Hitachi CHROMASTER 5160 Instruction Manual

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Hitachi High-Tech Science Corporation 2013.

INSTRUCTION MANUAL

CHROMASTER 5160 PUMP

 Before using the instrument, read the safety instructions and

precautions carefully.

 Be sure to observe the safety instructions in this manual and

the WARNING/CAUTION labels on the instrument.

 Keep this manual in a safe place nearby so it can be referred

to whenever needed.

24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan

FOR

3rd Edition, August 2014

1st Edition, 2012

Part No. 892-9162-2

Table of Contents

Chapters

Table of Contents

Troubleshooting

Summary of Contents for Hitachi CHROMASTER 5160

Page 1  Keep this manual in a safe place nearby so it can be referred to whenever needed. 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 3rd Edition, August 2014 Copyright C Hitachi High-Tech Science Corporation 2013. 1st Edition, 2012 All rights reserved. Printed in Japan. Part No. 892-9162-2...
Page 2 NOTICE: 1. The Information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Tech Science Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Tech Science Corporation.
Page 3: Preface
PREFACE Thank you very much for purchasing Chromaster 5160 Pump. The Chromaster 5160 Pump is specifically designed for automatic analysis in a liquid chromatograph system. Note that physiologically or biologically active samples are not applicable to the Chromaster 5160 Pump because of possible infection with bacteria or viruses.
Page 4: About This Manual
ABOUT THIS MANUAL This instruction manual describe how to use and maintain the Chromaster 5160 Pump. This instruction manual. consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 OUTLINE (Isocratic System, Low-Pressure Gradient System)
Page 5: Important
Warranty on Product Limited Warranty The Chromaster 5160 Pump is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 6 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 7: Installation, Relocation And After-Sale Technical Service
(m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Tech Science shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 8: Technical Seminars And Training Courses For Users
(b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 9: Caution On Disposal Of Instrument
In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 10: Information For Users On Weee (Only For Eu Countries)
Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 11 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 12: Safety Summary
SAFETY SUMMARY Before using the Chromaster 5160 Pump, be sure to read the following safety instructions carefully. The hazard warnings which appear on the warning labels on the product or in the manual have one of the following alert headings consisting of a safety alert symbol and signal word WARNING or CAUTION.
Page 13: General Safety Precautions
Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Technologies. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 14: Warning Precautions In The Manual
SAFETY SUMMARY WARNING Precautions in the Manual WARNING 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 (Section 3.4, 3.6)  Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 15 SAFETY SUMMARY WARNING Precautions in the Manual (Continued) WARNING Electric Shock due to Contact with Inside of Instrument When removing the pump cover for part replacement, etc., there is a risk of electric shock. Be sure to turn OFF the power switch and disconnect the power cord from the receptacle in advance.
Page 16: Caution Precautions In The Manual
SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Heavy Instrument This instrument is as much as 16 kg. When carrying this instrument, exercise care not to incur injury by dropping it off accidentally. (APPENDIX 1) Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over. When installing the instrument, provide a proper means for preventing the instrument from tipping over accidentally.
Page 17: Warning And Caution Labels On Instrument
If any one of the warning labels becomes illegible due to deterioration, contact your local Hitachi High-Technologies Corporation sales representative or service office of Hitachi High-Technologies Corporation sales representative for replacement with a new one.
Page 18: Notice Precautions
SAFETY SUMMARY NOTICE Precautions Precautions on Use of Solvents  Fluororesin, PEEK, quartz, Vespel® and SUS316 materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials.  This instrument has internal parts made of materials that could be corroded by strongly acidic solutions, strongly alkaline solutions or organic solvents.
Page 19 SAFETY SUMMARY NOTICE Precaution (Continued) Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally. If necessary, conduct measurement on a control sample. SAFETY - 8...
Page 20: Table Of Contents
CONTENTS PREFACE ....................... 1 ABOUT THIS MANUAL ..................2 IMPORTANT ..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users ... IMPORTANT-4 Estimated Life time of the Instrument ........IMPORTANT-4 Caution on Disposal of Instrument .........
Page 21 UTLTY Setting ....................3-18 3.2.1 Zero Pressure Calibration ..............3-18 3.2.2 Pump Motor Control Setting ............. 3-19 3.2.3 Purging Flow Rate Setting ............... 3-20 3.2.4 Flow Rate Calibration Setting ............3-21 3.2.5 Pressure Calibration Setting ............3-22 3.2.6 Pressure Unit Setting ............... 3-23 3.2.7 Column Flush Setting ...............
Page 22 Troubleshooting ..................4-11 4.3.1 Error Messages and Proper Measures ..........4-11 4.3.2 Troubleshooting ................4-13 Maintenance ....................4-15 4.4.1 Fluctuation, Noise, and Drift of Baseline .......... 4-15 4.4.2 Abnormal Pressure ................4-16 4.4.3 Poor Sensitivity, Poor Separation, Poor Reproducibility ....4-17 General Cautions for Handling ..............
Page 23: Outline
1. OUTLINE The liquid chromatograph system consists of a pump for feeding a mobile phase, a sample introducing section (autosampler, manual injector) for injecting a sample, a column for chromatographic separation of the injected sample, a column oven for maintaining the column at a constant temperature, and a detector section for detecting a signal of a separated component of the sample.
Page 24: Low-Pressure Gradient System
A mobile phase is fed by the pump through the degassing unit. A sample is injected from the autosampler. The injected sample is separated through the column which is maintained at a constant temperature by the column oven. Each component separated from the sample is then detected as a signal by the detector.
Page 25 Each of plural mobile phase is fed from the degassing unit to the low-pressure unit. In the low-pressure unit, the mobile phase are mixed at a pre-specified ratio. Through the mixer, the mixture mobile phase is delivered. A sample is injected by the autosampler. The injected sample is separated through the column which is maintained at a constant temperature by the column oven.
Page 26: Functions
2. FUNCTIONS 2.1 Name and Function of Each Part on Pump Power switch UI pad (option) Right door Left door Fig. 2-1 Front Panel Pump head 1 Check valve Pump head 2 (Discharge side) Purge valve Flow path filter Pressure sensor Drain tray Leak sensor Check valve...
Page 27 Auto purge valve Pressure sensor Pump head 1 Flow path filter Check valve Port 1 (Flow path for the system Pump head 2 (Discharge side) Port (Flow path for waste fluid) Check valve Leak sensor Drain tray Plunger wash mechanism (Intake side) Fig.
Page 28 Power switch Turns power ON/OFF.. Front doors (R/L) : The pump has double doors. Drain Valve : This valve is opened for purging the system. Leak sensor : Detects fluid leakage. UI pad : A keypad to be used for stand-alone operations (option).
Page 29 Wiring covers EVENT (LIMIT OUT) PUMP ON IN PUMP OFF IN PRESS OUT An external signal An external signal ポンプは外部。 Pressure value is output to starts the pump. stops the pump. the exterior Ground terminals (Approx. 70 MPa)/1 V Fig. 2-4 Rear Panel Wiring covers : Upon detaching the left-side cover (as viewed from the front), the...
Page 30 Table 2-1 Name and Function of Each Terminal at Rear Panel Classi- Contents of Contents of Name Function Remarks fication Signal Processing  Timer  EVENT No. and Event code Output EVENT Contact turns The ON/OFF (1 to 4) on/off according signal can output to coded setting ON: CLOSE...
Page 31: Name And Function Of Each Part On Ui Pad (Option)
2.2 Name and Function of Each Part on UI Pad (Option) Where the chromatograph data station or the Chromaster GUI controller (option) is not used for controlling operations, each module can be operated using the UI pad. This section describes how to use the UI pad for operations. The UI pad is provided with common control keys available for different modules and unique control keys for particular modules.
Page 32 Table 2-2 Name and Function of Each Key Function Remarks PUMP Performs Start/Stop of Pump. Press to When the flow rate is set at ON/OFF start, and press again to stop. 0 mL/min, the operating condition is "Waiting". PURGE Performs Start/Stop of purging the flow NOTE: path.
Page 33 Function Remarks Used for program editing. INSERT Inserts a new row as last row of a program. PROG 1. Press this key once to return the △ program by one step. 2. Selects the Monitor display etc. 1. Press this key once to advance the program by one step.
Page 34 Function Remarks INITIAL Makes the operation status Program Mode. The operation status at this moment becomes initial status (the contents of 0 minute of the time program) of the specified program. 1. When inputting numerical values, if you The CL key has the alarm notice a mistake before pressing the sound stop function.
Page 35: Specifications
2.3 Specifications Liquid delivery system Dual plunger type reciprocating pump (Tandem Type) Series connection, pulsation elimination system Maximum operating pressure 60.0 MPa (0.001 – 2.500 mL/min) 30.0 MPa (2.501 – 5.000 mL/min) Flow rate range 0.001 to 5.000 mL/min Pressure display method Digital display (bar, Psi, kgf/ cm², MPa can be selected.) Pressure limit range 0 –...
Page 36 Display data using UI-Pad (option) Parameters Gradient monitor: Elapsed time, mixing ratio, flow rate, pressure, timer value, etc. (m) Pump control mode: Isocratic mode Low-pressure gradient mode Input/output terminals Event timer: 4 channels Zero adjustment for pressure Enable Wetted parts material SUS316, Ruby, Sapphire, Ceramics, PTFE.
Page 37 (w) Temperature 4 to 35 C (non condensing) Humidity 25 to 85% RH Option  Chromaster GUI controller  UI pad  Low gradient unit  Dynamic mixer  Semi micro mixer  Auto purge valve (when a pump with auto purge valve is selected) ...
Page 38: Operation
3. OPERATION The method of pump operation using the optional UI pad is described here. CAUTION Fatigue due to Long-Hour Operation If you keep working with the display monitor in the same posture for long hours, your eyes and body will be fatigued. When working with the display monitor for a long time, take a break for 10 to 15 minutes per hour for health of your eyes and body.
Page 39 (a) Startup screen PUMP 8928116-00 (C) Hitachi High-Technologies Corp. 2012 Initializing, self-testing, and indicating a copyright are performed. The program number and version will be confirmed on the startup screen. The first monitor screen will be indicated after initialize-processing is completed normally.
Page 40 Description of status indication at upper right of monitor screen: [GR] ..Gradient program is in execution. [IN] ..Fluid is delivering with the initial condition of the programming mode. [ -- ] ..A pump is suspended in the programming mode. [MN] ..Manual mode [PG] ..Purge is in execution.
Page 41 USE/No USE P.WASH Wash pump ON: Running, OFF: Suspended NOTE: For Chromaster 5160 Pump, an internal maximum operating pressure will be set up according to the flow rate setting. Pressure limit range: 0 to 2.500 mL/min .... 60.0 MPa, 2.501 to 5.000 mL/min ..30.0 MPa.
Page 42 (e) 4 Monitor Screen EVENT PUMP FLUSH [ -- ] OFF OFF OFF OFF Table 3-5 4 Monitor Screen Indication Description EVENT EVENT terminal 1 to 4 state. 1, 2, 3, 4 Contact is closed, OFF : Contact is OPEN When a contact becomes ON while a program link is in execution, even in the next step it will be in the ON state.
Page 43 Monitor Screen Changeover Monitor Screen TIME FLOW PRESS [ -- ] 0.000 ▽ △ Monitor Screen P-UNIT P.MAX P.MIN D.MIX P.WASH [ -- ] 20.0 △ ▽ ▽ Monitor Screen △ OPTION LOW GR. P.WASH A.VALVE D.MIX [ -- ] ▽...
Page 44: Parameter Setting
3.1.2 Parameter Setting Carry out setting of the parameter and program. Parameter setup screen (a) Single numeric Parameter name Input range SET PROGRAM NO. (1 – 9) Input field (b) Plural numeric Input Item Parameter name PUMP SEAL CHANGE YYYY) <...
Page 45 Numerical input (a) A cursor is indicated on the first character in the input field. Previous setup value is indicated in the input field. (b) Numerical and decimal (.) input are allowed up to the number of maximum character input. (c) Press the ENT key to register the input value, and move to the next item.
Page 46: Operational State
When the setting condition is cancelled: press the ESC key to return to the 1 monitor screen. And reset a condition. When the setting condition isn’t changed/entered: press the ENT key or the ▽ key to move to the next screen (Use ▽...
Page 47: On/Off Setting
3.1.4 ON/OFF Setting The pump On/Off operation is described below. PUMP ON/OFF Press the key to start. FLOW in LED display will be lit in blue. PUMP ON/OFF Re-press the key while the pump is running. The pump will be suspended. 3.1.5 Purging Operation Purge execution and stop operation are described here.
Page 48: Manual Operation
3.1.6 Manual Operation The operation is used for delivering liquid under the constant condition without using a program. Isocratic Mode As an example: flow rate at 1.0 ml/min, upper pressure limit at 20.0 MPa, and lower pressure limit at 0 MPa. Monitor screen MANUAL MANUAL:...
Page 49 Constant pressure mode As an example: flow rate at 1.0 ml/min, upper pressure limit at 20.0 MPa, and lower pressure limit at 0 MPa. Monitor screen MANUAL MANUAL: (FLOW=1, PRESS=2) Select constant pressure mode (PRESS) CONSTANT PRESS INITIAL FLOW PRESS 0.2 –...
Page 50: Programming Operation
3.1.7 Programming Operation Operation with a program for isocratic mode is explained here. As an example: upper pressure limit at 20.0 MPa, lower pressure limit at 0 MPa, and flow rate is1.0 ml/min at 0 minute of analysis time. Output pulse signals by Event 1 to 4. Change the flow rate to 0.5 ml/min by 10 minutes of analysis time.
Page 51 Monitor screen INITIAL Press the key to change the mode from manual set screen to the programming mode. INSERT Program generation is started PROG SET PROGRAM: No. ( 1 – 9 ) Select a program number from 1 to 9. EDIT MODE (MODIFY = 0, NEW = 1) Select EDIT MODE...
Page 52: Exit Operation
NOTE: A maximum of 100 steps can be entered for program No.1 to 9 (92 steps per program). NOTE: The entered program will be saved. When the power supply is turned on next time, the initial screen (TIME=0) used for the previous program will be displayed.
Page 53 Inlet tube Drain tube Joint Waste solution bottle (beaker) Syringe Fig. 3-3a Manual wash Set up a waste solution bottle (or beaker) under the drain tube. NOTE: Please be careful about a tube tip position. When the tube tip touches liquid level, a liquid lead can’t be detected.
Page 54 Injection valve Syringe valve Port4 Fig. 3-3b Connecting with the Chromaster 5260 Autosampler 3 - 17...
Page 55: Utlty Setting
3.2 UTLTY Setting 3.2.1 Zero Pressure Calibration The zero pressure point may change a little due to a secular change of the pressure sensor. Please check the zero pressure point once a month (Stop the pump, and then open the drain valve).
Page 56: Pump Motor Control Setting
3.2.2 Pump Motor Control Setting The automatic flow rate control system (STANDARD) and the fixed flow rate control system (FIX) are available as the pump motor control method. Monitor screen SET UP UTLTY UTLITY (CONDITION=1, UNIT=2, FLUSH=3 EVENT=4, LINK=5, P.WASH=6, OTHERS=7) Select CONDITION CONDITION SET (Z-ADJ=1,...
Page 57: Purging Flow Rate Setting
3.2.3 Purging Flow Rate Setting Set up a purging flow rate. Monitor screen SET UP UTLTY UTLITY (CONDITION=1, UNIT=2, FLUSH=3 EVENT=4, LINK=5, P.WASH=6, OTHERS=7) Select CONDITION CONDITION SET (Z-ADJ=1, MOTOR-CTRL=2 PURGE=3, CALIBRATION=4, LPGR=5) Select PURGE PURGE SET (MANUAL=1, A.PURGE=2) Select MANUAL PURGE FLOW (0.001 –...
Page 58: Flow Rate Calibration Setting
Pressing the purge key in the state of PUMP ON executes purging at the set flow rate. Re-pressing the purge key during purge will reset it. During purge, the upper pressure limit is set at 2.9 MPa and the lower pressure limit at 0 MPa. 3.2.4 Flow Rate Calibration Setting Set up a calibration coefficient for the flow rate.
Page 59: Pressure Calibration Setting
3.2.5 Pressure Calibration Setting Set up a calibration coefficient for the pressure. Monitor screen SET UP UTLTY UTLITY (CONDITION=1, UNIT=2, FLUSH=3 EVENT=4, LINK=5, P.WASH=6, OTHERS=7) Select CONDITION CONDITION SET (Z-ADJ=1, MOTOR-CTRL=2 PURGE=3, CALIBRATION=4, LPGR=5) Select CALIBRATION CALIBRATION (FLOW=1, PRESS=2) Select PRESS PRESSURE CALIB (0.900 –...
Page 60: Pressure Unit Setting
3.2.6 Pressure Unit Setting Select a pump pressure unit from bar, psi, kgf/cm , MPa. Monitor screen SET UP UTLTY UTLITY (CONDITION=1, UNIT=2, FLUSH=3 EVENT=4, LINK=5, P.WASH=6, OTHERS=7) Select UNIT PRESSURE UNIT (MPa=1, bar=2, psi=3, kgf/cm Select a unit Monitor screen The set pressure unit will be stored even if the power supply is turned on.
Page 61: Column Flush Setting
3.2.7 Column Flush Setting The pump automatic stop function and the column flushing function after the completion of analyses is set. By setting of the column flush, the flushing will start automatically at specified time after the analysis. When a salt solution is used for analysis, the column must be flushed with water to prevent elution of the salt component.
Page 62 Select PARAM COLUMN FLUSH FLOW 1.000 Enter column flash condition FLUSHING TIME (1.0 – 600.0) min 30.0 Enter column flash time from 1.0 to 600 min Monitor screen Select PROGRAM No.9 Monitor screen The execution of the column flush will start by program No.9. NOTE: The program of column flush is automatically fixed as No.9.
Page 63 Delay time and Column flush Delay time Column Flush Completion of the gradient AUTO PUMP OFF = YES (a) COLUMN FULSH = YES Analysis 1 Analysis 2 Analysis 3 Analysis n Delay time COLUMN FLUSH Stabilization time Pump stop *: “n” is the analysis number of times set up for the autosampler. (b) COLUMN FLUSH = NO Pump stop Analysis 1...
Page 64: Event Code Setting
3.2.8 Event Code Setting An event is carried out manually. The event function will start with input of an event code. Events are: starting of the external unit, stop of a pump, and buzzer. Additionally, an event will be output to EVENT No.4 when a pressure limiter error is detected.
Page 65 Table 3-8 Event code and behavior Item Event code Remarks Timer digit: Timer No. digit: Behavior class Behavior Start point *Contact point for one Contact point OPEN OPEN sec. CLOSE Contact point CLOSE Signal Close marker Signal ON Start point Pump Pump has stopped Buzzer...
Page 66: Link Program Function
3.2.9 Link Program Function Plural programs can be linked. NOTE: When connecting with CDS, setting should be set to NO. In this case, setting will be made on the system manager side. Setting of Link Program Set the conditions for link program. Explained below is an example where you set one run of program No.
Page 67 STEPS PROG-NO. CYCLE CONDITION TIME Input program No. (PROG-No.), repetitive cycles (CYCLE) and conditioning time (COND. TIME). STEPS PROG-NO. CYCLE CONDITION TIME The conditions for 2nd step are settable here. Input program No. (PROG-No.), repetitive cycles (CYCLE) and conditioning time (COND. TIME).
Page 68 Actions in Link Program In a link program, two or more programs are used in succession. Explanation is given in case a link program is set under the following conditions. (a) Programs PROGRAM No. = 1 PRESSURE VALUE : MAX 19.6 TIME CONCENTRATION...
Page 69 (b) Column flushing conditions (Refer to 3.2.7 for column flush setting). DELAY TIME 10.0 COLUMN FLUSH = FLOW = 6.00 mL/min TIME 10.0 (c) Link program conditions STEP PROG-No. CYCLE COND.TIME(min) 10.0 10.0 (i) Upon start after gradient elution Screen transition in the above example is explained. The encircled numerals in this execution example correspond to the step numbers of screen display.
Page 70 ① Initial %A %B %C %D FLOW PRESS ［IN］ TIME 1.000 Liquid is delivered in the initial status (initial condition of program No. 1 in this example). ② Gradient %A %B %C %D FLOW PRESS ［GR］ TIME 10.0 1.000 Gradient elution is carried out (program No. 1 is executed in this example).
Page 71 ⑦ Delay time (initial) %A %B %C %D FLOW PRESS ［IN］ TIME 1.000 Liquid is delivered in the initial status of the first step (initial condition of program No. 1 in this example). When “start” is not input during the delay time, column flushing in ⑧ will begin.
Page 72 ① Initial %A %B %C %D FLOW PRESS ［IN］ TIME 1.000 Liquid is delivered in the initial status (initial condition of program No. 1 in this example). ② Gradient %A %B %C %D FLOW PRESS ［GR］ TIME 10.0 1.000 Gradient elution is carried out (program No. 1 is executed in this example).
Page 73 (iii) Upon STOP during gradient elution ① Initial TIME %A %B %C %D FLOW PRESS ［IN］ 1.000 Liquid is delivered in the initial status (initial condition of program No. 1 in this example). ② Gradient %A %B %C %D FLOW PRESS ［GR］ TIME 10.0 1.000...
Page 74 ⑤ Conditioning time %A %B %C %D FLOW PRESS ［LC］ TIME 1.000 During the conditioning time, liquid is delivered under the initial condition of execution step (program No. 2 in this example). ⑥ Initial %A %B %C %D FLOW PRESS ［IN］ TIME 1.000 Liquid is delivered in the initial status (initial condition of...
Page 75: Plunger Wash Pump Setting
