line Problem Fixed? degasser is highly recommended.) Purge On and Pump sufficient volume of thoroughly degassed Problem Fixed? mobile phase. (1ml/min for 10 min) Broken Flow Cell? Refer to 8-2-1 Flow Problem Fixed? Cell Assembly of Service Manual.
  • Page 54 Excessive Noise Air Bubble trapped in Flow Cell? Purge on and Pump thoroughly Problem Fixed? degassed mobile phase. (on-line degasser is highly recommended.) Try to use solvent delivery pump that minimize pulsation of flow or Problem Fixed? use pulse dampener. Broken Flow Cell? Refer to 8-2-1 Flow Problem Fixed?

  • Page 55: Test Points On Pc Boards

    7-6. Test Points on PC Boards 7-6-1. A/D-D/A Board (28-5025) Test Point # Item Voltage TP 1 A-B (x1) 500micro RIU/V TP 2 Pre-Amp Signal Output B 0 to –2.5V TP 3 Pre-Amp Signal Output A 0 to –2.5V TP 4 A-B (x4) 125micro RIU/V TP 5 ADC Reference Voltage...

  • Page 56: Section 8. Repair Services

    Section 8. Repair Services 8-1. Optical Block 8-1-1 Dismount the optical block Power off the unit Remove the cabinet cover Disconnect Inlet and Outlet tubing that are fixed bulkhead unions on the front panel. Place the unit (optical block side as bottom) carefully as follow and remove M10 screws (4 ea) that fix the optical block onto the chassis.
  • Page 57 Dismount the optical block from the chassis. Detach connectors that connect the optical block and A/D-D/A board.

  • Page 58: Dismantle The Optical Block

    8-1-2 Dismantle the optical Block Loosen M3 screws (6 ea) and remove the optical block cover. Loosen screws and remove brackets that hold Inlet and Outlet Capillary tubing. Loosen screws (3 ea) and remove capillary tubing from the joint block.
  • Page 59 4. Loosen shock absorbing rubber foot (4 ea) Loosen screws (4 ea) that fix side cover. Remove the side cover. Remove heat-insulating foam. Detach drain tube from the elbow joint. (Press or squeeze the coupler edge to hatch the locking mechanism).

  • Page 60: Replacement

    Pull out the optical block out of optical block cabinet. 8-2 Replacement 8-2-1. Flow Cell Assembly Loosen screws (4 ea) and remove the top cover of optical block. Loosen M4 screws (12 ea) and remove heat-exchange block plates (both side of optical block) Loosen M3 screws (2 ea) that fix the Flow Cell Assembly.

  • Page 61: Source Lamp

    8-2-2. Source Lamp Loosen screws (4 ea) and remove the top cover of optical block. Loosen M3 set screw that mount source lamp to the lamp holder and carefully pull the source lamp out. Pull off wires (2 ea) out of Pre-Amp Board. Mount new source lamp back to the source lamp holder by reversal procedure.
  • Page 62 Manipulate two setscrews (both side) of source lamp holder to adjust a position of lamp so that light beam can cover the second slit (#5 of the above figure) completely. Center the light beam on photodiodes as below. Diagonal area represents a light beam.

  • Page 63: Solenoid Valve

    8-2-4. Solenoid Valve Refer to the procedure 8-1-1 Dismount the optical block ((1) to (3)) Detach front panel from chassis by removing M4 screws (3 ea) as follow. Dismount solenoid valve from the mounting plate by removing M3 screws (2 ea)

  • Page 64: Main Board And A/D-D/A Board

    Loosen finger tight fittings and disconnect plastic tubing from solenoid valve as follow. Detach wires of solenoid valve from A/D-D/A Board (Connector CN-10) Mount new solenoid valve back by reversal procedure. Make sure that tubing (in and out) are connected with right port. 8-2-5.

  • Page 65: Pre-Amp Board

    cables. 11. Dismount Boards from board stand by loosening M3 screws (4 ea). 12. Mount new Boards back to board stand by reversal procedure. 13. Mount the board stand back to chassis by reversal procedure. 8-2-6. Pre-Amp Board Refer to 8-1-1 Dismount the optical block, 8-1-2 Dismantle the optical block and 8-2-2. Source Lamp Disconnect wires from source lamp.

  • Page 66: Front Panel Assembly And Its Components

    8-2-8. Front Panel Assembly and its components Refer to 8-2-4. Solenoid Valve ((1) to (2)) Detach cables from Main Board (CN-4, CN-5 and CN-8). Detach Ground Cable from front panel (sheet metal) Detach front panel (sheet metal) from the front frame by loosening M4 screws (5 ea). Detach LCD Display (with mounting panel) from front frame by loosening screws (4 ea) Detach LCD Display from mounting panel by loosening M3 screws (4 ea) as follow.

  • Page 67: Leak Sensor

    Detach Key Assembly from front frame by loosening screws (4 ea) as follow. Mount either new Front Panel Assembly or its new components back to by reversal procedure respectively. 8-2-9. Leak Sensor Refer to 8-2-4. Solenoid Valve ((1) to (2)) Detach Leak Sensor from metal leak tray by loosening a screw.

  • Page 68: Appendix 1. Shodex Ri-101 Components And Subassemblies

    Appendix 1. Shodex RI-101 Components and Subassemblies Item/Description Part Number RI-101 Refractive Index Detector Operator’s Manual 9409000 A/D-D/A Board (28-5025) 8815220 Main Board (28-5026) 8815210 Pre Amplifier Board 8815470 Back-light inverter (PH-BLC08-K3) 4908230 Liquid Crystal Display (KCS057QV1AJ-A26) 4908240 Front Panel Assembly...

  • Page 69: Appendix 2. Miscibility Chart Of Solvents

    Appendix 2. Miscibility Chart of Solvents Acetic Acid Acetonitrile Chloroform Cyclohexane Methylene Chloride X = Immiscible Dimethyl Formamide Dioxane Ethyl Ether Hexane Methanol Methyl t-Butyl Ether Trimethylpentane Pentane Propanol-2 Tetrahydrofuran Water...

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