3.2.10 Plunger Wash Pump Setting The plunger wash pump (option) is set. This operation is enabled only when the plunger wash pump is connected. Monitor screen SET UP UTLTY UTLITY (CONDITION=1, UNIT=2, FLUSH=3 EVENT=4, LINK=5, P.WASH=6, OTHERS=7) Select P.WASH WASH TIME (0 –...
Page 76: Leak Sensor Setting
3.2.12 Leak Sensor Setting Enable or disable the leak sensor. Monitor screen SET UP UTLTY UTLITY (CONDITION=1, UNIT=2, FLUSH=3 EVENT=4, LINK=5, P.WASH=6, OTHERS=7) Select OTHERS OTHERS (ERROR OUT=1, LEAK SENSOR=2 Select LEAK SENSOR LEAK SENSOR (OFF=0, ON=1) 0=The leak sensor is disabled 1=The leak sensor is enabled Monitor screen NOTE: ON=1 is default setting.
Page 77: Glp
3.3 GLP The logbook (a pump seal, an optional part, etc.) are displayed and reset. Additionally, a keylock is set up to prevent incorrect input during an analysis. 3.3.1 Pump Seal Logbook The total volume of the delivery liquid after replace of a pump seal is indicated.
Page 78: Plunger Wash Pump Logbook
3.3.2 Plunger Wash Pump Logbook The total running time after replacement of a plunger wash pump (option) is indicated. This function is enabled only when the plunger wash pump is connected. This function is used as an index of a replacement for plunger wash pump. Monitor screen (LOGBOOK=1, PRESSURE M=2,...
Page 79: Auto Purge Valve Logbook
3.3.3 Auto Purge Valve Logbook The total number of times of the changeover after replace of a maintenance part for an auto purge valve (option) is indicated. This function is enabled only when the auto purge valve is connected. This function is used as an index of a replacement for maintenance parts of the auto purge valve.
Page 80: Dynamic Mixer Logbook
3.3.4 Dynamic Mixer Logbook The total running time after replacement of a maintenance part for a dynamic mixer (option) is indicated. This function is enabled only when the dynamic mixer is connected. This function is used as an index of a replacement for maintenance parts of the dynamic mixer.
Page 81: Low Gradient Unit Logbook
3.3.5 Low Gradient Unit Logbook The total number of times of the changeover after replace of a proportioning valve for a low gradient unit (option) is indicated. This function is enabled only when the low gradient unit is connected. This function is used as an index of a replacement for maintenance parts of the low gradient unit.
Page 82 Select RESET REPSET (A=1, B=2, C=3, D=4) Select a proportioning valve P.VALVE CHANGE YYYY) <2000 – 2100> 2010 Reset logbook Monitor screen NOTE: Enter the maintenance part for the dynamic mixer replacing date. Enter Month, Date, Year. And press ENT. In other words, it can’t be reset without pressing the ENT key.
Page 83: Pressure Monitor
3.3.6 Pressure Monitor The total number of times of the double speed section error is indicated. The double-speed section error indicates that the pressure fails to return to the reference level (previous pressure) even after double-speed control (an increase of pump motor speed) was effected to compensate for decreased pressure.
Page 84: Key Lock
3.3.7 Key Lock This function serves to lock the keys on the keyboard, and thus prevent erroneous activation of keys on the control panel. NOTE: The UI pad operation will be disabled when the Chromaster GUI controller and CDS are connected. Monitor screen (LOGBOOK=1, PRESSURE M=2,...
Page 85: Analysis Operation
3.4 Analysis Operation WARNING Ignition of Flammable Chemicals This instrument is not explosion-proof. In unattended operation, do not use organic solvents having a flash point below 70 C. Be aware of ignition hazard when using flammable chemicals such as organic solvents. a) Do not bring a heat or flame source near the instrument.
Page 86 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 87: Operation Procedure
3.4.1 Operation Procedure When the settings are all finished, carry out operation in the following procedure. Make sure the pump, column, detector and data processor are properly connected. Set the mobile phase and waste solution bottle in place. Start the pump and wait until the flow path is filled with the mobile phase.
Page 88 PROG No.=1 PRESSURE MAIN (MPa) 20.0 TIME FLOW EVENT 1.000 10.0 1.000 11 21 31 41 10.1 1.000 20.0 1.000 25.0 10 20 30 40 30.0 2.000 30.1 1.000 40.0 1.000 00 92 Fig. 3-4 Example of Program (a) For EVENT, up to 4 event codes are settable at each time point.
Page 89 New Generation of a Program This section shows the generation of a new program. PROG (SET PROG No.) No. of program to be generated (m) (MODIFY=0, NEW=1) (MAX) Upper limit pressure (MIN) Lower limit pressure level level (TIME) Set time (Ti) (FLOW) Set flow rate (Fi) (EVENT)
Page 90 Program number can be from 1 to 9. When you want to define a new program, enter 1. As a result, you will delete the previous program. For modifying the contents of program, enter 0. If pump pressure rises beyond the level set here, the pump automatically stops.
Page 91 Deletion of Program How to delete a program is shown next. PROG (SET PROG No.) No. of program to be deleted (m) (MODIFY=0, NEW=1) Program number can be from 1 to 9. Input 1 to generate a new program. The contents of the existing program will be deleted.
Page 92 Deletion of Step How to delete one step in a program is shown next. PROG (SET PROG No.) No. of program containing step to be (MODIFY=0, NEW=1) deleted (m) (MAX) Upper limit pressure (MIN) level Lower limit pressure level Program number can be from 1 to 9. For editing, input 0.
Page 93 Addition of Step PROG (SET PROG No.) No. of program for adding a step (m) (MODIFY=0, NEW=1) (MAX) Upper limit pressure (MIN) Lower limit pressure level level (TIME) Time point of step added (Ti) (FLOW) Set flow rate (Fi) (EVENT) Event code (E1i) Event code (E2i) Event code (E3i)
Page 94 Program number can be from 1 to 9. For editing, input 0. For generating a new program, input If pump pressure rises beyond the level set here, the pump automatically stops. Values that can be inputted are 0.1 to 60.0 MPa. If pump pressure falls below the level set here, the pump automatically stops.
Page 95 Correction of Step Step correction method is explained here. PROG (SET PROG No.) No. of program containing step to be corrected (m) (MODIFY=0, NEW=1) (MAX) Upper limit pressure (MIN) Lower limit pressure level level (TIME) Time point of step added (Ti) (FLOW) Set flow rate (Fi) (EVENT)
Page 96 Program number can be from 1 to 9. For correction, input 0. For generating a new program, input 1. If pump pressure rises beyond the level set here, the pump automatically stops. Values that can be inputted are 0.1 to 60.0 MPa. If pump pressure falls below the level set here, the pump automatically stops.
Page 97 Deletion of Parameter The parameter deletion method is shown next. PROG (SET PROG No.) No. of program containing parameter to be deleted (m) (MODIFY=0, NEW=1) (MAX) Upper limit pressure (MIN) Lower limit pressure level level Program number can be from 1 to 9. For correction, input 0.
Page 98: Setup
3.5 Setup 3.5.1 Pump Mode Setting This section shows how to set the pump in the single-liquid delivery mode (FLOW mode). NOTE: Once this setting is made, it is memorized and need not be made each time. SET UP POWER ON UTLTY Press the POWER and SET UP UTLTY keys simultaneously.
Page 99 SETUP: PUMP MODE CONTRAST S.NO FLOW 02AB-111 POWER OFF Turn off the power supply once. POWER ON Turn on the power supply again. Self-diagnosis is performed. TIME FLOW PRESS [--] 0.00 A monitor screen of the isocratic mode will be indicated. 3 - 62...
Page 100: Lcd Contrast Setting
3.5.2 LCD Contrast Setting For LCD contrast setting on the UI pad, take the procedure shown below. SET UP POWER ON UTLTY Press the POWER and SET UP UTLTY keys simultaneously. LCD contrast setting screen will be displayed. Continue pressing SET UP UTLTY until the setting screen appears. SETUP: PUMP MODE...
Page 101: Before Performing Analysis
3.6 Before Performing Analysis This chapter describes the basic items to be careful about before starting analysis. WARNING Ignition of Flammable Chemicals This instrument is not explosion-proof. In unattended operation, do not use organic solvents having a flash point below 70 C. Be aware of ignition hazard when using flammable chemicals such as organic solvents.
Page 102 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 103: Selection Of Mobile Phase And Cautions On Handling
3.6.1 Selection of Mobile Phase and Cautions on Handling Be careful about restriction on use due to characteristics and temperature of mobile phase to be used. (See Table 3-10 Characteristics of Organic Solvents) When performing high sensitivity analysis with a UV detector, use solvents whose UV absorption characteristics are especially small.
Page 104 NOTE: When unsuitable reagents absolutely necessary for ingredient separation or reaction of a constituent have been used, or when mobile phase which deposits salt has been used, wash all the flow paths with distilled water after completing analysis without fail. If not, the plunger may wear down.
Page 105 Chemical resistance of the auto purge valve Ⓡ Vespel is used for the parts in drive system of the auto Ⓡ purge valve for the Chromaster 5160 pump. Vespel resin is weak against over pH10 over or more, so avoid using those. 3 - 68...
Page 106: Characteristics Of Organic Solvents
3.6.2 Characteristics of Organic Solvents Characteristics of organic solvents as mobile phase for liquid chromatograph are shown in Table 3-10. Use it for reference. WARNING Ignition of Flammable Chemicals This instrument is not explosion-proof. In unattended operation, do not use organic solvents having a flash point below 70 C.
Page 107 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 108 WARNING Explosion of Vapor from Flammable Chemicals If a flammable chemical such as organic solvent leaks from the flow path of the instrument and its vapor concentration exceeds the explosion limit, it may cause spontaneous combustion with dangerously explosive results. When using a flammable and readily volatile chemical, be sure to check for leakage from the instrument flow path and ventilate the laboratory room adequately.
Page 109 Table 3-10 Characteristics of Organic Solvents Polarity Viscosity Refractive UV cut Flash Ignition point Vapor Boiling Specific (cP20  C)  C index off (nm) point density point gravity Lower Upper (  C) (  C) (Air: 1) (Water: 1) limit limit Fluoroalkanes...
Page 110 NOTE: For Using Organic Solvents as Mobile Phase When using organic solvents, be careful about UV cut off wavelength. UV cut off wavelength: Light cannot be transmitted in the range shorter than this wavelength. For example: Cut off wavelength of chloroform is 245 nm. Chloroform cannot be used in the range shorter than 245 nm (e.g.
Page 111: Cautions On Static Electricity
3.6.3 Cautions on Static Electricity WARNING Ignition of Flammable Chemicals by Static Electricity 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 Since flammable organic solvents are used for the High Speed Liquid Chromatograph, be careful about heat and fire.
Page 112: Preparation
3.7 Preparation NOTE: Refer to the instruction manuals for usage of Ultrasonic Cleaner etc. 3.7.1 Degassing and Removing Dust from Mobile Phase Degas mobile phase before use without fail. Oxygen gas and nitrogen gas contained in mobile phase cause the following when used under high pressure. (a) Change in quality of mobile phase sample (b) Loss of column efficiency caused by bubbles (c) Noise of detector caused by bubbles...
Page 113 Remove cap Mobile phase container Ultrasonic cleaner Fig. 3-8 Degassing Mobile Phase by the Ultrasonic Cleaner (a) Set mobile phase container well stirred into ultrasonic cleaner. * When using a mixed mobile phase, stir it completely by using a stirrer, or else low repeatability or baseline drift may be caused.
Page 114 Devices to be prepared Ultrasonic cleaner (Put water in the bath without fail.) (ii) Aspirator with rubber stopper which fits the mouth of mobile phase container Rubber stopper should fit the mouth of container. Ultrasonic cleaner Mobile phase container Aspirator Fig.
Page 115: Removing Dust From Mobile Phase
When bubble generation finishes, remove rubber tube of aspirator from the reagent bottle. (g) Shut off the city water. (h) Turn off the power of ultrasonic cleaner. Take mobile phase container out of ultrasonic cleaner, wipe the water from the container, and set it to liquid chromatograph.
Page 116: Sample Pretreatment
3.7.4 Sample Pretreatment Filter samples without fail if they may contain fine dust. Dust can clog column and deteriorate it. Remove foreign matter from samples without fail. Foreign matter can lower the reliability of data, e.g. generating abnormal peaks etc. (a) Example of Filtering Samples Dust in sample can be removed easily as follows.
Page 117: Maintenance & Inspection
4. MAINTENANCE & INSPECTION NOTE: Make sure to request our authorized service agent for repair of the instrument in case it breaks down. Repair by anyone who has not received technical training by us is prohibited since it could be hazardous. 4.1 Performance and Specifications Check Performance checking method is explained here.
Page 118: Preparing The System For Operation
4.1.2 Preparing the System for Operation Fig. 4-1 shows how to connect the units for performance check. According to this figure, carry out tubing. Before energizing the system, ensure that the tubing between the autosampler and pump/detector is properly connected. Detector Load resistance coil Autosampler...
Page 119 Prepare other units to be connected to the autosampler as described in the respective instruction manuals. Put the drain tube from the detector into the exclusive detector waste solution bottle. If this tube is put into other waste solution bottle such as for the Chromaster 5260 autosampler, baseline fluctuation may be caused due to unstable back pressure.
Page 120 (10) Input the following contents as instrument conditions of autosampler. RACK CODE SYRINGE SPEED RACK PARAM : RACK CODE = 1 X1 = 57.1 X2 = 178.6 Nx = 10 Y1 = 0.0 Y2 = 148.5 Ny = 12 Z = 48 P = 5 INJ.METHOD : CUT...
Page 121: Flow Rate Precision Check
4.1.3 Flow Rate Precision Check Check the precision of flow rate in the following procedure. Set the following conditions to autosampler. STEP RACK VIALS VOL (uL) TIME 1- 1 10.0 Press the ESC key to complete setting. Prepare methanol for the mobile phase and detergent. Wait until the pump, detector, etc.
Page 122 Data Check Determine the coefficient of variation (RSD) of peak retention time by the following calculations.   Mean value     Standard deviation   Relative standard deviation   100(%) Retention time due to each injection Number of injections Make sure the RSD value is 0.075% or less.
Page 123: Periodic Maintenance
4.2 Periodic Maintenance 4.2.1 Liquid Leak Sensor Check The Chromaster 5160 pump is equipped with a liquid leak sensor for detecting liquid leakage. Note, however, that liquid leakage may not be detected correctly due to sensitivity of the leak sensor. To prevent this, perform periodic operation check for the liquid leak sensor as instructed below.
Page 124 Cleaning Preparation: Hexagon wrench (Accessory, P/N: N315003, Size: B2.5) (a) Remove fixation screws of the liquid leak sensor with a hexagon wrench, and detach the liquid leak sensor from a drain tray. (b) Wipe up water on the liquid leak sensor and the drain tray.
Page 125: Periodical Inspection
4.2.2 Periodical Inspection Perform periodic maintenance and inspection according to Table 4-1. This prevents problems and ensures that your system meets specifications. Table 4-1 Periodical Maintenance and Inspection Check Item Procedure Remarks Drain tray Check the drain tray for any Contamination or dirt in the drain contamination or dirt to be cleaned tray causes the leak sensor errors.
Page 126 Check Item Procedure Remarks Wash Check the amount and generated air Depends on the state of the wash mechanism bubbles of wash fluid in the wash fluid, it causes deterioration of the mechanism every day. pump seal and the plunger. Leaks lead to poor baseline stability and data reproducibility.
Page 127 OFF the power switch and disconnect the power cord from the receptacle. If an abnormality occurs on the Model Chromaster 5160 pump, an error message appears on the LCD (Liquid Crystal Display). Error displays result from either the...
Page 128 LCD. Use the CL key to erase the error messages. Unless the cause of an error is eliminated, the same error message will display again. For units other than the Model Chromaster 5160, check the corresponding instruction manuals. Table 4-2...
Page 129 30 MPa for 2.501 to 5.000 mL/min. 4.3.2 Troubleshooting Table 4-3 offers a guideline for the troubleshooting of the pump. Refer to this table first, if a problem occurs. Table 4-3 The Chromaster 5160 Pump Troubleshooting Symptom Cause Measure Even if the PROG key is The program mode is not displayed.
Page 130 Symptom Cause Measure Liquid doesn’t flow. 1) Looseness of the piping joint. Tighten the joint manually. 2) Clogging of the solvent filter. Wash the solvent filter. 3) Negative pressure depending on Place the solvent bottle in the position of the solvent bottle. the same height as the instrument.
Page 131 4.4 Maintenance 4.4.1 Fluctuation, Noise, and Drift of Baseline Symptom Check position Possible cause Check Result Remedy Turn off the power and wait for 10 minutes. Turn on the power. If Peak or Replace the D lamp. Fluctuation, Noise of Baseline Noise level is high as shown in the symptom figures, the life of the lamp is Replace the W lamp.
Page 132 4.4.2 Abnormal Pressure Symptom Check position Possible cause Check Result Remedy Replace the column. Clogged Column Filter. Remove the Column, and pump the liquid. Column or Clogging caused by Has the pressure become close to zero? contamination of Fillers. Replace the filter. (See 5.5.) Remove the filter, and clean it with an ultrasonic cleaner.
Page 133 4.4.3 Poor Sensitivity, Poor Separation, Poor Reproducibility Symptom Check position Possible cause Check Result Remedy Tighten. Poor sensitivity Connection piping Check leak visually. Any Leakage? Tighten. Replace Injection port seal. Leak from (See the instruction manual for Autosampelr.) Check leak visually. Injection port Replace the Valve seal.
Page 134 4.5 General Cautions for Handling (1) Replacement of Solvent, Cleaning Of Flow Path System When replace the solvent for the inside of the flow path system, use solvents that can be mixed with each other. (Also substitute the solvent for the inside of the detector cell and the flow path of the sample injector.) Perform cleaning similarly.
Page 135 (Outlet) Stopcock 0.2 ml/min. (Inlet) Pump (0.02 ml/min.) Fig. 4-6 Column Storage Solvent Selection (a) Select a wavelength for measurement considering absorption characteristics (wavelength) of the solvent that is a wavelength with less absorption. Use a solvent for high speed liquid chromatography if possible.
Page 136 Cleaning Microsyringe (a) Wipe the needle before and after sampling. (b) Wipe the needle before aspirating a cleaning solvent. Clean the inside of the syringe seven times or more. (c) Clean the syringe after injection immediately. Fig. 4-8 Cleaning Microsyringe Tightening Connection Tube If a Teflon tube is tightened too much, the inside diameter becomes short, and the pressure increases abnormally.
Page 137 SUS ferrule SUS pipe SUS push crew Fig. 4-9 Tightening Connection Tube Handling Detector If the detector is not used for a long time, clean the detector, then short the inlet and the outlet to seal the liquid so that the inside of the detector will not dry.
Page 138 5.1 Pump Main Unit Normal Part No. Name Shape and Specifications Position Used Life 891-1213 Plunger seal Pump head for 640 h Chromaster 5160 (Pump seal) (4 months) Color: Black 885-1884 Wash Wash mechanism 640 h mechanism seal plunger guide (4 month)
Page 139 Normal Part No. Name Shape and Specifications Position Used Life 810-1031 Flow path filter 1920 h Pressure sensor Filter holder 638-1423 (1 year) Packing 638-1422 893-0800 Check valve (IN) Pump head 1 – 3 year If check valve doesn't work properly, clean. If this doesn't solve the problem, replace the valve.
Page 140 Normal Part No. Name Shape and Specifications Position Used Life 893-0902 Auto purge valve Auto purge valve 40000 rotor seal times (Option) Ⓡ Vespel 5.2 Flow Path Tubing Parts Part No. Name Shape and Specifications Position Used L329235 SUS push screw (M6) 1/16 inch (1.57 mm) OD SUS pipe 655-1458...
Page 141 Part No. Name Shape and Specifications Position Used L369053 PCTFE ferrule 1/16 1/16 inch OD (1.57 mm inch PTFE tube 0.33 mm ID  1.57 mm OD  10 m F275144 PTFE tube Example of use: Outlet tube for detectors 0.5 mm ID ...
Page 142 5.3 Replacement of Pump Seal <Required articles> Pump seal (P/N: 891-1213x 2) Hexagon wrench (P/N: N315005, Size: B4) Workshop tools (P/N: 810-1353) Receiving tray Remover N (P/N: 893-1372) Wash bottle Gauze or soft cloth Ultrasonic cleaner Disconnect the inlet tube and outlet pipes (1)(2) from the pump heads using a 1/4 inch double-end wrench of workshop tools.
Page 143 Carefully pull out the plunger wash mechanism toward you. NOTE: Do not remove the seal in the plunger wash mechanism guide. Take out the pump seal. When the pump seal remains in the pump head, pull out the pump seal by screwing the exclusive seal-removing rod into it.
Page 144 Install the new pump seal on the pump head. Place the pump seal in the center-hollow of the pump head. Insert the plunger wash mechanism into the pump head while paying attention for the direction of the flow path. Give the pump seal a final push with a finger to correctly sit the seal in the pump head.
Page 145 Guide Pump head Spring washer Hexagon screws Plunger wash mechanism (11) Install the stainless steel pipe on the pump head. Use a 1/4 inch double-end wrench. (12) Open the drain valve. Turn on the pump. And eliminate air bubbles from the flow path to the drain valve. Then, fill it with the mobile phase.
Page 146 Packing(Purge valve seal (P/N: 885-2920) Seal remover PV NOTE: Recap after use the seal remover PV. Keep the seal remover PV in an accessory box of Chromaster 5160 Pump. Loosen the purge valve knob (in "Open" direction) and pull it out.
Page 147 5.5 Washing of the Flow Path Filter <Required articles> Workshop tools (P/N: 810-1353) Wash bottle Ultrasonic cleaner Receiving tray Beaker When replacement is required: Packing (PEEK)(P/N: 891-1228 for flow path filters) Filter (P/N: 638-1423) Seal (P/N: 638-1422 for filters) Using the wrench 21, loosen and remove the flow path filter from the drain valve.
Page 148 If a clogged filter has to be replaced, allow the filter has to be replaced, allow the filter assembly to dry, then place it in a freezer (-10℃) for about five minutes. The cold ® temperature will contract the Teflon packing and facilitate removal of the filter.
Page 149 Purge valve Inlet tube Sample bottle Fig. 5-1 Front Face of Chromaster 5160 Pump Loosen the cap of the mobile phase bottle. Pull out the inlet tube from the mobile phase bottle. Remove the solvent filter from the inlet tube.
Page 150 Prepare the wash fluid in a beaker, and place the filter in it. Place the beaker in the ultrasonic bath. Run the ultrasonic cleaner for 5 to 6 minutes. Solvent filter Beaker Wash fluid ↓ Distilled water Ultrasonic cleaner Replace the wash fluid with distilled water. Run the ultrasonic cleaner for an additional 5 to 6 minutes.
Page 151 5.7 Washing of the Check Valve (suction and discharge side) Open the purge valve. Use isopropanol as the wash fluid. Flow the isopropanol for 3 to 5 minutes at a maximum flow rate of 9.999 mL/min, or you may also use the purge function. If this procedure proves ineffective, take out and wash the valve following the procedure.
Page 152 Fill the beaker with the wash fluid (neutral detergent). Immerse the entire valve holder assembly into the beaker. Fill the ultrasonic cleaner with water. Put the beaker containing the valve holder assembly in it and perform washing for about 10 minutes. Valve holder assembly Beaker Ultrasonic cleaner...
Page 153 Attach the check valve (suction and discharge valve) to the Pump head. Turn the head about 375 degrees with the wrench 10. To prevent biting, apply distilled water to the whole male thread of the valve when tightening. Check valve (Discharge side) Check valve (Suction side)
Page 154 5.8 Parts Replacement for the Check Valve (suction and discharge side) After long use, the packings in the discharge valve and the suction valve may be damaged and cause leaks. If the leaks persist after retightening with a wrench, you must replace the packing.
Page 155 Suction Discharge Valve Valve Valve Valve holder holder Packing (A) Packing (A) Check valve Check valve Packing (A) Packing (A) Check valve Check valve Packing (B) Packing (B) Beaker Beaker Beaker Beaker Beaker Beaker Fill the ultrasonic cleaner bath with water. Put the beakers in the ultrasonic cleaner bath and perform ultrasonic washing for 5 to 6 minutes.
Page 156 Sufficiently dry the valve holder and packings. Direction of liquid flow Glossy side (Top) Valve chest Ball Valve seat Filter paper (6) Mount the assembled check valves into the valve holder in the order shown in the illustration. Direction of liquid flow Direction of liquid flow Packing B 891-1364...
Page 157 5.9 Parts Replacement for the Plunger Wash Mechanism <Required Articles> Hexagon wrench (P/N: N315005, Size: B4) Workshop tools (P/N: 810-1353) Double-end wrench (P/N: N311017, Size: 13/17) Flathead screwdriver (P/N: N330062) Receiving tray Wash mechanism seal (P/N: 885-1884x 2) Plunger seal(Pump seal)(P/N; 891-1213x 2) *Replace it as necessary.
Page 158 Remove the wash mechanism seal in the wash mechanism plunger guide. Remove the plunger wash mechanism guide from the plunger while rotating it to the left and right gently. Loosen a seal holder with the flathead screwdriver while holding the bearing of the wash mechanism plunger guide with wrench17, and then remove it.
Page 159 Install the new wash mechanism seal in the bearing of the wash mechanism plunger guide. Wash mechanism seal Bearing (10) Tighten the seal holder with the wrench and the flathead screwdriver. Seal holder Flathead screwdriver Bearing Wrench17 (11) Install the plunger wash mechanism and the pump head on the main body of the pump.
Page 160 Guide Pump head Spring washer Hexagon screws Plunger wash mechanism (14) Install the stainless steel pipe on the pump head. Use a 1/4-inch double-end wrench. (15) Open the drain valve. Turn on the pump. And eliminate air bubbles from the flow path to the drain valve. Then, fill it with the mobile phase.
Page 161 5.10 Parts Replacement for the Auto Purge Valve After long use, the packings in the discharge valve and the suction valve may be damaged and cause leaks. If the leaks persist after retightening with a wrench, you must replace the packing.
Page 162 Put seal guide pins into holes of the auto purge valve seal, and install a new auto purge valve seal. NOTE: Avoid touching the rotor seal and the stator directly with your hands. It may influence the result of analysis. Auto purge valve main unit NEW auto purge valve rotor seal NEW auto purge valve stator...
Page 163 INDEX Check valve ........................5 - 2 CL ........................... 2 - 9 Contact point ......................... 3 - 28 DEL ..........................2 - 8 Degassing ........................3 - 75 Drain tray ........................2 - 1 e-Line connector ................... APPENDIX 2 - 1 ENT ..........................
Page 164 Key lock ........................3 - 47 Leak sensor ......................2 - 1, 3 - 39 LED ..........................2 - 3 Logbook ........................3 - 40 Low pressure gradient............. APPENDIX 1 - 9, APPENDIX 3 - 1, Maintenance & Inspection ....................4 - 1 Mobile phase ....................
Page 165 UI Pad ..........................2 - 6 UTLTY ......................... 2 - 7, 3 - 18 Wiring covers ..................2 - 4, APPENDIX 1 - 19 Zero pressure calibration ....................3 - 18 INDEX - 3...
Page 166 APPENDIX 1. INSTALLATION CAUTION Caution in Carrying Heavy Instrument Chromaster 5160 pump weighs as much as 16 kg. Be careful not to drop it and to handle it with care when carrying it, for preventing injury. Hold the right and left parts of the instrument firmly.
Page 167 2. Place for Installation For installation of the instrument, select a place which meets the following conditions. Operating temperature: Within 4 to 35 C and with minimum temperature variation during measurement. Utmost care should be used for preventing condensation. Operating humidity: 25 to 85% Atmospheric gas (a) Adequate ventilation is required.
Page 168 Shall be free from excessive dust. Otherwise, performance degradation might be caused. (g) Shall be free from a sudden change of power supply voltage. Otherwise, noise might be caused. (h) Power supply to motor-driven equipment (such as stirrer and vibrator) without a noise suppressor shall not be turned ON/OFF frequently on the same power supply line as that of this instrument.
Page 169 WARNING Electric shock due to improper grounding! This instrument is designed to meet the basic insulation stipulated in the international standard IE C61010-1. To prevent an electric shock hazard due to improper grounding, provide a proper grounding connection. Be sure to use the grounded 3P power cable, which is supplied as a standard accessory for the instrument.
Page 170 (a) Usual Grounding Connection (with grounded 3P power outlet) Grounded 3P power outlet (15 A) Grounded 3P table tap Chromaster 5110/5160 pump Ground resistance 750 mm or 100  or less more below Organizer or ground AC adapter (option) Connector Rear panel Grounding electrode (underground section)
Page 171 (b) Connection when Grounded Power Outlet is Unavailable 2P power outlet (15 A) 3P table tap with grounding wire Chromaster Grounding 5110/5160 pump terminal 750 mm or Organizer or more below Ground AC adapter (option) ground resistance Connector 100  or less Grounding wire (green) Screw diameter : M4 or larger...
Page 172 3.2 Installation Space For composing a liquid chromatograph system with the Chromaster series module units, a space of 540 mm wide (980 mm for stacking the units in two blocks) and 550 mm deep is required at least. Behind each unit, a space of 150 mm or more must be secured.
Page 173 5. Assembling NOTE: It is not permitted for the user to carry out installation at the time of delivery. For ensuring safety and high accuracy in operation of the instrument, installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its authorized service agent.
Page 174 Isocratic System/Low-pressure Gradient System (stacked in one block) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5310 column oven Chromaster 5210/5260 autosampler Interface control board Chromaster 5110/5160 pump To AC power supply Appended Fig. 1-4 Power Cable Connection Diagram Appended Table 1-1 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer) Connector cable 2)
Page 175 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5440 fluorescence detector To AC power supply Chromaster 5310 column oven Chromaster 5210/5260 autosampler Chromaster Interface control 5110/5160 board pump Appended Fig. 1-5 Power Cable Connection Diagram Appended Table 1-2 Cables to be Used Connector cable 1)
Page 176 5.2 System Cabling In the Chromaster series, the module units are cabled by plugging the e-Line cable into the e-Line connector at the rear left of each unit. e-Line connector Rear panel of module unit Power connector Isocratic System/Low-pressure Gradient System Chromaster organizer e-Line cable 1)
Page 177 Isocratic System/Low-pressure Gradient System (stacked in two blocks) e-Line cable 1) Chromaster 5410/ 5420/5430 detector e-Line cable 2) Chromaster 5440 fluorescence detector Chromaster 5310 column oven Chromaster organizer Chromaster 5210/5260 autosampler Chromaster 5110/5160 pump Interface control board Appended Fig. 1-7 e-Line Cable Connection Appended Table 1-4 Cables to be Used e-Line cable 1) (50 cm)
Page 178 5.3 System Tubing In the Chromaster series, the inlet tube up to the pump is fastened to the right/left side face of each unit with tube clamps. And the tubes are connected from the pump to the autosampler, column and detector through the central hole of the drain tray. Drain receiver Isocratic System Detergent...
Page 179 Chromaster 5440 fluorescence detector Detector cell Mobile- phase Chromaster 5310 liquid Detergent column oven Column Chromaster Injection valve organizer Chromaster 5210/5260 autosampler Chromaster 5110/5160 pump Wash pump Degassing unit Drain Appended Fig. 1-9 Tubing Diagram of Isocratic System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to the IN port of degassing unit.
Page 180 Low-pressure Gradient System Detergent Mobile-phase liquid Chromaster organizer Chromaster 5410/5420/ 5430 detector Chromaster 5310 Injection valve column oven Syringe valve Chromaster 5210/5260 autosampler Wash pump Low-pressure gradient unit/ proportioning valve Chromaster 5110/5160 pump Degassing unit Drain Appended Fig. 1-10 Tubing Diagram of Low-Pressure Gradient System (stacked in one block) APPENDIX 1 - 15...
Page 181 Chromaster 5440 fluorescence detector Detector cell Mobile-phase liquid Detergent Chromaster 5310 column oven Mixer Column Chromaster Injection valve organizer Chromaster 5210/5260 autosampler Chromaster 5110/5160 pump Wash pump 4-way joint Degassing unit Proportioning Drain valve Appended Fig. 1-11 Tubing Diagram of Low-Pressure Gradient System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to...
Page 182 Drain Tubing Drain tube A1 Chromaster organizer Chromaster 5410/5420/ T-joint 5430/5450 detector Chromaster 5310 column oven Drain tube A2 Chromaster 5210/5260 autosampler Drain tube 4 Chromaster 5110/5160 T-joint N1 pump Drain tube B1 Drain tube L-joint Appended Fig. 1-12 Tubing Diagram for Drain (when stacking module units in one block) Appended Table 1-5 Drain Tubes to be Used Drain tube A2...
Page 183 Chromaster 5440 fluorescence detector T-joint Drain tube A1*3 Chromaster Chromaster 5310 organizer column oven Drain tube B1 Chromaster 5210/5260 Drain tube *2 autosampler T-joint N1 Drain tube A1*1 Chromaster I-joint 5110/5160 pump L-joint Drain tube A1*2 Drain tube *1 Appended Fig. 1-13 Tubing Diagram for Drain (when stacking module units in two blocks) Appended Table 1-6 Drain Tubes to be Used Drain tube B1...
Page 184 5.5 Fastening between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over. When installing the instrument, provide a proper means for preventing the instrument from tipping over accidentally. On the rear of each module unit, a cabling cover is attached. The adjacent models are fastened with each other by attaching the fastening plate between the wiring covers.
Page 185 APPENDIX 2. DESCRIPTION ON CONTACT SIGNAL COMMUNICATION Outline The following two types of contact signals are used in the Chromaster series. Contact signals (START, ERROR, BUSY) entering the e- Line connector. These are contact signals having input/output functions 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.
Page 186 Connection with L-2000 Series Use 3-pin connectors of the e-DIO cable (890-6145) in the connection shown below. ERROR START STOP e-Line connector To L-2000 To Chromaster series instrument series instrument e-Line connector BUSY 3-pin connector e-DIO cable e-DIO cable (890-6145) (890-6145) Connection with Model D-2500 Use the e-DIO cable (890-6146) for connection.
Page 187 Individual Contacts of Each Unit Contact Signal Input Terminals These are contact signal input terminals for control using contact signals from an external switch, relay etc. Any of the signals is activated by shorting the terminal for 0.1 second or longer. The input circuit is shown in Appended Fig.
Page 188 +5 V 320  Max. 10 mA Chromaster series unit External unit Activated upon shorting contacts of external unit. Appended Fig. 2-3 Contact Signal Input Circuit 0.1 A max. 30 V max. Chromaster series unit External unit Appended Fig. 2-4 Contact Signal Output Circuit APPENDIX 2 - 4...
Page 189 APPENDIX 3. TERMINOLOGIES e-line Used for an analysis-specific digital network. UI pad A keypad with LCD to operate an instrument. Interface control board to control the Chromaster series instrument by PC. One IFC for every one system is required. Isocratic system A single liquid is fed using one pump.
Page 190 Log book Means the information containing records of instrument operating conditions. APPENDIX 3 - 2...
Page 191 • Keep this manual in a safe place nearby so it can be referred to whenever needed. 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 3rd Edition, June 2011 Copyright C Hitachi High-Technologies Corporation 2011. 1st Edition, 2011 All rights reserved. Printed in Japan. Part No. 892-9805-2 HH-M (RT-HMS)
Page 192 NOTICE: 1. The Information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Technologies Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Technologies Corporation.
Page 193 PREFACE Thank you very much for purchasing the Chromaster Organizer. The Chromaster Organizer is designed to supply power to each unit (pump, autosampler, detector) and to provide storage space for reagent and other solution bottles in Chromaster liquid chromatograph system. Note that physiologically or biologically active samples are not applicable to the Chromaster Organizer because of possible infection with bacteria or viruses.
Page 194 ABOUT THIS MANUAL This instruction manual describe how to use and maintain the Chromaster Organizer. This instruction manual consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 GENERAL (Outline of Chromaster Organizer) Section 2 FUNCTIONS (Name and Function of Each Part on Pump, Specifications) Section 3 REPLACEMENT PARTS (Replacement Procedure) Section 4 TROUBLESHOOTING...
Page 195 IMPORTANT Warranty on Product Limited Warranty The Chromaster Organizer is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 196 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 197 (m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Technologies shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 198 (b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 199 In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 200 Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 201 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 202 Do not perform any operation or action other than described in these manuals. • On occurrence of any trouble in the instrument, notify the nearest sales service representative of Hitachi High-Technologies. • 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.
Page 203 Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Technologies. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 204 SAFETY SUMMARY WARNING precautions in the Manual WARNING 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 (Section 1) • Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 205 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure to turn off the power switch before proceeding to fuse replacement. (Section 3.1) Electric Shock due to Improper Grounding This instrument is designed in conformity with the specifications of Class I in Annex H of...
Page 206 SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over. When installing the instrument, provide a proper means for preventing the instrument from tipping over accidentally. (APPENDIX 1) SAFETY - 5...
Page 207 If any one of the warning labels becomes illegible due to deterioration, contact your local Hitachi High-Technologies Corporation sales representative or service office of Hitachi High-Technologies Corporation sales representative for replacement with a new one.
Page 208 SAFETY SUMMARY NOTICE precautions Disposal of Waste Solution Be sure to collect waste solution and treat it for proper disposal in accordance with the relevant laws and regulations regarding water pollution control and sewage treatment. Improper treatment of waste solution may result in environmental pollution and could also lead to a penalty.
Page 209 CONTENTS PREFACE.......................1 ABOUT THIS MANUAL..................2 IMPORTANT..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users....IMPORTANT-4 Estimated Life Time of the Instrument........IMPORTANT-4 Caution on Disposal of Instrument .........IMPORTANT-5 Disposal of This Instrument and Its Parts ......IMPORTANT-5 Precautions on CE Conformity Marking .........IMPORTANT-5 Information for Users on WEEE (only for EU Countries) ..IMPORTANT-6 Other Precautions..............IMPORTANT-6...
Page 210 APPENDIX APPENDIX 1. INSTALLATION ............APPENDIX 1-1 Unpacking ................APPENDIX 1-1 Place for Installation .............. APPENDIX 1-2 Items to be Prepared by Customer ........APPENDIX 1-3 Power Supply Arrangement ......... APPENDIX 1-3 Installation Space............APPENDIX 1-7 Check against Packing List ........... APPENDIX 1-7 Assembling................
Page 211: General
1. GENERAL WARNING 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.
Page 212 1. GENERAL WARNING Explosion of Vapor from Flammable Chemicals If a flammable chemical such as organic solvent leaks from the flow path of the instrument and its vapor concentration exceeds the explosion limit, it may cause spontaneous combustion with dangerously explosive results. When using a flammable and ready volatile chemical, be sure to check for leakage from the instrument flow path and ventilate the laboratory room adequately.
Page 213: Outline Of Chromaster Organizer
1.1 Outline of Chromaster Organizer This Chromaster Organizer is capable of providing necessary power sources in Chromaster Series liquid chromatograph system. In addition, the Chromaster organizer can accommodate reagent and other solution bottles for analytical operation of the liquid chromatograph system. 1.2 Configuration of Liquid Chromatograph System The liquid chromatograph system consists of a pump for feeding an eluent, a sample introducing section (autosampler, manual...
Page 214: Isocratic System
1.2 Configuration of Liquid Chromatograph System 1.2.1 Isocratic System The isocratic system has a simple configuration in which single-solvent analysis is performed. Wash fluid Mobile phase Chromaster organizer box Chromaster 5410/5420 5430/5440 detector Chromaster 5310 column oven Column Injection valve Syringe valve Chromaster 5210 autosampler...
Page 215: Low-Pressure Gradient System
1.2.2 1.2.2 Low-Pressure Gradient System In the low-pressure gradient system, two or more solvents are mixed in its low-pressure section from which a liquid feed is performed by a single pump. The composition of an eluent is made to vary with time in chromatographic separation. Wash fluid Mobile phase Chromaster organizer...
Page 216 1.2 Configuration of Liquid Chromatograph System The injected sample is separated through the column which is maintained at a constant temperature by the column oven. Each component separated from the sample is detected as a signal by the detector. 1 - 6...
Page 217: Functions
2. FUNCTIONS 2.1 Name and Function of Each Part on Chromaster Organizer Front bar Fig. 2-1 Front side View • LED : Lights up when power is turned on. • Front bar : The front bar is lowered before the reagent bottle is set up.
Page 218 2.1 Name and Function of Each Part on Chromaster Organizer • Ground terminals : Two ground terminals are provided for grounding connection. • AC inlet : Connect the power cable to this connector. Power button Fig. 2-3 Right side View •...
Page 219: Specifications
2.2 Specifications (1) Power Requirement, and Power Consumption 100 to 240 V AC (50/60 Hz), 520 VA (2) Output 24 V DC, 450 W Provides DC volgate to following units. • Chromaster 5110 pump : 1 unit • Chromaster 5210 autosampler : 1 unit •...
Page 220: Replacement Parts
3.1.1 3. REPLACEMENT PARTS 3.1 Replacement Procedure 3.1.1 Fuse Replacement WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure to turn off the power switch before proceeding to fuse replacement.
Page 221 3.1 Replacement Procedure (b) Replace the fuse with a new one, and then attach the fuse holder by pressing it. 3 - 2...
Page 222: Troubleshooting
3) If power is still not supplied despite taking the above steps (1) and (2), contact our service office of Hitachi High- Technologies Corporation sales representative. LED does not light up. 1) Power is not supplied to 1) Check that power is organizer main unit.
Page 223 5. INDEX Configuration (liquid chromatograph system) ......1-3 Disposal of waste solution..........SAFETY-7 Electric shock ........SAFETY-4, SAFETY-6, 3-1 Explosion of Vapor from Flammable Chemicals ...SAFETY-3 Fuse ..................3-1 Grounding terminal..........APPENDIX1-4 How to replace the fuse ............3-1 Ignition of flammable chemicals ........SAFETY-3 Instrument tipover ............SAFETY-5 Isocratic system ...............
Page 224 Power connector ............ APPENDIX1-8 Power switch ................3-1 Precautions on CE conformity marking....IMPORTANT-4 Specifications ................2-3 Troubleshooting ............... 4-1 Warning and caution labels on instrument ....SAFETY-6 Warranty on Product ..........IMPORTANT-1 5 - 2...
Page 225 If relocation of the instrument becomes necessary after delivery, consult your dealer or nearest Hitachi High- Technologies service representative in order to avoid possible trouble involved in relocation. APPENDIX 1 - 1...
Page 226 2. Place for Installation For installation of the instrument, select a place which meets the following conditions. Operating temperature: Within 4 to 35 °C and with minimum temperature variation during measurement. Utmost care should be used for preventing condensation. Operating humidity: 25 to 85% Atmospheric gas (a) Adequate ventilation is required.
Page 227 Shall be free from excessive dust. Otherwise, performance degradation might be caused. (g) Shall be free from a sudden change of power supply voltage. Otherwise, noise might be caused. (h) Power supply to motor-driven equipment (such as stirrer and vibrator) without a noise suppressor shall not be turned ON/OFF frequently on the same power supply line as that of this instrument.
Page 228 WARNING Electric shock due to improper grounding This instrument is designed to meet the basic insulation stipulated in the international standard IE C61010-1. To prevent an electric shock hazard due to improper grounding, provide a proper grounding connection. Be sure to use the grounded 3P power cable, which is supplied as a standard accessory for the instrument.
Page 229 (a) Usual Grounding Connection (with grounded 3P power outlet) Grounded 3P power outlet (15 A) Grounded 3P table tap Power cord (attached to Chromaster instrument) Organizer Ground resistance 750 mm or 100 Ω or less more below Connector ground Rear panel Grounding electrode 300 mm (underground section)
Page 230 (b) Connection when Grounded Power Outlet is Unavailable 2P power outlet 3P table tap with (15 A) grounding wire Power cord (attached to Chromaster instrument) Grounding Organizer terminal Ground 750 mm or resistance more below Connector 100 Ω or less ground Grounding wire (green) Rear panel...
Page 231 3.2 Installation Space For composing a liquid chromatograph system with the Chromaster series module units, a space of 540 mm wide (980 mm for stacking the units in two blocks) and 550 mm deep is required at least. Behind each unit, a space of 150 mm or more must be secured.
Page 232 5. Assembling NOTE: It is not permitted for the user to carry out installation at the time of delivery. For ensuring safety and high accuracy in operation of the instrument, installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its authorized service agent.
Page 233 Isocratic System/Low-pressure Gradient System (stacked in one block) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump To AC power supply Appended Fig. 1-4 Power Cable Connection Diagram Appended Table 1-1 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer) Connector cable 2)
Page 234 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5440 fluorescence detector To AC power supply Chromaster 5310 column oven Chromaster 5210 autosampler Interface control Chromaster board 5110 pump Appended Fig. 1-5 Power Cable Connection Diagram Appended Table 1-2 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer)
Page 235 5.2 System Cabling In the Chromaster series, the module units are cabled by plugging the e-Line cable into the e-Line connector at the rear left of each unit. e-Line connector Rear panel of module unit Power connector Isocratic System/Low-pressure Gradient System Chromaster organizer e-Line cable 1)
Page 236 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/ e-Line cable 1) 5420/5430/5450 detector e-Line cable 2) Chromaster 5440 fluorescence detector Chromaster 5310 column oven Chromaster organizer Chromaster 5210 autosampler Chromaster Interface control 5110 pump board Appended Fig. 1-7 e-Line Cable Connection Appended Table 1-4 Cables to be Used e-Line cable 1) (50 cm) P/N 890-6105 (attached to each unit)
Page 237 5.3 System Tubing In the Chromaster series, the inlet tube up to the pump and drain tube are fastened to the right/left side face of each unit with tube clamps. And the tubes are connected from the pump to the autosampler, column and detector through the central hole of each module unit.
Page 238 Chromaster 5440 fluorescence detector Detector cell Mobile- phase Chromaster 5310 liquid Detergent column oven Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump Degassing unit Drain Appended Fig. 1-9 Tubing Diagram of Isocratic System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to the IN port of degassing unit.
Page 239 Low-pressure Gradient System Detergent Mobile-phase liquid Chromaster organizer Chromaster 5410/5420/ 5430 detector Chromaster 5310 Injection valve column oven Syringe valve Chromaster 5210 autosampler Wash pump Low-pressure gradient unit/ proportioning valve Chromaster 5110 pump Degassing unit Drain Appended Fig. 1-10 Tubing Diagram of Low-Pressure Gradient System (stacked in one block) APPENDIX 1 - 15...
Page 240 Chromaster 5440 fluorescence detector Detector cell Mobile-phase liquid Detergent Chromaster 5310 column oven Mixer Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump 4-way joint Degassing unit Proportioning Drain valve Appended Fig. 1-11 Tubing Diagram of Low-Pressure Gradient System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to...
Page 241 Drain Tubing Drain tube A1 Chromaster organizer Chromaster 5410/5420/ T-joint 5430/5450 detector Chromaster 5310 column oven Drain tube A2 Chromaster 5210 autosampler Drain tube 4 Chromaster 5110 T-joint N1 pump Drain tube B1 Drain tube L-joint Appended Fig. 1-12 Tubing Diagram for Drain (when stacking module units in one block) Appended Table 1-5 Drain Tubes to be Used Drain tube A2...
Page 242 Chromaster 5440 fluorescence detector T-joint Drain tube A1*3 Chromaster Chromaster 5310 organizer column oven Drain tube B1 Chromaster 5210 Drain tube *2 autosampler T-joint N1 Drain tube A1*1 Chromaster 5110 I-joint pump L-joint Drain tube A1*2 Drain tube *1 Appended Fig. 1-13 Tubing Diagram for Drain (when stacking module units in two blocks) Appended Table 1-6 Drain Tubes to be Used Drain tube B1...
Page 243 5.4 Fastening between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over. When installing the instrument, provide a proper means for preventing the instrument from tipping over accidentally. On the rear of each module unit, a cabling cover is attached. The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers.
Page 245 APPENDIX 2. TERMINOLOGY Degassing Eliminates the air in a mobile phase and wash fluid. e-line Used for an analysis-specific digital network. Interface control board to control the chromaster series instrument by PC. One IFC for every one system is required. Isocratic system A single liquid is fed using one pump.
Page 246 • Keep this manual in a safe place nearby so it can be referred to whenever needed. © Copyright Hitachi High-Technologies Corporation 2011. All rights reserved. Printed in Japan. Part No. 892-9520-1 HH-M (SG-LT) 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 3rd Edition, June 2011 Copyright C Hitachi High-Technologies Corporation 2011.
Page 247 NOTICE: 1. The Information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Technologies Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Technologies Corporation.
Page 248 PREFACE Thank you very much for purchasing Chromaster 5420 UV-VIS Detector. The Chromaster 5420 UV-VIS Detector is specifically designed for the change in absorbance in a liquid chromatograph system.. Note that physiologically or biologically active samples are not applicable to the Chromaster 5420 UV-VIS Detector because of possible infection with bacteria or viruses.
Page 249: Index
ABOUT THIS MANUAL This instruction manual describe how to use and maintain the Chromaster 5420 UV-VIS Detector. This instruction manual. consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 OVERVIEW (Isocratic System, Low-Pressure Gradient System) Section 2 FUNCTIONS (Explanation of Power Switch and Others on Front Panel) Section 3 OPERATION (Basic Operations, Utility Setting) Section 4 MAINTENANCE &...
Page 250 IMPORTANT Warranty on Product Limited Warranty The Chromaster 5420 UV-VIS Detector is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 251 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 252 (m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Technologies shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 253 (b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 254 In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 255 Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 256 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 257 Do not perform any operation or action other than described in these manuals. • On occurrence of any trouble in the instrument, notify the nearest sales service representative of Hitachi High-Technologies. • 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.
Page 258 Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Technologies. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 259 SAFETY SUMMARY WARNING precautions in the Manual WARNING 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 (Section 3.6, 4.4) • Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 260 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Electric Shock due to Contact with Inside of Instrument Before removing the light source cover for replacement of the light source lamp, be sure to turn off the power switch and unplug the power cord. (Section 5.2) Electric Shock due to Improper Grounding This instrument is designed in conformity with the specifications of Class I in Annex H of...
Page 261 SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Touching Hot Part Could Result in Burns The light source lamp and its cover become hot during operation and remain hot for a while even after power-off. They can severely burn you if touched. Before replacement of the lamp, turn power off and wait for about 30 minutes until it cools down sufficiently.
Page 262 If any one of the warning labels becomes illegible due to deterioration, contact your local Hitachi High-Technologies Corporation sales representative or service office of Hitachi High-Technologies Corporation sales representative for replacement with a new one.
Page 263 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument (3) Electric Shock due to Contact with (4) Burns due to Contact with Hot Parts Power Supply to Light Source Front View SAFETY - 7...
Page 264 SAFETY SUMMARY NOTICE precautions Precautions on Use of Solvents • Fluororesin, PEEK, quartz and SUS316 materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials. • This instrument has internal parts made of materials that could be corroded by strongly acidic solutions, strongly alkaline solutions or organic solvents.
Page 265 SAFETY SUMMARY NOTICE precaution (Continued) Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally. If necessary, conduct measurement on a control sample. Possible Carryover When examining the results of measurements, take account of the possibility of occurrence of a carryover.
Page 266 CONTENTS PREFACE.......................1 ABOUT THIS MANUAL..................2 IMPORTANT..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users....IMPORTANT-4 Estimated Life Time of the Instrument........IMPORTANT-4 Caution on Disposal of Instrument .........IMPORTANT-5 Disposal of This Instrument and Its Parts ......IMPORTANT-5 Precautions on CE Conformity Marking .........IMPORTANT-5 Information for Users on WEEE (only for EU Countries) ..IMPORTANT-6 Other Precautions..............IMPORTANT-6...
Page 267 3.1.6 Washing after Use ................3-9 Utility Setting ....................3-10 3.2.1 Setting the Offset................3-10 3.2.2 Setting the Time Constant ..............3-12 3.2.3 Setting the Use or Non-use of Time Program ........3-13 3.2.4 Setting the Polarity ................3-14 3.2.5 Other Settings ...................
Page 268 Maintenance/Check Procedure ..............4-10 4.4.1 Checking the Energy and Wavelength Accuracy of Light Source Lamp ................4-10 4.4.2 Checking the Logbook of Light Source Lamp ........4-11 4.4.3 Checking and Cleaning the Flow Cell ..........4-12 4.4.4 Disassembling and Cleaning the Flow Cell ........4-15 Troubleshooting ....................
Page 269: Overview
1. OVERVIEW The liquid chromatograph system comprises a pump for delivering mobile-phase liquid, a sample introduction unit for injecting samples (autosampler, manual injector), a column unit for separating components of each sample, a column oven unit for maintaining the column at a constant temperature, and a detector unit for detecting separated components as analytical signals.
Page 270 1.1 Isocratic System Mobile-phase liquid is delivered with the pump through the degassing unit. A sample is injected with the autosampler. The injected sample is separated into its constituents with the column maintained at a constant temperature by means of the column oven. The separated sample constituents are taken out as analytical signals with the detector.
Page 271 1.2 Low-Pressure Gradient System This is a system for mixing plural solvents in the low pressure section and delivering the mixture with a single pump. Sample constituents are separated by changing the composition of mobile phase with time. Detergent Mobile phase Chromaster organizer Chromaster 5410/...
Page 272 1.2 Low-Pressure Gradient System The injected sample is separated into its constituents with the column maintained at a constant temperature by means of the column oven. The separated sample constituents are taken out as analytical signals with the detector. 1 - 4...
Page 273: Functions
2. FUNCTIONS 2.1 Explanation of Power Switch and Others on Front Panel Power switch Door (left) UI pad (option) Door (right) Fig. 2-1 Front View • Power switch : Turns on/off power supply. • UI pad : A keypad required for stand-alone operation of this module unit (available at option).
Page 274: Part Names And Functions Of Ui Pad (Option)
2.2 Part Names and Functions of UI Pad (Option) 2.2 Part Names and Functions of UI Pad (Option) When this module unit is not controlled by Chromato Data Station (CDS) or GUI controller (option), it is controllable with the UI pad. For details of operation keys, refer to Chapter 3.
Page 275 (cont’d) Indication Function Refer to: (GLP) Used for setting key lock, for checking lamp energy and wavelength accuracy, and for displaying and resetting the light source lamp logbook. INSERT (Set program = Insert) 3.4.4 (1) Selects and sets the time program. 3.4.7 (2) Inserts a new step in the time PROG...
Page 276: Rear Panel
2.3 Rear Panel 2.3 Rear Panel MARKER IN PROCESSOR RECORDER Fig. 2-3 Rear Panel Indication Function Remarks e-Line (1) Used to transmit the (1) Absorbance values are acquisition signal (or acquired output. spectral data) via the e-Line. Also, used to send/receive the instrument condition data via the e-Line.
Page 277: Principle Of Operation
2.4 Principle of Operation W lamp Aberration-free Condensing concave grating G1 mirror M1 Filter F (O-54/UV-32) Slit S1 Slit S2 Detector R Detector S Flow cell Half mirror lamp Condensing mirror M2 Fig. 2-4 Optical Schematic of this UV-VIS Detector Unit The light emitted from the light source (D /W lamp) strikes condensing mirror M1, passes through slit S1 and then is...
Page 278 2.4 Principle of Operation And, for measurement in the D2&W lamp mode, filter F (UV-32) is inserted in the optical path within 351 to 400 nm, and filter F (O-54) is inserted in the optical path within 601 to 900 nm in order to cut off the second-order diffraction light.
Page 279: Specifications
2.5 Specifications Optical system : Double-beam ratio photometric system (dispersion with diffraction grating) Light source : D2 lamp W lamp Hg lamp (for checking monochromator wavelength) Measuring wavelength range (a) 1-wavelength measurement : 190 to 900 nm In the D2&W mode, the D2 lamp is used at 400 nm or shorter and the W lamp is used at 401 nm or longer.
Page 280 2.5 Specifications Noise (a) 1-wavelegth measurement : 0.5 × 10 AU or less (conditions: wavelength 250 and 600 nm, air in cell, time constant 2.0 sec, data sampling period 400 (b) 2-wavelegth measurement : 3.5 × 10 AU or less (conditions: wavelength 210 and 250 nm, air in cell, data sampling period 800 ms)
Page 281 (15) Spectrum acquisition range : 200 to 900 nm (D2&W mode) 200 to 600 nm (D2 mode) 380 to 900 nm (W mode) BACK MEMO (background spectrum memory) acquisition range : 190 to 600 nm (D2&W mode) 190 to 600 nm (D2 mode) 380 to 900 nm (W mode) (max.
Page 282 (28) Power consumption : 85 VA : 340 (W) × 440 (D) × 140 (H) mm (29) Dimensions (30) Weight : 14 kg NOTE: Please contact your local Hitachi High- Technologies Corporation sales representative about a purchas of the Thermo cell. 2 - 10...
Page 283: Operation
3.1.1 3. OPERATION The method of operating this detector with the UI pad (option) is explained here. For operation method of each option, and operation methods by GUI controller (option) and CDS, refer to the respective instruction manuals. CAUTION Fatigue due to long-hour operation If you keep working with the display monitor and keyboard for long hours, your eyes and body will be fatigued to jeopardize your health.
Page 284 Upon turning on power supply to the detector, copyright indication and program No. Rev. can be checked. UV-VIS Detector 8928142-00 (C)Hitachi High-Technologies Corp. 2010 After a few seconds, the next screen appears and self- diagnostic test (initialization) is carried out. WL DRIVE & LAMP INITIALIZING When initialization has been normally terminated, the next screen, or monitor screen appears.
Page 285 3.1.1 Monitor Screen in 1-wavelength Measurement Monitor screen 1 (ABS indication) Status display TIME PROG LAMP 0.0000 D2&W Elapsed Lamp indication time Program No. Wavelength Absorbance (a) The currently selected program No. is indicated. (b) LAMP indicates the lit or extinguished status of each lamp.
Page 286 3.1 Turning on Power Supply Monitor Screen in 2-wavelength Measurement Setting for 2-wavelength measurement can be made by CDS. The monitor screen of UI pad displays the present instrument status. Monitor screen 1 (ABS indication) Status display ABS1 ABS2 0.0001 0.0001 Wave- length 1...
Page 287: Parameter Input Method
3.1.2 NOTE: The time for the instrument to stabilize varies with the measurement conditions. Secure a warm-up time depending on the conditions. (Reference warm-up time: About 1 hour) NOTE: Temperature of the thermostatic flow cell varies with the set time (measuring conditions). If pump flow velocity or oven temperature is changed, provide a warmup time in accordance with measuring conditions (reference: about 30...
Page 288 3.1 Turning on Power Supply (d) Program setup screen Input item TIME BASE (A/Z=1, HOLD=2) Input part Numerical Input Procedure (a) A cursor appears at the head of input part. In this part, the previously set numeral is indicated. (b) Within the acceptable number of characters, input by numerical keys and decimal point key will be accepted.
Page 289 3.1.2 1) For canceling an input, use the [CL] key when the [ENT] key has not yet been pressed, and carry out input again. When the [ENT] key has already been pressed, use the [ESC] key for cancellation. Display will return to the first monitor screen.
Page 290: Auto Zero
3.1 Turning on Power Supply 3.1.3 Auto Zero (Auto zero) ABS indication and output signal on the monitor screen can be zeroed. TIME PROG LAMP 0.0000 Auto zero adjustable range: -0.2 to 2 AU If this range is exceeded, the following message appears. A/Z OVER RANGE PRESS “CL”...
Page 291: Shutdown
3.1.5 3.1.5 Shutdown The instrument can be shut down by turning off its power switch. Even when power supply is turned off, the set measurement conditions are stored in memory. Therefore, when turning on power supply again, the set conditions before turning off power supply are called out to allow measurement under the conditions.
Page 292: Utility Setting
3.2 Utility Setting 3.2 Utility Setting SET UP UTLTY (Utility) The utility setup screen appears. UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Input Numeral Function OFFSET Set an offset. TIME CONSTANT : Set a time constant. USE PROG Select or avoid use of a time program.
Page 293 3.2.1 Set an offset value. Press [numerical] key (within [0] to [1][0][0][0]: Usually input [0]), and then the [ENT] key. * Settable range : 0 to 1000 AU, settable in increments of 1 * Default value ■ Since the negative voltage input range is around -10 mV with the usual data processor, a baseline lower than -10 mV level may disable integration of some chromatogram peaks (Fig.
Page 294: Setting The Time Constant
3.2 Utility Setting 3.2.2 Setting the Time Constant An electrical response speed/time can be set. SET UP UTLTY Press key. The utility setup screen appears. Utility Setup Screen UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Select TIME CONSTANT. Press [numerical] key [2], and then the [ENT] key. The time constant setup screen appears.
Page 295: Setting The Use Or Non-Use Of Time Program
3.2.3 3.2.3 Setting the Use or Non-use of Time Program Automatic change of measurement conditions with time (time program) can be selected or avoided. SET UP UTLTY Press key. The utility setup screen appears. Utility Setup Screen UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Select USE PROG.
Page 296: Setting The Polarity
3.2 Utility Setting 3.2.4 Setting the Polarity When NEGATIVE is selected, absorbance can be output in a negative value. SET UP UTLTY Press key. The utility setup screen appears. Utility Setup Screen UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Select POLARITY.
Page 297: Other Settings
3.2.5 3.2.5 Other Settings Input Numeral Function PROCESSOR Set the full scale of processor output. ERROR OUT Select the Enable or Disable status of error signal output. LEAK SENSOR : Select use or non-use of the leak sensor. LAMP Select ON/OFF status of the /W lamp.
Page 298 3.2 Utility Setting Set the full scale of processor output. Press [numerical] key (within [1] to [4]), and then the [ENT] key. * Default value: 3 Upon completion of processor setting, the first monitor screen reappears. Setting the Enable or Disable Status of Error Signal Output SET UP UTLTY Press...
Page 299 3.2.5 Setting the Use (ON) or Non-use (OFF) Status of Leak Sensor SET UP UTLTY Press key. The utility setup screen appears. Utility Setup Screen UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Select OTHERS. Press [numerical] key [5], and then the [ENT] key. The OTHERS setup screen appears.
Page 300 3.2 Utility Setting Setting the ON/OFF Status of D Lamp/W Lamp SET UP UTLTY Press key. The utility setup screen appears. Utility Setup Screen UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Select OTHERS. Press [numerical] key [5], and then the [ENT] key. The OTHERS setup screen appears.
Page 301 3.2.5 Upon completion of LAMP setting, the first monitor screen reappears. Setting the Gain Gain is selectable so as to match the flow cell to be used. SET UP UTLTY Press key. The utility setup screen appears. Utility Setup Screen UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, POLARITY=4, OTHERS=5) Select OTHERS.
Page 302 3.2 Utility Setting NOTE: When MICRO is set for GAIN, energy level may reach the upper limit of measurement or A/Z OVER RANGE may be caused when auto zero is executed. For a wavelength where light quantity is large or when a difference in light quantity is large between sample and reference sides, you should set NORMAL for GAIN.
Page 303: Glp-Related Functions
3.3 GLP-Related Functions Logbooks of D , W, and Hg lamps can be displayed and reset. And, keys on the keyboard can be locked so that key input will not be attempted in error during analysis, etc. (Good Laboratory Practice) Pressing the GLP key presents the GLP setup screen.
Page 304: Logbook Of D2/W/Hg Lamp
3.3 GLP-Related Functions 3.3.1 Logbook of D /W/Hg Lamp The cumulative lamp-on time (referential lifetime), lamp-on count and lamp exchange date can be displayed for each of D2, W and Hg lamps. Display of D /W/Hg Lamp Logbook at Lamp Exchange Press key.
Page 305 3.3.1 Select REPORT. Press [numerical] key [1], and then the [ENT] key. For D lamp logbook: D2 LAMP SWITCHING LAST CHANGED DATE 123 h 23 times 2/25/2010 For W lamp logbook: W LAMP SWITCHING LAST CHANGED DATE 123 h 23 times 2/25/2010 For Hg lamp logbook: Hg LAMP...
Page 306 3.3 GLP-Related Functions The lamp selection screen appears. LAMP SELECT (D2=1，W=2，Hg=3) For selection of D lamp : Press [numerical] key [1], and then the [ENT] key. For selection of W lamp : Press [numerical] key [2], and then the [ENT] key. For selection of Hg lamp : Press [numerical] key [3], and then the [ENT] key.
Page 307 3.3.1 Press numerical (month) key ([1] to [1][2]), and then the [ENT] key. Press numerical (day) key ([1] to [3][1]), and then the [ENT] key. Press numerical (year) keys ([2][0][0][0] to ([2][1][0][0]), and then the [ENT] key. For resetting of Hg lamp: （MM Hg LAMP CHANGE YYYY）...
Page 308: Key Lock
3.3 GLP-Related Functions 3.3.2 Key Lock Keys on the keyboard are settable in the unacceptable status. Wrong key input is prevented by applying key lock to the operation panel. NOTE: When the GUI controller or CDS is connected, operation with the UI pad becomes ineffective. Press key.
Page 309: Checking The Energy And Wavelength Accuracy Of D2 Lamp
When no bright lines have been detected, “NOT DETECTED” is indicated. In this case, confirm mounting of the flow cell, and then turn on power supply again. If the situation does not improve, contact the nearest maintenance service company authorized by Hitachi High- Technologies. 3 - 27...
Page 310: Checking The Energy Of W Lamp
3.3 GLP-Related Functions 3.3.4 Checking the Energy of W Lamp Energy of the W lamp is checked using the 600 nm bright line of W lamp. Press key. The GLP setup screen appears. GLP Setup Screen GLP (LOGBOOK=1, KEY LOCK=2, D2 CHECK=3, W CHECK=4, Hg CHECK=5) Select W CHECK.
Page 311: Checking The Wavelength Accuracy With Hg Lamp
“NOT DETECTED” is indicated. In this case, confirm mounting of the flow cell, and then turn on power supply again. If the situation does not improve, contact the nearest maintenance service company authorized by Hitachi High-Technologies. 3 - 29...
Page 312: Analyzing Operation
3.4 Analyzing Operation 3.4 Analyzing Operation 3.4.1 Spectrum Measurement SPECT (Spectrum) The spectrum measurement mode setup screen appears. SPECTRUM MODE (ABS =1, BACK GROUND=2, D2 REF =3, W REF =4, Hg =5) Input Numeral Function Stores spectral data in memory. BACK GROUND : Stores background spectrum in memory.
Page 313 3.4.1 Next, set the maximum wavelength of scan range. SCANNING WL RANGE (WL1 WL2) nm <250 – 600> 200 – 600 Press [numerical] keys (within [2][5][0] to [9][0][0]), and then the [ENT] key. * Enterable range: Minimum scan range is 50 nm. Measuring span is max.
Page 314 3.4 Analyzing Operation Storing the Background Spectral Data in Memory (“2” key followed by ENT key) Scan is automatically carried out. During acquisition of the background spectrum, the following screen is presented. SCANNING BACK GROUND SPECTRUM WL: *** nm Upon completion of spectral data acquisition, the monitor screen automatically appears.
Page 315 3.4.1 Press [numerical] key (within [1] to [3]), and then the [ENT] key. During spectrum acquisition, the following screen is presented. SCANNING SPECTRUM NO.: 1 MODE: D2 REF WL: *** nm After spectrum acquisition, the monitor screen automatically appears. Storing the Reference Energy with W Lamp in Memory (“4” key followed by ENT key) Set the minimum wavelength of scan range.
Page 316 3.4 Analyzing Operation During spectrum acquisition, the following screen is presented. SCANNING SPECTRUM NO.: 1 MODE: W REF WL: *** nm After spectrum acquisition, the monitor screen automatically appears. Storing the reference energy with mercury lamp (“5” key followed by ENT key) Upon selection of this function, the mercury lamp is ignited and automatically selected during spectrum scan.
Page 317 3.4.1 Press [numerical] key (within [1] to [3]), and then the [ENT] key. During spectrum acquisition, the following screen is presented. SCANNING SPECTRUM NO.: 1 MODE: Hg WL: *** nm After spectrum acquisition, the monitor screen automatically appears. 3 - 35...
Page 318: Setting Of Recorder And Spectrum Output
3.4 Analyzing Operation 3.4.2 Setting of Recorder and Spectrum Output RECORD (Record) The setup screen appears. RECORD (RCD RANGE=1, RCD SPEED=2, SPECT RCD=3) Input Numeral Function RCD RANGE : Sets the full scale range of recorder. RCD SPEED : Sets the spectrum output speed of recorder.
Page 319 3.4.2 Setting the Spectral Data to be Output (“3” key followed by ENT key) RECORD SPECTRUM NO. (1–3) Press [numerical] key (within [1] to [3]), and then the [ENT] key. Next, input the spectrum No. for output. In ABS data mode: The output wait screen appears.
Page 320: Operation Of Marker
3.4 Analyzing Operation 3.4.3 Operation of Marker MARKER (Marker) Marker is output to the recorder terminal alone. This is usable as a reference for measurement start or as an event marker when the set condition is changed during measurement, for example.
Page 321 3.4.4 Input of Time Press [numerical] key (within [0] to [6][0][0]), and then the [ENT] key. * Enterable range: 0.0 to 600.0 minutes, enterable in steps of 0.1 minute. (The first step is fixed at 0.0 minute.) Upon pressing the ENT key, the cursor moves to the measuring wavelength.
Page 322: Execution Of Time Program
3.4 Analyzing Operation 3.4.5 Execution of Time Program START (Start) The time program starts. TIME PROG LAMP 0.0000 D2&W Status display becomes “R” (time program being executed) and time indication is being updated. 3.4.6 Stop of Time Program STOP (Stop) The time program stops and display returns to the monitor screen.
Page 323 3.4.7 Explained here is how to create a new time program exemplifying the one shown above. At start, the measuring wavelength is set at 250 nm and auto zero adjustment is carried out for baseline. After 10 minutes, the measuring wavelength is changed to 270 nm.
Page 324 3.4 Analyzing Operation TIME BASE (A/Z=1, HOLD=2) 10.0 Press the [ENT] key. TIME BASE (A/Z=1, HOLD=2) Press [numerical] keys [2][0], and then the [ENT] key. Press [numerical] keys [2][7][0], and then the [ENT] key. Press numerical] key [1]. TIME BASE (A/Z=1, HOLD=2) 20.0 Press the [ESC] key.
Page 325 3.4.7 TIME BASE (A/Z=1, HOLD=2) _ 0.0 ▽ For displaying the next step, press the key. TIME BASE (A/Z=1, HOLD=2) _10.0 ▽ For displaying the next step, press the key. TIME BASE (A/Z=1, HOLD=2) _20.0 Press the [ESC] key, and display will return to the monitor screen.
Page 326: Setups
3.5 Setups 3.5 Setups The SETUP screen appears when you press the UTLTY key simultaneously with power-on. SET UP (Setup) POWER UTLTY The SETUP screen now appears. SETUP: DETECTOR THERMO CONTRAST S.NO. NO USE 1401-001 Press the [ENT] key. The selection screen appears. SETUP ITEMS (DETECTOR=1, THERMO CELL=2, CONTRAST=3) Input Numeral...
Page 327: Selection Of Communication Channel
3.5.1 3.5.1 Selection of Communication Channel SET UP POWER UTLTY Press keys simultaneously. The SETUP screen now appears. SETUP: DETECTOR THERMO CONTRAST S.NO. NO USE 1401-001 Press the [ENT] key. The selection screen appears. SETUP ITEMS (DETECTOR=1, THERMO CELL=2, CONTRAST=3) Press [numerical] key [1], and then the [ENT] key.
Page 328: Setting Of Thermostatic Flow Cell
3.5 Setups 3.5.2 Setting of Thermostatic Flow Cell SET UP POWER UTLTY Press keys simultaneously. The SETUP screen now appears. SETUP: DETECTOR THERMO CONTRAST S.NO. NO USE 1401-001 Press the [ENT] key. The selection screen appears. SETUP ITEMS (DETECTOR=1, THERMO CELL=2, CONTRAST=3) Press numerical key [2], and then the [ENT] key.
Page 329: Setting Of Lcd Contrast
3.5.3 3.5.3 Setting of LCD Contrast SET UP POWER UTLTY Press keys simultaneously. The SETUP screen now appears. SETUP: DETECTOR THERMO CONTRAST S.NO. NO USE 1401-001 Press the [ENT] key. The selection screen appears. SETUP ITEMS (DETECTOR=1, THERMO CELL=2, CONTRAST=3) Press [numerical] key [3], and then the [ENT] key.
Page 330: Before Analysis
3.6 Before Analysis 3.6 Before Analysis Basic precautions before start of analysis are described here. WARNING Ignition of flammable chemicals! ● This instrument is not explosion-proof. During unmanned operation, avoid use of organic solvents having an ignition point below 70 °C. ●...
Page 331: Precautions On Selection And Handling Of Mobile Phase
3.6.1 WARNING Inflammation or injury due to toxic, corrosive or stimulative solvent! When using a toxic, corrosive or stimulative solvent, be careful not to incur inflammation or injury. For details of the properties of each solvent and how to handle it, refer to Material Safety Data Sheet (MSDS).
Page 332 3.6 Before Analysis Be sure to degas the mobile phase before its use. (a) Because an organic solvent has a particularly high air content, fluctuations of the baseline, malfunction of the check valve and a fall in column efficiency may be caused by air bubbles.
Page 333 3.6.1 NOTE: If the suction or discharge valve on the side of pump head (1) is dry, the mobile phase may not be sucked in the early stage after pump start. In this case, aspirate the mobile phase into the furnished syringe and discharge the mobile phase from the suction valve to the discharge valve side.
Page 334 3.6 Before Analysis Table 3-1 Reagents Restricted in Use as Mobile Phase Usable Usable below 50% Usable below 10% Undesirable for SUS 316 Phosphoric acid Acetic acid Disodium phosphate Ammonium chloride Sodium phosphate Ammonium citrate Ammonium formate Potassium chloride Ammonium nitrate Ammonium perchlorate Sodium chloride Citric acid...
Page 335: Characteristics Of Organic Solvents
3.6.2 3.6.2 Characteristics of Organic Solvents The characteristics of organic solvents as mobile phases of liquid chromatograph are listed in Table 3-2. Utilize this table for your reference. WARNING Ignition of flammable chemicals! ● This instrument is not explosion-proof. During unmanned operation, avoid use of organic solvents having an ignition point below 70 °C.
Page 336 3.6 Before Analysis WARNING Inflammation or injury due to toxic, corrosive or stimulative solvent! When using a toxic, corrosive or stimulative solvent, be careful not to incur inflammation or injury. For details of the properties of each solvent and how to handle it, refer to Material Safety Data Sheet (MSDS).
Page 337 3.6.2 Table 3-2 Characteristics of Organic Solvents Ignition Point Specific Refrac- Flash Vapor Boiling Polarity Viscosity Gravity tive Cutoff Point Density Point Lower Upper (cP20°C) (water = (°C) Index (nm) (°C) (air = 1) (°C) Limit Limit Fluoroalkanes -0.25 1.25 0.00 0.23 <-40...
Page 338 3.6 Before Analysis NOTE: For Using Organic Solvent as Mobile Phase (1) When using an organic solvent, pay attention to UV cutoff wavelength. • UV cutoff wavelength refers to a wavelength below which light will not be transmitted. For example, because chloroform has a cutoff wavelength of 245 nm, it cannot be used at a wavelength shorter than 245 nm (e.g., 210 nm).
Page 339: Caution On Static Electricity
3.6.3 3.6.3 Caution on Static Electricity WARNING Ignition of flammable chemicals due to static electricity! When using flammable chemicals, be careful about possible ignition due to static electricity. To prevent ignition due to static electricity, observe the following precautions. (a) Use a grounded and conductive container for waste solution in order to prevent a build-up of static electricity.
Page 340: Preparatory Operation
3.7 Preparatory Operation 3.7 Preparatory Operation NOTE: When using an ultrasonic washer or the like, follow its instruction manual. 3.7.1 Degassing and Decontamination of Mobile Phase Be sure to degas the mobile phase before its use. Oxygen, nitrogen and other gases contained in the mobile phase will cause the following if used at a high pressure;...
Page 341: Degassing Of Mobile Phase
3.7.2 3.7.2 Degassing of Mobile Phase There are various degassing methods. Use a method suitable for your analytical purpose. Example of Degassing by Ultrasonic Wave (when mobile phase is an organic solvent) Example : Methanol 100%, mixed solution of methanol 80% + acetonitrile 20% Necessary device : Ultrasonic washer (Be sure to fill the bath with water.) Be sure to...
Page 342 3.7 Preparatory Operation (d) After confirming that no bubbles are discharged, turn OFF the power switch of the ultrasonic washer. (e) Take out the mobile phase container from the ultrasonic washer and wipe off moisture adequately. Then set the container in a liquid chromatograph. Example of Degassing by Decompression (when mobile phase is an aqueous solution) Example:...
Page 343 3.7.2 (b) Insert the rubber tube from the aspirator into the mouth of the mobile phase container. (c) Turn ON the power switch of the ultrasonic washer. (d) Reduce pressure by “opening” the tap water spigot connected with the aspirator. (e) As degassing progresses, small bubbles are discharged and they gradually become larger.
Page 344: Decontamination Of Mobile Phase
3.7 Preparatory Operation 3.7.3 Decontamination of Mobile Phase There are various methods of decontamination of mobile phase. Select a decontamination method suitable for your analytical purpose. Example of Mobile Phase Filtration with Membrane Filter Decontamination and degassing can be achieved simultaneously by passing the mobile phase through a 0.45 μm membrane filter.
Page 345: Sample Treatment
3.7.4 3.7.4 Sample Treatment Be sure to filtrate a sample which contains fine-particle dusts. Otherwise, the column might be clogged and deteriorated earlier than normal. Be sure to remove inclusions from a sample. Otherwise, data reliability may be degraded due to appearance of abnormal peaks, etc.
Page 346: Maintenance And Checkup
4. MAINTENANCE AND CHECKUP 4.1 Confirmation of Basic Actions Prepare the instrument as instructed in Appendix 1. Turn on the power switch of this detector. Confirm that measuring conditions (time constant, output range, etc.) can be set normally. Confirm wavelength operation using key.
Page 347: Confirmation Of Performance Specifications
4.2 Confirmation of Performance Specifications 4.2 Confirmation of Performance Specifications 4.2.1 Items of Performance Specification Check Measurement of Light Source Lamp Energy (See 4.4.1) • Measuring wavelength: 250 nm • Reference at the time of installation Energy indication of 150,000 or more at wavelength 250 nm The indicated energy value has a slight difference among the light source lamps due to their characteristics.
Page 348: Measurement Of Baseline Noise
4.2.2 Baseline Measurement in 2-wavelength Measurement 2-wavelength measurement is settable from the CDS. This measurement cannot be carried out by the detector alone. • Conditions......Room temperature constant, air in flow cell, data sampling period 800 ms • Measuring wavelength..Wavelength 1; 210 nm, wavelength 2;...
Page 349 4.2 Confirmation of Performance Specifications After turning on power supply, set wavelength at 250 nm and conduct warm-up for about 1 hour. Press key. WAVELENGTH (190 – 600) nm Press [numerical] keys [2][5][0], and then the [ENT] key. Carry out auto zero. Press key.
Page 350: Measurement Of Baseline Drift
4.2.3 4.2.3 Measurement of Baseline Drift Detector specifications are to be checked by measuring drift of the baseline. For this measurement, the following devices should be prepared. • Recorder or Model D-2500 chromato-integrator • Vernier caliper (max. measurable length 200 mm or more, minimum readable value 0.1 mm or less) NOTE: When the inside of flow cell is wetted with liquid, baseline noise and drift may increase.
Page 351 4.2 Confirmation of Performance Specifications Start the chromato-integrator and record the baseline for 1 hour. From the recorded chart, figure out drift value according to ASTM1657-98 (JAIMAS 0005-2008). Drift value = D (Excerpt from JAIMAS 0005-2008) 4 - 6...
Page 352: Periodic Checkup
4.3.1 4.3 Periodic Checkup 4.3.1 Check of Liquid Leak Sensor For detection of liquid leak, a liquid leak sensor is mounted. However, if the sensor is contaminated, liquid leak might not be detected properly. To prevent this, checkup and cleaning should be carried out periodically.
Page 353 4.3 Periodic Checkup Cleaning of Leak Sensor <Item to be prepared> Hexagonal wrench (P/N: N315003) (a) Remove the leak sensor fastening screw with the furnished hexagonal wrench and separate the leak sensor from the drain tray. (b) Wipe off the water adhering to the leak sensor and drain tray.
Page 354: Periodic Maintenance/Checkup
4.3.2 4.3.2 Periodic Maintenance/Checkup For ensuring reliable routine operations through prevention of a trouble, periodic checkup must be carried out, referring to Table 4-1. This table lists the items of periodic maintenance/checkup. Table 4-1 Periodic Maintenance/Checkup Check Item Interval Check Procedure Remarks Drain tray Every day...
Page 355 DETECTED” is indicated. In this case, confirm mounting of the flow cell, and then turn on power supply again. If the situation does not improve, contact the nearest maintenance service company authorized by Hitachi High- Technologies. NOTE: When the D2 ENERGY level has fallen to 50% or...
Page 356 In this case, confirm mounting of the flow cell, and then turn on power supply again. If the situation does not improve, contact the nearest maintenance service company authorized by Hitachi High-Technologies. 4.4.2 Checking the Logbook of Light Source Lamp Lamp...
Page 357 4.4 Maintenance/Check Procedure The cumulative ON period, number of ON times and the input date of replacement (month, day, year) are indicated at Hg LAMP, SWITCHING and LAST CHANGED DATE, respectively. 4.4.3 Checking and Cleaning the Flow Cell WARNING Ignition of flammable chemicals! ●...
Page 358 4.4.3 WARNING Inflammation or injury due to toxic, corrosive or stimulative solvent! When using a toxic, corrosive or stimulative solvent, be careful not to incur inflammation or injury. For details of the properties of each solvent and how to handle it, refer to Material Safety Data Sheet (MSDS).
Page 359 4.4 Maintenance/Check Procedure Check and clean the flow cell in the following procedure. Unplug the connector of thermostatic flow cell control cable. Loosen the clamp screws and take out the flow cell section. Visually check the inside of flow cell for sticking of foreign material (such as crystallized substance) and for contamination.
Page 360 4.4.4 4.4.4 Disassembling and Cleaning the Flow Cell WARNING Ignition of flammable chemicals! ● This instrument is not explosion-proof. During unmanned operation, avoid use of organic solvents having an ignition point below 70 °C. ● Beware of an ignition hazard when using flammable chemicals such as organic solvents.
Page 361 4.4 Maintenance/Check Procedure WARNING Inflammation or injury due to toxic, corrosive or stimulative solvent! When using a toxic, corrosive or stimulative solvent, be careful not to incur inflammation or injury. For details of the properties of each solvent and how to handle it, refer to Material Safety Data Sheet (MSDS).
Page 362 4.4.4 Disassemble the parts, referring to the flow cell disassembling diagram shown below. Clamp screw 1 (655-1899) Fastening screw (M3) Sleeve (L369053) Pressure withstanding cell (893-4404) Packing 7.8 × 2.4 (885-2836) Spacer 1 (890-2958) Cell window (885-2832) Cell lid (893-4409) Window support 1 (893-4427)(M11) Window support 2...
Page 363 4.4 Maintenance/Check Procedure NOTE: Window supports 1 and 2 should be tightened to torque value 5.4 N·m using a torque wrench (for bolt diameter M11). (If a torque wrench is unavailable, manually tighten the window supports as far as possible, and then retighten them at an referential angle of about 45°...
Page 364 (0.25 mm I.D. × 1 inadequate. m Teflon tube or the like) should be added. For details, contact the nearest maintenance service company authorized by Hitachi High-Technologies. 4) Impurities are Check the solvent. Purify or replace the contained in solvent.
Page 365 4.5 Troubleshooting (cont’d) Symptom Cause Judgment/Check Remedy 5. Leak error occurs. 1) Liquid has Visual check Wipe off the liquid that has leaked. leaked in drain receiver. Wipe off the liquid that has adhered to leak sensor. 2) “Contaminant” Visual check Wipe off “contaminant”...
Page 366 2) Confirm proper mounting of the flow cell, and then turn on power supply again. 3) Contact the maintenance service company authorized by Hitachi High-Technologies. WL MOTOR DRIVE DRIVER Motor driver for 1) Turn on power supply again. ERROR wavelength is faulty.
Page 367 UTILITY function. PRESS “CL” KEY TO TURN because cooling fan has 2) Contact the maintenance service stopped. company authorized by Hitachi High-Technologies. LAMP OFF BY EXTERNAL Lamp goes off in 1) Press the CL key and light the...
Page 368 5. REPLACEMENT PARTS 5.1 Replacement Parts and Consumables The following table lists the replacement parts and consumables used in this instrument. The majority of these parts (such as lamps) have a lifetime which varies significantly with usage of the instrument. The service life of each part is based on the assumption that the instrument operates 160 hours/month (8 hours/day), 1920 hours/year (240 days).
Page 369 M790019 Screw S (SUS) 9600 hours/5 years Example use: Connecting pipe L329109 Ferrule (SUS) 9600 hours/5 years Example use: Connecting pipe Only the maintenance service company authorized by Hitachi High-Technologies is allowed to replace this item. 5 - 2...
Page 370 5.2 Lamp Replacement WARNING Electric shock due to contact with inside of instrument! Be sure to turn off the power switch and unplug the power cord from the wall receptacle before detaching the light source cover for lamp replacement. WARNING Prohibition of releasing the safety mechanism! In this instrument, the safety mechanism functions to turn off power supply automatically when detaching the lamp...
Page 371 5.2 Lamp Replacement 5.2.1 Replacement of D Lamp Part and Tools to be Prepared • New D lamp • Phillips screwdriver • Blade-edged screwdriver Check the following. • The power switch of this instrument is turned off. • The power cord is unplugged from the instrument. How to Replace D Lamp (a) Detach the lamp cover (by removing 2 fastening...
Page 372 5.2.1 (c) Loosen three screws of the D lamp cover and separate this cover (remove lead wires one by one through the cover). Cover Fastening screw (d) Loosen the 3 screws fastening the D lamp by turning each screw 2 revolutions with a blade-edged screwdriver.
Page 373 5.2 Lamp Replacement (g) Pass the lead wires (one by one) through the cover holes. Then, attach the cover. Cover Fastening screw (h) Connect the lead wires to the terminal block. R terminal B1 terminal B2 terminal Attach the lamp cover at the original position. Fastening screw 5 - 6...
Page 374 5.2.1 Operation Check Plug the power cord into the instrument and turn on the power switch. Make sure the lamp comes on. NOTE: The D lamp does not come on if it has been mounted improperly. On the monitor screen 2, check the wavelength (WL) and reference energy (REF), and write down their values as a record of the D lamp after use.
Page 375 5.2 Lamp Replacement (e) Key in the date of replacement in the format of month- day-year. For instance, if the lamp is replaced on March 1, 2010, key in the date as shown below. [3] → [ENT] → [1] → [ENT] → [2][0][1][0] → [ENT] Thus, the date of lamp replacement is stored in memory.
Page 376 5.2.2 (b) Remove the connector hook from the W lamp lead wire. Connector hook W lamp cover W lamp lead wire <Enlarged view> Pull down while pressing (c) Remove two W lamp cover fastening screws and detach the W lamp cover. Fastening screw (2 pcs) W lamp cover...
Page 377 5.2 Lamp Replacement (d) Pull out the W lamp and replace it with a new one (avoid loosening the screws). W lamp W lamp cover (e) Attach the W lamp cover at the original position. (f) Reconnect the connector hook of the W lamp lead wire. (g) Attach the lamp cover at the original position (by tightening 2 fastening screws).
Page 378 5.2.2 Check the energy of W lamp. (Refer to 4.4.1.) Input the date of W lamp replacement as follows. (a) Press the (GLP) key, and the following screen will appear. GLP (LOGBOOK=1, KEY LOCK=2, D2 CHECK=3, W CHECK=4, Hg CHECK=5) (b) Press [numerical] key [1], and then the [ENT] key.
Page 379 5.2 Lamp Replacement 5.2.3 Replacement of Hg Lamp Part and Tool to be Prepared • New Hg lamp • Phillips screwdriver Check the following. • The power switch of this instrument is turned off. • The power cord is unplugged from the instrument. How to Replace Hg Lamp (a) Detach the lamp cover (by removing 2 fastening screws), and then separate the Hg lamp cover (by...
Page 380 5.2.2 (c) Remove the Hg lamp. Hg lamp (d) Fit a new Hg lamp and insert it into the instrument. (e) Attach the Hg lamp cover at the original position. In succession, attach the lamp cover at the original position. Check the wavelength accuracy of Hg lamp, referring to 4.4.1.
Page 381 5.2 Lamp Replacement Key in the date of replacement in the format of month- day-year. For instance, if the lamp is replaced on March 1, 2010, key in the date as shown below. [3] → [ENT] → [1] → [ENT] → [2][0][1][0] → [ENT] Thus, the date of lamp replacement is stored in memory.
Page 382 6. INDEX 2-wavelength measurement..........2-5, 4-3 Auto Zero ................2-2, 3-8 Background spectrum ............3-30 Baseline ................... 4-2 CL..................... 2-3 Cabling ................... 1-13 Characteristics of organic solvents ........3-53 Check against packing list ........APPENDIX1-8 Checking and cleaning of flow cell ......... 4-12 Confirmation of basic actions ...........
Page 383 Hold..................3-39 INSERT ..................2-3 Installation .............. APPENDIX1-1 Installation conditions..........APPENDIX1-1 LAMP ..................3-3 LCD ..................3-47 LED ..................2-1 LOGBOOK ................3-21 Measurement of wavelength accuracy........4-10 Measuring wavelength ............. 3-8 Noise ..................2-8 OFFSET ................. 3-10 Operation ................. 3-1 POLARITY ................
Page 384 Replacement of Hg Lamp ............5-12 Replacement of W Lamp............5-8 Replacement parts ..............5-1 Replacement parts and consumables........5-1 Sample treatment..............3-63 Selection of mobile phase ............3-49 Setting of time program............3-38 Shutdown ................. 3-9 Specifications ................2-6 Time constant.................
Page 385 If relocation of the instrument becomes necessary after delivery, consult your dealer or nearest Hitachi High- Technologies service representative in order to avoid possible trouble involved in relocation. 2. Place for Installation For installation of the instrument, select a place which meets the following conditions.
Page 386 Atmospheric gas (a) Adequate ventilation is required. (b) The room shall not be filled with highly corrosive gas of acid or alkali. (c) The room shall not be filled with gas of an organic solvent (particularly, benzine and paint thinner) which dissolves coating.
Page 387 3. Items to be Prepared by Customer 3.1 Power Supply Arrangement Power supply voltage: 100 to 115 V AC/220 to 240 V AC Fluctuation shall be ±10% of the rated voltage. Frequency: 50 or 60 Hz Fluctuation shall be ±0.5 Hz of the rated frequency. Power capacity: 100 VA or more for this detector alone, 600 VA or more for the total system...
Page 388 WARNING Electric shock due to improper grounding! This instrument is designed to meet the basic insulation stipulated in the international standard IE C61010-1. To prevent an electric shock hazard due to improper grounding, provide a proper grounding connection. Be sure to use the grounded 3P power cable, which is supplied as a standard accessory for the instrument.
Page 389 (a) Usual Grounding Connection (with grounded 3P power outlet) Grounded 3P power outlet (15 A) Grounded 3P table tap Chromaster 5420 UV-VIS detector Ground resistance 750 mm or 100 Ω or less Organizer or more below AC adapter (option) ground Connector Rear panel Grounding electrode...
Page 390 (b) Connection when Grounded Power Outlet is Unavailable 2P power outlet (15 A) 3P table tap with grounding wire Chromaster 5420 UV-VIS detector Grounding terminal 750 mm or Ground more below Organizer or resistance ground AC adapter (option) 100 Ω or less Connecto Grounding wire (green) Rear panel...
Page 391 3.2 Installation Space For composing a liquid chromatograph system with the Chromaster series module units, a space of 540 mm wide (980 mm for stacking the units in two blocks) and 550 mm deep is required at least. Behind each unit, a space of 150 mm or more must be secured.
Page 392 4. Check against Packing List Check the delivered items against the packing list. 5. Assembling NOTE: It is not permitted for the user to carry out installation at the time of delivery. For ensuring safety and high accuracy in operation of the instrument, installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its...
Page 393 Reattach all two handle screws at the original positions D. Appended Fig. 1-3 Bottom Panel of Detector NOTE: If the screws are not set at the positions A and C after transport, baseline noise and baseline drift might increase. Appended Fig. 1-4 Front Panel of Detector APPENDIX 1 - 9...
Page 394 5.2 System Power Supply For the Chromaster series, the organizer unit has been prepared. To the organizer (available at option), one Chromaster 5110 pump, one Chromaster 5210 autosampler, one Chromaster 5410/5420/5430/5450 detector and one IFC board can be connected. For the Chromaster 5310 column oven and Chromaster 5440 fluorescence detector, the power cord needs to be connected to the column oven unit.
Page 395 Isocratic System/Low-pressure Gradient System (stacked in one block) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump To AC power supply Appended Fig. 1-6 Power Cable Connection Diagram Appended Table 1-1 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer) Connector cable 2)
Page 396 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5440 fluorescence detector To AC power supply Chromaster 5310 column oven Chromaster 5210 autosampler Interface control Chromaster board 5110 pump Appended Fig. 1-7 Power Cable Connection Diagram Appended Table 1-2 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer)
Page 397 5.3 System Cabling In the Chromaster series, the module units are cabled by plugging the e-Line cable into the e-Line connector at the rear left of each unit. e-Line connector Rear panel of module unit Power connector Isocratic System/Low-pressure Gradient System Chromaster organizer e-Line cable 1)
Page 398 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/ e-Line cable 1) 5420/5430/5450 detector e-Line cable 2) Chromaster 5440 fluorescence detector Chromaster 5310 column oven Chromaster organizer Chromaster 5210 autosampler Chromaster Interface control 5110 pump board Appended Fig. 1-9 e-Line Cable Connection Appended Table 1-4 Cables to be Used e-Line cable 1) (50 cm) P/N 890-6105 (attached to each unit)
Page 399 5.4 System Tubing In the Chromaster series, the inlet tube up to the pump and drain tube are fastened to the right/left side face of each unit with tube clamps. And the tubes are connected from the pump to the autosampler, column and detector through the central hole of each module unit.
Page 400 Chromaster 5440 fluorescence detector Detector cell Mobile- phase Chromaster 5310 liquid Detergent column oven Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump Degassing unit Drain Appended Fig. 1-11 Tubing Diagram of Isocratic System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to the IN port of degassing unit.
Page 401 Low-pressure Gradient System Detergent Mobile-phase liquid Chromaster organizer Chromaster 5410/5420/ 5430 detector Chromaster 5310 Injection valve column oven Syringe valve Chromaster 5210 autosampler Wash pump Low-pressure gradient unit/ proportioning valve Chromaster 5110 pump Degassing unit Drain Appended Fig. 1-12 Tubing Diagram of Low-Pressure Gradient System (stacked in one block) APPENDIX 1 - 17...
Page 402 Chromaster 5440 fluorescence detector Detector cell Mobile-phase liquid Detergent Chromaster 5310 column oven Mixer Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump 4-way joint Degassing unit Proportioning Drain valve Appended Fig. 1-13 Tubing Diagram of Low-Pressure Gradient System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to...
Page 403 Drain Tubing Drain tube A1 Chromaster organizer Chromaster 5410/5420/ T-joint 5430/5450 detector Chromaster 5310 column oven Drain tube A2 Chromaster 5210 autosampler Drain tube 4 Chromaster 5110 T-joint N1 pump Drain tube B1 Drain tube L-joint Appended Fig. 1-14 Tubing Diagram for Drain (when stacking module units in one block) Appended Table 1-5 Drain Tubes to be Used Drain tube A2...
Page 404 Chromaster 5440 fluorescence detector T-joint Drain tube A1*3 Chromaster Chromaster 5310 organizer column oven Drain tube B1 Chromaster 5210 Drain tube *2 autosampler T-joint N1 Drain tube A1*1 Chromaster 5110 I-joint pump L-joint Drain tube A1*2 Drain tube *1 Appended Fig. 1-15 Tubing Diagram for Drain (when stacking module units in two blocks) Appended Table 1-6 Drain Tubes to be Used...
Page 405 5.5 GUI Controller The GUI controller is a touch panel type operation panel. This operation panel alone enables the user to control the respective modules. For operation, refer to the instruction manual of the GUI controller. 5.6 Fastening between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips...
Page 407 APPENDIX 2. EXPLANATION OF CONTACT SIGNALS 1. Introduction The following two types of contact signals are used in the Chromaster series. Contact Signals (START, ERROR, BUSY) Entering the e- Line Connector These are contact signals having input/output functions that are used in common for respective units. The contact signals are composed of START (IN/OUT), ERROR (IN/OUT) and BUSY (IN/OUT) lines.
Page 408 Connection with L-2000 Series Connect 3-pin connectors of e-DIO cable (890-6145) as shown below. START START STOP ERROR BUSY BUSY To L-2000 series To Chromaster unit series unit e-Line e-Line connector connector 3-pin connector e-DIO cable e-DIO cable (890-6145) (890-6145) Connection with D-2500 For connection, use the e-DIO cable (890-6146).
Page 409 3. Individual Contacts of Each Unit Contact Input Terminals These are contact signal input terminals for control using contact signals from an external switch, relay, etc. Any of the signals is activated by shorting the terminal for 0.1 second or longer. The input circuit is shown in Appended Fig.
Page 410 +5 V 320 Ω Max. 10 mA Chromaster series External unit Activated upon shorting contacts of external unit Appended Fig. 2-3 Contact Signal Input Circuit 0.1 A max. 30 V max. Chromaster series External unit Appended Fig. 2-4 Contact Signal Output Circuit APPENDIX 2 - 4...
Page 411 Appendix 3. TERMINOLOGY lamp .......... A deuterium discharge lamp. This lamp emits an intense UV beam. e-Line..........A digital network cable exclusive for analysis, which is used for connecting the Chromaster series units. GLP ..........A function for checking the conditions of instrument. Hg lamp .........
Page 412 Slit..........A device for restricting the passage of beam so that the necessary component alone can pass through it. Time program ........ A program to be generated for changing measurement parameters such as detection wavelength with the lapse of measurement time. Half mirror........
Page 413 • Keep this manual in a safe place nearby so it can be referred to whenever needed. 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 3rd Edition, June 2011 Copyright C Hitachi High-Technologies Corporation 2011. 1st Edition, 2011 All rights reserved. Printed in Japan. Part No. 892-9720-2 HH-R (FT-HMS)
Page 414 NOTICE: 1. The Information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Technologies Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Technologies Corporation.
Page 415 PREFACE Thank you very much for purchasing Chromaster 5440 FL Detector. The Chromaster 5440 FL Detector is specifically designed for fluorescence detection of sample components in a liquid chromatograph system. Note that physiologically or biologically active samples are not applicable to the Chromaster 5440 FL Detector because of possible infection with bacteria or viruses.
Page 416 ABOUT THIS MANUAL This instruction manual describe how to use and maintain the Chromaster 5440 FL Detector. This instruction manual. consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 OVERVIEW (Basic Operation) Section 2 FUNCTIONS (Name and Function of Each Part on FL detector) Section 3 OPERATION (Basic Operation) Section 4 MAINTENANCE &...
Page 417 IMPORTANT Warranty on Product Limited Warranty The Chromaster 5440 FL Detector is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 418 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 419 (m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Technologies shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 420 (b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 421 In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 422 Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 423 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 424 Do not perform any operation or action other than described in these manuals. • On occurrence of any trouble in the instrument, notify the nearest sales service representative of Hitachi High-Technologies. • 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.
Page 425 Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Technologies. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 426 SAFETY SUMMARY WARNING precautions in the Manual WARNING 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 (Section 3.6, 4.4) • Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 427 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Electric Shock due to Contact with Inside of Instrument When removing the pump cover for part replacement, etc., there is a risk of electric shock. Be sure to turn OFF the power switch and disconnect the power cord from the receptacle in advance.
Page 428 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Injury due to Xenon Lamp Explosion [In use] • When the cumulative turn-on time of the xenon lamp exceeds the guaranteed useful lifetime, the electrodes evaporate and the scattered matter sticks to the bulb wall, so its blackening progresses and heat dissipation is hindered.
Page 429 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Injury due to Xenon Lamp Explosion [At mounting] (Continued) • Do not touch the quartz glass part of the xenon lamp with bare hands. If the quartz glass part of the xenon lamp is contaminated with dust or fingerprints, wipe it using a gauze sheet or absorbent cotton cloth slightly moistened with high-quality alcohol.
Page 430 SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Touching Hot Part Could Result in Burns The light source lamp and its cover become hot during operation and remain hot for a while even after power-off. They can severely burn you if touched. Before replacement of the lamp, turn power off and wait for about 30 minutes until it cools down sufficiently.
Page 431 If any one of the warning labels becomes illegible due to deterioration, contact your local Hitachi High-Technologies Corporation sales representative or service office of Hitachi High-Technologies Corporation sales representative for replacement with a new one.
Page 432 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument (2) Explosion of Vapor from Flammable (3) Electric Shock due to Contact with Light Chemicals Source Power Supply Front View (5) Explosion of Xenon (4) Ignition of Flammable Chemicals (6) Burns due to Contact with Hot Part SAFETY - 9...
Page 433 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument (7) Before Turning on Xenon Lamp Front View SAFETY - 10...
Page 434 SAFETY SUMMARY NOTICE precautions Precautions on Use of Solvents • Fluororesin, PEEK, quartz and SUS316 materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials. • This instrument has internal parts made of materials that could be corroded by strongly acidic solutions, strongly alkaline solutions or organic solvents.
Page 435 SAFETY SUMMARY NOTICE precaution (Continued) Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally. If necessary, conduct measurement on a control sample. Possible Carryover When examining the results of measurements, take account of the possibility of occurrence of a carryover.
Page 436 CONTENTS PREFACE.......................1 ABOUT THIS MANUAL..................2 IMPORTANT..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users....IMPORTANT-4 Estimated Life time of the Instrument........IMPORTANT-4 Caution on Disposal of Instrument .........IMPORTANT-5 Disposal of This Instrument and Its Parts ......IMPORTANT-5 Precautions on CE Conformity Marking .........IMPORTANT-5 Information for Users on WEEE (only for EU Countries) ..IMPORTANT-6 Other Precautions..............IMPORTANT-6...
Page 437 3.1.4 Wavelength setting ................3-6 3.1.5 Shutdown procedure ................. 3-7 3.1.6 Flushing the flow cell after use ............3-7 UTLTY Setting....................3-8 3.2.1 Offset setting ..................3-8 3.2.2 Time constant setting ................ 3-9 3.2.3 Use time program setting ..............3-10 3.2.4 PMT voltage setting................
Page 438 4.2.3 Sensitivity check ................4-2 4.2.4 Wavelength accuracy check and calibration ........4-15 4.2.5 Leak sensor check ................4-18 4.2.6 Drain tray check ................4-20 Periodic Checks .................... 4-21 4.3.1 Xe lamp energy check ............... 4-21 4.3.2 Wavelength accuracy check using Hg lamp........4-21 4.3.3 Lamp logbook check .................
Page 439: Outline
1. OUTLINE The liquid chromatograph system consists of a pump for feeding a mobile phase, a sample introducing section (autosampler, manual injector) for injecting a sample, a column for chromatographic separation of the injected sample, a column oven for maintaining the column at a constant temperature, and a detector section for detecting a signal of a separated component of the sample.
Page 440: Low-Pressure Gradient System
Each component separated from the sample is then detected as a signal by the detector. 1.2 Low-Pressure Gradient System In the low-pressure gradient system, two or more solvents are mixed in its low-pressure section from which a liquid feed is performed by a single pump.
Page 441: Functions
2. FUNCTIONS 2.1 Name and Function of Each Part on FL detector Power switch Right door UI pad Left door Fig. 2-1 Front Panel 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.
Page 442 LAMP OFF IN e-Line AUTO ZERO IN Analog signal output unit (option) Power source connector Ground terminal Fig. 2-2 Rear Panel Analog signal output unit (Option) :Provides PROCESSOR, RECORDER, MAKER IN terminal. Ground terminal :The terminals for grounding connection (three terminals). Power source connector :Connects the power supply cable.
Page 443: Name And Function Of Each Part On Ui Pad (Option)
Indication Function Remarks MARKER IN The marker function is activated by The marker function is started (option) means of contact signal input. when the short-circuit signal of more than one second is input. RECORDER Analog output for recorder The florescence intensity value (option) data is output.
Page 444 Table 2-3 Key Functions Indication Function Remarks Sets display and output to zero at each measuring wavelength. (Auto zero) Used to set each measuring wavelength. (Wavelength) (1) Sets offset value, time constant, etc (UTILTY). SET UP (2) Sets digital communication channel via the e-Line, UTILTY LCD contrast, and constant temperature flow cell (SET Keep pressing...
Page 445 Indication Function Remarks RECORD Used to specify the recorder full-scale range, recorder output speed, and output data. (Record) SPECT Obtains spectrum over a specified wavelength range and stores the spectrum in memory. (Spectrum) MARKER Places a marker on the recording. (Marker) LOCK OFF (1) Used to return from data input mode to the monitor...
Page 446: Description Of Fluorometry
2.3 Description of Fluorometry 2.3.1 Principle of fluorometry Excitation Fluorescence or Phosphorescence Stable condition Unstable condition (Ground state) (Excited state) Radiationless Radiationless transition transition Excited state V = Excited triplet state Light Light Excitation light Ground state V = Absorption Fluorescence Phosphorescence Fig.
Page 447 When light strikes an organic molecule in the ground state, it absorbs radiation of specific wavelengths and several excited states are populated. A part of the excitation (absorbed) energy is lost in vibrational relaxation, i.e. radiationless transition to the lowest vibrational level in the excited state. The molecule can return to the ground state by;...
Page 448: Advantages Of Fluorometry
2.3.2 Advantages of fluorometry For verifying the advantage of fluorometry, the limitation of absorbance measurement in its application to low-concentration samples is explained first. In this discussion, we will consider the detection of a sample that has a transmittance of 99% (relative to the blank). If we assume that the inaccuracy of the % transmittance measurement is 0.1%, the reliability of the observed data is as follows: 100.0 ±...
Page 449 A graphical description of why fluorescence can provide better sensitivity than absorbance is presented in Fig. 3-5. In this figure, the signal I is used to represent the difference between the intensity of the incident beam I and the intensity of the transmitted beam I in absorptiometry.
Page 450 In contrast, if the fluorescence spectra do not overlap (Fig. 3-6 (b)), quantitative analysis of each compound can be made by selecting the appropriate fluorescence emission wavelength (even if the absorption wavelengths of two components are the same). Absorption spectra Excitation spectra Fluorescence spectra Component A...
Page 451: Notes On Fluorescence Analysis
2.3.3 Notes on fluorescence analysis Raman Scattering When fluorescence is measured, two additional peaks may appear in the spectrum. The Rayleigh peak appears at the excitation wavelength and is due to scattered light, while the Raman peak appears at longer wavelength than the excitation.
Page 452 Raman scattering (nm) Excitation wavelength Fig. 2-7 Raman Spectrum of Water Notes on Handling Samples that Contain a High Concentration of the Compound of Interest When the concentration of the compound of interest is relatively high, various error factors will arise. The greatest factor is that the excitation beam is substantially absorbed near the entrance slit of a cell and it cannot reach the cell center adequately.
Page 453 If emission occurs only in the entrance area for excitation beam, such a sample needs to be diluted with an appropriate factor before measurement. The second factor is called “concentration quenching” where activity is disturbed by interaction of molecules. Another potential error that may occur when fluorescence detection is used is the re-absorption of fluorescence (self- absorption of fluorescence).
Page 454 Second-order and Third-order Radiation The Raman peak is described as a cautionary item when the excitation and emission wavelengths are comparatively close to each other. Conversely, when these wavelengths are comparatively distant from each other, the analyst should be aware of the second and third-order radiation phenomenon.
Page 455 In measurement of a fluorescence spectrum, many peaks appear besides that of sample fluorescence. It is necessary to find the correct sample peak according to the explanation given above. Temperature Dependency of Fluorescence Intensity In most cases, the fluorescence intensity decreases by 1 to 2% as the temperature of sample increases by 1 °C.
Page 456: Principle Of Operation
2.3.4 Principle of operation Excitation Diffusion plate monochromator Plane mirror Sample Monitor detector Xenon lamp Measuring detector Emission monochromator Xenon lamp (Fluorescence starter monochromator) Xenon lamp Photomultiplier high ballast voltage circuit Monitor detector Sample amplifier fluorescence amplifier Operational circuit Recorder or integrator Electrical connection Optical path...
Page 457: Features Of Light Source
2.3.5 Features of light source The light source thermally dissociates ozone via the heat generated by the xenon lamp itself. This allows the use of a quartz-bulb 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...
Page 458 (10) Recorder output (Option): 10 mV Full scale. Full scale 1 to 1000 FLU (settable in steps of 1). (11) Processor output (Option): 1 V Full scale, digital by e-Line. -40 (-40 mV) to 1000(1000 mV) (12) Response: Changeable in 7 steps corresponding to time constants of 0.01 / 0.02 / 0.05 / 0.1 / 0.5 / 1.0 / 2.0 seconds.
Page 459 (19) Time program Number of programs....9 Settable time......Up to 600 minutes in increments of 0.1 minute Number of steps storable..100 steps for a total of 9 files Programmable parameters ..Measurement wavelength (Ex and Em) Baseline processing PMT gain (20) GLP support function: Lamp energy check...
Page 460 (31) Dimensions: 340(W) mm × 440(D) mm × 280(H) mm (32) Weight: Approx. 25 kg NOTE: Please contact your local Hitachi High- Technologies Corporation sales representative about a purchas of the Thermo cell. 2 - 20...
Page 461: Operation
3. OPERATION The method of FL detector operation using the optional UI pad is described here. CAUTION Fatigue due to Long-Hour Operation If you keep working with the display monitor and keyboard for long hours, your eyes and body will be fatigued to jeopardize your health.
Page 462 * The current channel setting LED and the Xe LAMP LED will light in blue. <Initial screen> FL Detector 8928148-00 © Hitachi High-Technologies Corp.2010 ↓ <Initializing screen> WL DRIVE & LAMP INITIALIZING The sequence of wavelength drive (check of reference point for drive), lighting of the lamp and auto zeroing is performed.
Page 463 The 1st monitor screen (FL indication) TIME PROG LAMP Status Elapsed Program indicator time number Lamp Excitation indicator Fluorescence wavelength Emission intensity wavelength key or key, key or ESC key The 2nd monitor screen (energy indication) MONITOR (Ex) (Em) CELL ****** ****** Thermo cell indication...
Page 464: Parameter Setting
Turn off the power switch of the detector. 3.1.2 Parameter setting For entering a value, press numeric key, then ENT (enter) key. (a) Single numeric input Parameter name Input range PROGRAM NO.(1 – 9) Input part (b) Plural numeric input Input item Parameter name LAMP CHANGE...
Page 465 Input procedure The cursor is indicated on the front line of the input part. Currently set values are indicated in the input part. (ii) Numeric keys and decimal points (.) are accepted by the upper limit. (iii) Numeric inputs are accepted by the ENT key, and moves to the next item.
Page 466: Auto Zero Adjustment
The UI pad operation is disabled when connecting with the chromato data station or the GUI controller (option). 3.1.3 Auto Zero adjustment The output value should be zeroed when zero point adjustment is required or when the data baseline deviates from the recorder zero point.
Page 467: Shutdown Procedure
Then, the cursor moves to Em. Set an emission wavelength (Em). <Em wavelength setting screen> (250 - 900.0) nm Press numeric keys ((2 5 0 to 9 0 0)) and then the ENT key. * This wavelength is settable within a range from 250 to 900 nm in increments of 1 nm.
Page 468: Utlty Setting
3.2 UTLTY Setting The UTILITY key sets the following conditions. • OFFSET • TIME CONSTANT • USE PROG (whether to use time program or not) • PMT VOLT (photomultiplier voltage) • OTHERS 3.2.1 Offset setting The OFFSET is a set input signal amount that is added to the actually measured value for output.
Page 469: Time Constant Setting
♦ Typically, the negative input limit 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. 3-2 (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 Fig.
Page 470: Use Time Program Setting
Select TIME CONSTANT. Press numeric key 2 and then the ENT key. The following display will be presented. <Time constant setting screen> TIME CONSTANT (0.01s=1, 0.02s=2, 0.05s=3, 0.1s=4, 0.5s=5, 1.0s=6, 2.0s=7) Set a time constant value. Press numeric key (1 to 7, usually input 4) and then the ENT key.
Page 471: Pmt Voltage Setting
Select use (YES=1) or non-use (NO=0) of a time program. Press a numeric key (1 or 0) and then the ENT key. * 1: Time program starts by start input. 0: Time program does not start despite start input. * Default value: 1 Selection or avoidance of a time program is now completed and the 1 monitor screen returns.
Page 472: Other Settings
Set a photomultiplier voltage. Press numeric key (1 to 5, usually input 3) and then the ENT key. * Default value: 3 Photomultiplier voltage setting is now completed and the 1 monitor screen returns. 3.2.5 Other settings Set the following items. •...
Page 473 (d) The following display will be presented. <Em bandwidth selecting screen> Em BANDWIDTH (STANDARD=1, WIDE=2) Set an Em bandwidth value. Press numeric key (1 or 2, usually input 1) and then the ENT key. * Default value: 1 (e) Em bandwidth setting is now completed and the 1 monitor screen returns.
Page 474 (c) The following display will be presented. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Select ERROR OUT. Press numeric key 2 and then the ENT key. (d) The following display will be presented. <Error out signal selecting screen> ERROR OUT SIGNAL (DISABLE=0, ENABLE=1) Invalid (0) or valid (1) status of error out signal output is settable.
Page 475 (c) The following display will be presented. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Select LEAK SENSOR. Press numeric key 3 and then the ENT key. (d) The following display will be presented. <Leak sensor selecting screen> LEAK SENSOR (OFF=0, ON=1) Select use (ON=1) or non-use (OFF=0) of the leak sensor.
Page 476 Select OTHERS. Press numeric key 5 and then the ENT key. (c) The following display will be presented. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Select LAMP. Press numeric key 4 and then the ENT key. (d) The following display will be presented.
Page 477: Glp Functions
3.3 GLP Functions For this function, the following items are settable. • Xe lamp LOGBOOK data display and resetting • Hg lamp LOGBOOK data display and resetting • KEY LOCK setting • WL CHECK (wavelength accuracy check) by using Hg lamp •...
Page 478: Xe Lamp Logbook Data Resetting
The following display will be presented. <Logbook selecting screen> LOGBOOK (REPORT=1, RESET=2) Select Report. Press numeric key 1 and then the ENT key. On the logbook report screen, the total on period of the Xe lamp and its standard lifetime (in parentheses under Xe LAMP), the number of switching-on times and the date of the last lamp change will be indicated.
Page 479 The following display will be presented. <Lamp selecting screen> LAMP SELECT (Xe=1, Hg=2) Select Xe. Press numeric key 1 and then the ENT key. The following display will be presented. <Logbook selecting screen> LOGBOOK (REPORT=1, RESET=2) Select RESET. Press numeric key 2 and then the ENT key. Next, advance to the Xe lamp change date setting screen for setting the date of xenon lamp change.
Page 480: Hg Lamp Logbook Data Display
(c) Input a year for YYYY. <Xe lamp change date setting screen (year)> Xe LAMP CHANGE YYYY) <1-31> 2010 Press numeric keys (2 0 0 0 to 2 1 0 0) and then the ENT key. * Even when the same year as desired is indicated, its numeral must be input again without fail.
Page 481: Hg Lamp Logbook Data Resetting
The following display will be presented. <Logbook selecting screen> LOGBOOK（REPORT=1, RESET=2） Select Report. Press numeric key 1 and then ENT key. On the logbook report screen, the total ON period of the Hg lamp, the number of switching-on times and the date of the last lamp change will be indicated.
Page 482 Select Hg. Press numeric key 2 and then ENT key. The following display will be presented. <Logbook selecting screen> LOGBOOK（REPORT=1, RESET=2） Select RESET. Press numeric key 2 and then ENT key. Next, advance to the Hg lamp change date setting screen for setting the date of mercury lamp change.
Page 483: Key Lock Setting
* Even when the same year as desired is indicated, its numeral must be input again without fail. Logbook setting is now completed and the 1st monitor screen returns. * When a mercury lamp change date is set, the total ON period of the Hg lamp and the number of switching-on times will be automatically reset accordingly.
Page 484: Wavelength Accuracy Check By Using Hg Lamp
3.3.6 Wavelength accuracy check by using Hg lamp Whether wavelength is normal or not can be checked by using the 254 nm bright line of mercury lamp. Press the key. The following display will be presented. <GLP initial screen> (LOGBOOK=1, KEY LOCK=2, WL CHECK=3, Xe CHECK=4) Select WL CHECK.
Page 485: Xe Lamp Energy Check
* 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 1 monitor screen. The result of emission wavelength (Em) check will now be displayed.
Page 486 <Xe lamp energy check screen> (energy check is in progress) CHECKING LAMP ENERGY (Xe) The result of Xe lamp energy check will be displayed 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.
Page 487: Operating Instructions
3.4 Operating Instructions 3.4.1 Time program setting A time program is used for automatic change of the chromatograph measurement conditions with time. The time program takes priority over other settings. The following items can be set. • Measurement time (TIME) •...
Page 488 PROG Press the key. The time program No. setting screen appears. <Time program No. setting screen> SET PROGRAM NO. (1-9) Press a numeric key 1 to 9 and then the ENT key to create or change the program No., or select the existing program * Initial (default) value: 1 * If the setting will not be changed, press the ESC key to return to the 1st monitor screen.
Page 489 Setting of first step (start conditions) of time program: (a) Set the TIME. <Step setting screen (TIME indicated)> TIME BASE _ 0.0 Press numeric keys 0.0 and then the ENT key. * Be sure to enter “0.0” for TIME. * Initial (default) value: 0.0 * The program No.
Page 490 Press numeric keys 2 5 0 to 9 0 0 and then the ENT key. * Setting range: 250 to 900 nm It is recommended to set the same wavelength as was set for Em of the measuring wavelengths. * Initial (default) value: blank The cursor next moves to BASE.
Page 491 Setting of second and subsequent steps of time program: (a) Set the TIME to be changed. <Step setting screen (TIME indicated)> TIME BASE _ 10.0 Press numeric keys 0 to 6 0 0 and then the ENT key. * Setting range: 0 to 600 minutes, in increments of 0.1 minute The cursor now moves to Ex.
Page 492 (d) Set the BASE (baseline processing) to be changed. <Step setting screen (BASE indicated)> TIME BASE 10.0 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 the one in the previous step.
Page 493: Time Program Starting
(b) When the time program settings are completed, the 1 monitor screen reappears. 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.
Page 494 HOLD Auto zero START STOP TIME (minutes) 10.0 20.0 Ex (nm) Em (nm) HOLD Described here is an example of newly setting a time program at program No. 1. Ten minutes after the start (1), photomultiplier voltage is changed from MID to LOW, excitation wavelength from 250 to 270 nm, emission wavelength from 350 to 370 nm, and hold function is applied, then measurement is completed after 20 minutes...
Page 495 PROG Press key. ↓ SET PROGE NO. (1 - 9) Press 1 key and then the ENT key. ↓ EDIT MODE (MODIFY=0, NEW=1) Press 1 key and then the ENT key. ↓ TIME BASE Press 0 key and then the ENT key. Press 2 5 0 keys and then the ENT key.
Page 496 Check of time program Take the following procedure for checking the program that was set in the above. Press the key. ↓ SET PROGE NO. (1 - 9) Press 1 key and then the ENT key. ↓ EDIT MODE (MODIFY=0, NEW=1) Press 0 key and then the ENT key.
Page 497: Spectrum Measurement
3.4.5 Spectrum measurement Set the wavelength scan range (maximum and minimum values) for excitation (Ex) and emission (Em), then measure and record the spectral data for each. * Carry out recording of spectral data with sample contained in the cell (sample not flowing, but stationary in cell). The spectral bandwidth is 15 nm on both excitation and NOTE: emission sides (bottom width of peak is about 30 nm).
Page 498 <Scan range setting screen (indicate WL1)> SCANNING WL RANG (WL1 WL2) nm FL (Ex) <200-800> 200 - 600 Press numeric keys 2 0 0 to 8 0 0 and then the ENT key. * Setting range : 200 to 800 nm * Initial (default) value : 200 * If setting will not be changed, press key to...
Page 499 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 the ESC key during spectral acquisition will cancel the process.
Page 500 Press numeric keys 2 5 0 to 8 5 0 and then the ENT key. * Setting range : 250 to 850 nm * Initial (default) value : 250 * If setting will not be changed, press key to proceed to WL2 setting. The cursor now moves to WL2.
Page 501: Recorder And Spectrum Output Factors Setting
* Pressing the ESC key during spectral acquisition will cancel the process. Spectral data will not be memorized. * The memorize spectrum No. set in the preceding step will be indicated at SCANNING SPECTRUM * Em is effective within the scan range set above. (g) When the spectral data memorization is completed, the system returns to the 1 monitor screen automatically.
Page 502 Full Scale Range of Recorder (a) Press the RECORD key. (b) The recorder setting screen appears. <Recorder setting screen> RECORD (RCD RANGE=1, RCD SPEED=2, SPECT RCD=3) Press numeric key 1 and then the ENT key to select RCD RANGE (recorder range). (c) The recorder full scale range setting screen appears.
Page 503 (c) The recorder speed setting screen appears. <Recorder speed setting screen> RCD SPEED (40 nm/min=1, 60 nm/min=2) Press numeric key 1 or 2 and then the ENT key to set a recorder speed. * Initial (default) value: 2 (d) When the setting of recorder output speed is finished, the system returns to the 1 monitor screen.
Page 504 <Background spectrum No. setting screen> BACKGROUND SPECTRUM NO. (0 ~ 4) Press a numeric key 0 to 4 and then the ENT key to select whether or not to correct the output spectrum. : 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...
Page 505: Marker Operation
* The output spectrum No. set before will be indicated at RCD NO. (g) When the spectrum output is finished, the 1 monitor screen will return automatically. 3.4.7 Marker operation A marker line is indicated only on the recorder. It is usable as an event marker to indicate, for example, the start of measurement or the point where set conditions were changed during measurement.
Page 506: Set Up Setting
3.5 Set Up Setting Before analytical operation, communication channel (CH) and liquid crystal display contrast (LCD CONTRAST) need to be set. • This setting is not required every time. When unnecessary, skip this setting. • The default value or currently set value is indicated before your input.
Page 507: Thermo Cell Setting
Select a channel (CH). Press numeric key 1 or 2 and then the ENT key. * Default value: 1 * Two channels can be selected for two detectors. Channel setting is now completed and the setup initial screen appears. Under DETECTOR, the selected channel setting is indicated.
Page 508 The following display will be presented. <Thermo cell selecting screen> THERMO CELL (NO USE=0, USE=1) Select use (USE=1) or non-use (NO USE=0) of the thermo cell. Press a numeric key (0 or 1) and then the ENT key. * Default value: 1 * Two channels can be selected for two detectors.
Page 509: Liquid Crystal Display Contrast Setting
3.5.3 Liquid crystal display contrast setting Set a contrast (brightness) level of the LCD screen. SET UP UTLTY Turn on the power switch with the key held down. The following display will be presented. <Setup initial screen> SETUP: DETECT THERMO CONTRAST S.
Page 510: Standard Xenon Lamp Lifetime Setting
* When you press the ENT key here, the setup items selecting screen is presented to allow reentry. * The selected setting will be fetched upon turning on power supply at the next time. Turn OFF the power switch. 3.5.4 Standard xenon lamp lifetime setting WARNING Injury due to Xenon Lamp Explosion When the cumulative turn-on time of the xenon lamp exceeds...
Page 511 Select EXCHANGE STANDARD. Press numeric key 4 and then ENT key. The following display will be presented. <Standard Xe lamp lifetime setting screen> XE LAMP EXCHANGE STANDARD (1 - 2500) H _500 The standard lifetime of the Xe lamp is settable here. Press numeric key (to input 1 to 2 5 0 0) and then the ENT key.
Page 512: Before Performing Analysis
3.6 Before Performing Analysis This chapter describes the basic items to be careful about before starting analysis. WARNING 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. •...
Page 513: Selection Of Mobile Phase And Cautions On Handling
WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 514 (b) When performing analysis with a UV detector in the short wavelength range or highly sensitive analysis with an RI detector, degassing the mobile phase before use is not enough, and the baselines may be fluctuated by the bubbles. In such a case, use degassing unit which can degas mobile phase on-line.
Page 515 Table 3-1 Reagents for Mobile Phase that may be Restricted Use is Use is Possible if Use is Possible if 10% or Reagents Unsuitable for Possible 50% or Lower Lower SUS316 Phosphoric Acetic acid Disodium phosphate Ammonium chloride acid Ammonium citrate Ammonium formate Potassium chloride Sodium...
Page 516 3.6.2 Characteristics of organic solvents Characteristics of organic solvents as mobile phase for liquid chromatograph are shown in Table 4-2. Use it for reference. WARNING 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.
Page 517 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 518 Table 3-2 Characteristics of Organic Solvents Ignition Point Vapor Specific Polarity Viscosity Refractive UV Cut Flash Boiling Density Gravity (cP20 °C) Lower Upper Index off (nm) Point (°C) Point (°C) °C (Air: 1) (Water: 1) Limit Limit Fluoroalkanes -0.25 1.25 n-Pentane 0.00 0.23...
Page 519 Notes for Using Organic Solvents as Mobile Phase When using organic solvents, be careful about UV cut off wavelength. • UV cut off wavelength Light cannot be transmitted in the range shorter than this wavelength. For example: Cut off wavelength of chloroform is 245 nm. Chloroform cannot be used in the range shorter than 245 nm (e.g.
Page 520: Cautions On Static Electricity
3.6.3 Cautions on static electricity WARNING Ignition of Flammable Chemicals by Static Electricity 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 Since flammable organic solvents are used for the high speed liquid chromatograph, be careful about heat and fire.
Page 521: Preparation
3.7 Preparation When using an ultrasonic cleaner etc., follow the NOTE: instruction manual for it. 3.7.1 Degassing and removing dust from mobile phase Degas mobile phase before use without fail. Oxygen gas and nitrogen gas contained in mobile phase cause the following when used under high pressure. (a) Change in quality of mobile phase sample (b) Loss of column efficiency caused by bubbles (c) Noise of detector caused by bubbles...
Page 522 Remove cap. Mobile phase container Ultrasonic cleaner (a) Set mobile phase container well stirred into ultrasonic cleaner. * When using a mixed mobile phase, stir it completely by using a stirrer, or else low repeatability or baseline drift may be caused. NOTE: Degas mobile phase of organic solvent by using ultrasonic cleaner with water.
Page 523 Devices to be prepared • Ultrasonic cleaner (Put water in the bath without fail.) • Aspirator with rubber stopper which fits the mouth of mobile phase container Rubber stopper should fit the mouth of container. Ultrasonic cleaner Mobile phase container Aspirator (a) Set mobile phase container in ultrasonic cleaner after sufficient stirring.
Page 524: Removing Dust From Mobile Phase
(g) Shut off the city water. (h) Turn off the power of ultrasonic cleaner. Take mobile phase container out of ultrasonic cleaner, wipe the water from the container, and set it to liquid chromatograph. NOTE: Bubble generation depends on constitution of mobile phase.
Page 525: Sample Pretreatment
3.7.4 Sample pretreatment Filter samples without fail if they may contain fine dust. Dust can clog column and deteriorate it. Remove foreign matter from samples without fail. Foreign matter can lower the reliability of data, e.g. generating abnormal peaks etc. (a) Example of filtering samples Dust in sample can be removed easily as follows.
Page 526 (b) Example of Removing foreign matters in sample For example, when analysis is performed with Reversed Phase Column (e.g. ODS Column), foreign matters can be removed as follows. Take sample in Syringe, attach Normal Phase cartridge, and perform filtering. See the figure left. NOTE: There are various ways for removing foreign matters in sample.
Page 527: Maintenance And Troubleshooting
When this detector unit is used in combination with NOTE: Hitachi Chromaster control option, the lamp energy, wavelength accuracy and sensitivity can be automatically calculated. For details, refer to the instruction manual of Hitachi Chromaster control option.
Page 528: Wavelength Accuracy Check By Using Hg Lamp
4.2.2 Wavelength accuracy check by using Hg lamp Check the wavelength accuracy by using the bright line at 254 nm of the Hg lamp (see section 3.3.6). “GOOD” will appear on the display when the wavelength error is within ±3 nm, or “FAIL” will appear when the error exceeds ±3 nm.
Page 529 Chromaster 5440 Flow cell D-2500 Chromato-data processor FL Detector Distilled water Waste Chromaster 5110 solution Pump Fig. 4-1 Tubing Diagram Measurement of Raman Spectrum of Water Set the flow cell unit in place, measure the Raman spectrum of water under the conditions given below, and record the results (see sections 3.4.2, 3.4.3, 3.4.5 and 3.4.6).
Page 530 <Wavelength setting screen (Ex indicated)> (200 - 850.0) Press numeric keys 3 5 0 and then the ENT key. (ii) An emission (Em) wavelength will not be set here. Leave the present setting as it is. <Wavelength setting screen (Em indicated)> （250 - 900.0）...
Page 531 <Utility setting screen> UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, PMT VOLT=4, OTHERS=5) Press numeric key 4 and then the ENT key. The pmt voltage setting screen appears. <Pmt voltage setting screen> PMT VOLTAGE (SUPER HIGH=1, HIGH=2, MID=3, LOW=4, SUPER LOW=5) Press numeric key 3 and then the ENT key.
Page 532 The 1 monitor screen returns. (d) Setting of spectrum measurement: Press the SPECT key. The scan mode setting screen appears. <Scan mode setting screen> SPECTRUM MODE (FL (Ex)=1, FL (Em)=2) Press numeric key 2 and then the ENT key. (ii) Set a scanning range.
Page 533 <Scan monitor screen (spectrum acquisition under way)> SCANNING SPECTRUM NO.: 1 MODE: FL (Em) Ex: 350 nm Em: *** nm When the recording of spectral data finishes, the monitor screen returns automatically. (e) Setting of recorder full scale range, speed and memory No.: Press the RECORD key and the recorder setting screen appears.
Page 534 Press numeric key 2 and then the ENT key. (vi) The 1 monitor screen returns. (vii) Press the RECORD key. The recorder setting screen reappears. <Recorder setting screen> RECORD (RCD RANGE=1, RCD SPEED=2, SPECT RCD=3) Press numeric key 3 and then the ENT key. (viii) The output data spectrum No.
Page 535 (xi) The spectrum output screen appears, and spectrum output begins. <Spectrum output screen> RCD NO. SPEED MODE 1000.0 (xii) When the spectrum output is completed, the 1 monitor screen returns automatically. Set the following conditions for the D-2500 NOTE: chromato-data processor. CHART SPEED : 60 mm/min If the detector and data processor are NOTE:...
Page 536 NOTE: When the instrument is combined with Hitachi Chromaster driver for Empower™2, and Chromaster System Manager for Hitachi, the Raman signal intensity can be obtained automatically by means of the furnished maintenance software. For details refer to the instruction manual on the maintenance software.
Page 537 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 S/N ratio = S/N (baseline method, S/N ratio ≥ 700) S/N ratio = S/N (tangent method, S/N ratio ≥...
Page 538 (ii) Check the position and useful life of the xenon lamp. (b) When peak separation is not good Check the distilled water. * Distilled water should be used soon after its purification. If left for a long time in a container made of resin or the like, fluorescent substance may mix in with the distilled water.
Page 539 Create a time program as indicated below for measuring the Raman spectrum of water. TIME BASE (A/Z=1, HOLD=2) The above time program shows an NOTE: example where the minimum FL value was obtained at 380 nm and the maximum at 400 nm. For the top Em of the program, set a wavelength that includes the wavelengths where the maximum and minimum FL values were...
Page 540 Read out the value corresponding to “S” from the spectrum obtained with the time program. (tangent method) (baseline method) Baseline Tangent Fig. 4-4 Calculate the Raman Peak of Water When using the D-2500 chromato-data processor, calculation can be made using the length (L in mm) of S on the chart.
Page 541: Wavelength Accuracy Check And Calibration
Raman spectrum of Baseline (emission water wavelength 397 nm) S (tangent method) 15 minutes (baseline method) Drift: Baseline D/A x 100 ≤ 3%/15min Max. 450 nm wavelength Emission wavelengths Conditions: Excitation(Ex) wavelength ..... 350 nm Response ....... 2 seconds Flow cell......12 μL Distilled water in cell Room temperature kept constant Fig.
Page 542 (b) Check of wavelength accuracy Check the wavelength accuracy by using the bright line at 254 nm of the Hg lamp (see section 4.4.4 (6)). “GOOD” will be indicated if the wavelength error is within ±3 nm, or “FAIL” will be indicated if the error exceeds ±3 nm.
Page 543 Wavelength calibration is conducted by entering a new offset value (value to which the deviation is added). Press numeric keys (from 1 to 2 0) and then the ENT key. Input range for offset value: 1 to 20 Calculation of new offset value: New offset value = present offset value –...
Page 544: Leak Sensor Check
(iii) The 1 monitor screen appears. 4.2.5 Leak sensor check Operational Check of Leak Sensor (a) Drip water onto the leak sensor. Drip water. Leak sensor Fig. 4-6 Leak Sensor Check (b) Confirm that a leak error is detected. Specification: A leak error must be detected. NOTE: Observe the following precautions before using the leak sensor which detects a liquid leak.
Page 545 Cleaning of Liquid Leak Sensor <Item to be prepared> • Hexagonal wrench (P/N: N315003, size: B2.5) (a) Separate the liquid leak sensor from the drain tray by removing the liquid leak sensor fastening screw with the furnished hexagonal wrench. (b) Wipe off the water adhering to the liquid leak sensor and drain tray, and then fasten the sensor to the drain tray again.
Page 546: Drain Tray Check
4.2.6 Drain tray check WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 547: Periodic Checks
4.3 Periodic Checks Frequency of Check Item Check Procedure Remarks Check Drain tray Daily Check the drain tray, and wash it when needed. Lighting of lamp Daily Check that “Xe” is indicated on LEDs. Liquid leakage Daily Visually check that liquid is not leaking from the mobile phase bottle, tubing and waste bottle.
Page 548: Lamp Logbook Check
If “FAIL” is indicated, wavelength calibration is required. NOTE: Refer to section 4.2.4 (2) for the calibration. 4.3.3 Lamp logbook check The cumulative turn-on time, number of lightings, and last replacement date for the Xe and Hg lamps can be checked via the GLP function (see 3.3).
Page 549: Flow Cell Unit Checks
4.4 Flow Cell Unit Checks WARNING 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. Do not bring a heat or flame source near the instrument.
Page 550: Check And Washing Of Flow Cell
4.4.1 Check and washing of flow cell If the inside of the flow cell is contaminated, it must be cleaned. Prepare the following items for the cleaning. • Glass syringe with capacity of about 10 mL • Wash fluid Flow cell unit (P/N 893-5350) or thermostatted flow cell unit (P/N 893-5370) Retaining screw Thermostatted flow cell...
Page 551 Connect the syringe to the tip of the drain tube, and inject the wash fluid into the cell for cleaning (Fig. 5-7). This flow cell unit (P/N 890-2967) uses a part similar to NOTE: the one used in the Chromaster 5440 FL Detector. Be careful not to mount the part of the flow cell unit to the detector and vice versa.
Page 552: Disassembly And Cleaning Of Flow Cell
From the pump Fig. 4-10 Removing Air Bubbles Applying too much pressure may damage the flow cell. NOTE: Set the pressure limiter of the pump at 1.0 MPa max. before removing air bubbles. 4.4.2 Disassembly and cleaning of flow cell Disassembly of Flow Cell If contamination is not removed by just flushing the interior of the flow cell, then disassemble and clean the cell in the...
Page 553 (c) Remove the cell clamp. (d) Loosen setscrews. (e) Take out the flow cell. Cell window Flow cell clamp Flow cell Retaining screw 1 Retaining screw 2 Fig. 4-12 Disassembly of Flow Cell Unit Washing of Flow Cell (a) Wash the flow cell in running water. If the contamination cannot be removed with running water, then use an ultrasonic cleaner.
Page 554 Assembly of Flow Cell (a) Assemble the flow cell into the cell holder in the orientation shown in Fig. 4-11 and fix it with the cell clamp. (b) Tighten the upper and lower retaining screws 1 and 2. View from top Enlarged view of flow cell Polished surface (Instrument front)
Page 555: Leakage From The Flow Cell
4.4.3 Leakage from the flow cell It is important to check for any liquid leakage from the flow cell unit prior to analysis. If a leak is found, stop the pump immediately and remove the flow cell unit. Take the following procedure to remedy the leak.
Page 556: Cautions On Storage Of The Flow Cell
4.4.4 Cautions on storage of the flow cell If the flow cell will be left unused for more than a few days, clean the flow cell interior thoroughly by pumping distilled water or alcohol through it and then store it in a safe place. If the period of nonuse is less than a few days, the inside of the cell may be filled completely with a solvent such as ethanol or acetonitrile and then stored.
Page 557: Troubleshooting
4.5 Troubleshooting Symptom Cause Judgment/Check Remedy Self-diagnosis The power cord plug is Visual check Plug in the power cord (initialization) is not not securely plugged in. securely. performed when the The fuse is blown. Check the fuse for Replace the fuse with a POWER switch is continuity.
Page 558 Symptom Cause Judgment/Check Remedy ⎯ Excessive drift The warm-up period is Wait until the instrument not sufficient. becomes stable (at least 10 minutes). Mobile phase is leaking Check each fitting. Retighten the offending from a fitting. fitting. An impurity is eluting Stop feeding liquid Wait until elution is from the column.
Page 559: Error Messages
1) Press CL key, and 1st monitor PRESS “CL” KEY TO screen returns. CLEAR MESSAGE. 2) Contact your nearest service office of Hitachi High-Technologies sales representative. RAM ERROR RAM is faulty. 1) Press CL key, and 1st monitor PRESS “CL” KEY TO screen returns.
Page 560 Message Description Remedy LAMP OFF BY Lamp has been turned off due 1) Release the key lock if it has EXTERNAL ERROR to an external error. Busy been activated. PRESS “CL” KEY TO status is assumed. 2) Press CL key and light up the TURN ON.
Page 561 1) Cannot be released by key ERROR ADC initialization. operation. 2) Turn on power again. 3) Contact your nearest service office of Hitachi High-Technologies sales representative. ADC ERROR Data transfer from ADC has 1) Cannot be released by key been interrupted.
Page 562: Spare Parts
5. SPARE PARTS 5.1 Replacement Parts and Consumables Table 5-1 lists the replacement parts and consumables for this instrument. It is suggested that a suitable quantity of each item be stocked in the laboratory to minimize down time. For many of these items (e.g.
Page 563 Part Number Part Name Estimated Service Life Remarks Example use: 893-0827 Connecting pipe 9600 hours/5 years Piping between (SUS, coated) column outlet and inlet tube For standard flow cell Length 350 mm, Inner diameter : 0.25 mm, Outer diameter : 1.57 mm, Material SUS,...
Page 564: Lamp Replacement
5.2 Lamp Replacement 5.2.1 Xe lamp replacement WARNING Injury due to Xenon Lamp Explosion Before removing the xenon lamp for replacement, turn off the xenon lamp (turn off power to the instrument) and then wait for at least one hour until the xenon lamp becomes sufficiently cool to reduce its internal pressure the normal safety level.
Page 565 <Utility setting screen> UTILITY (OFFSET=1, TIME CONSTANT=2, USE PROG=3, PMT VOLT=4, OTHERS=5) Press numeric key 5 and then the ENT key. (b) The others setting screen appears. <Others setting screen> OTHERS (Em BANDWIDTH=1, ERROR OUT=2, LEAK SENSOR=3, LAMP=4) Press numeric key 4 and then the ENT key. (c) The Xe lamp setting screen appears.
Page 566 Replacement of the Xe Lamp WARNING Electric Shock due to Contact with Inside of Instrument The xenon lamp is supplied with high voltage 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.
Page 567 (c) Put on safety goggles for the subsequent steps. (d) Detach the connector between lamp house and main body, and loosen the lamp house retaining screw. Lamp house Connecter Grip Retaining screw Fig. 5-2 Removal of Connector and Retaining Screw (e) Lift the grip of the lamp house lightly and pull it toward you, then detach the lamp house from the main body.
Page 568 Anode cable Lamp igniter Cathode cable Xenon lamp Grip Fig. 5-4 Lamp House after Removal Removal of old xenon lamp WARNING Injury due to Xenon Lamp Explosion (at disposal) The xenon lamp is filled with high-pressure gas (approx. 1 MPa at room temperature, approx. 4 MPa under operating condition), and this high-pressure gas still remains in the xenon lamp after it is demounted for replacement.
Page 569 Loosen the anode nut of the lamp and detach the anode terminal of the lamp (marked +) from the metal fixture on the ceramic plate (Fig. 5-5). Be careful not to touch the lamp bulb. Note that a thin metal wire is attached near the center of the bulb, which facilitates ignition of the lamp.
Page 570 (h) Mounting of new xenon lamp WARNING Injury due to Xenon Lamp Explosion (at mounting) Do not touch the quartz glass part of the xenon lamp with bare hands. If the quartz glass part of the xenon lamp is contaminated with dust or fingerprints, wipe it using a gauze sheet or absorbent cotton cloth slightly moistened with high-quality alcohol.
Page 571 Attach a new xenon lamp in place. Attach the cathode lead plate to the threaded part of the cathode, and secure the lead plate with the cathode nut (Fig. 5-6). Mount the lamp so that the protrusion on the bulb faces the instrument front panel (Fig.
Page 572 Lamp protrusion (faces instrument front panel) Metal wire Fig. 5-7 Orientation of Lamp Bulb Protrusion As shown in Fig. 5-6, put the anode terminal (marked “+”) of the lamp into the metal fixture on the ceramic plate. Then, using the anode nut, mount the lamp so that the protrusion on the bulb is positioned as shown in Fig.
Page 573 (k) When installation of the lamp house is finished, close the light source cover and turn ON the power (check that the lamp comes on). Now proceed to positional adjustment of the Xe lamp. Positional Adjustment of Xe Lamp CAUTION Direct Gazing at Illuminating Xenon Lamp Could Cause Eye Damage The xenon lamp radiates intense ultraviolet light when it is...
Page 574 Lamp position adjustment screw cover Cover fastening screw Fig. 5-8 Lamp Position Adjustment Screw Cover HORIZONTAL VERTICAL FOCUS Fig. 5-9 Lamp Positional Adjustment (a) Coarse adjustment Set the excitation (Ex) wavelength at 550 nm, and make the adjustment while observing the image of the light beam.
Page 575 Turn ON the power switch, and the 1 monitor screen appears. <1 monitor screen> TIME PROG LAMP (ii) In the present status, pull out the flow cell unit (see Fig. 5-2). “****” will be indicated at FL on the 1 monitor screen.
Page 576 (iii) Press the WL key and the wavelength setting screen appears. Set an excitation (Ex) wavelength. <Wavelength setting screen (Ex indicated)> (200 - 850.0) Press numeric keys 5 5 0 and then the ENT key. (iv) Emission (Em) wavelength will not be set here. Leave the present setting as it is.
Page 577 Observe excitation beam on paper strip Fig. 5-10 Observation of Ex Beam (b) Fine adjustment Following the coarse adjustment, set the excitation (Ex) wavelength at 350 nm make a fine adjustment while observing the data. Take the procedure given below (refer to sections 3.1.1, 3.1.4). Re-mount the flow cell unit.
Page 578: Hg Lamp Replacement
<Wavelength setting screen (Em indicated)> (250 - 900.0) Press the ENT key. (iv) The 1 monitor screen appears. Press key and the 2 monitor screen appears. <2 monitor screen> MONITOR (Ex) (Em) LAMP ******* ******* (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...
Page 579 Retaining screws Fig. 5-11 Removal of Light Source Cover (c) Loosen the screw retaining the mercury lamp cover (Fig. 5-12). Retaining screw Hg lamp cover Fig. 5-12 Removal of Hg Lamp Cover (d) Pull the Hg lamp cover straight out, and the Hg lamp will be seen attached at the right side interior of the main body (Fig.
Page 580 (e) Detach the connector between the Hg lamp and main body, loosen two retaining screws and detach the Hg lamp. Hg lamp Connector Close-up view Retaining screws Fig. 5-13 Removal of Hg Lamp Attach a new Hg lamp in place. Fasten the lamp with the two retaining screws, then connect the connector with the main body.
Page 581: Fuse Replacement
5.3 Fuse Replacement WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure turn off the power switch and unplug the power cord before proceeding to fuse replacement.
Page 582: Index
6. INDEX Assembling ........................... 2-9 AUTO ZERO IN ........................2-2 A/Z (Auto zero) ....................... 2-4, 3-6, 4-1 Baseline..........................4-11 CL (Clear) ..........................2-5 Checking the Contents ..................APPENDIX1-6 Consumables........................5-1 DEL (Delete)........................2-5, 3-5 Drift Measurement ......................4-15 E-Line .......................... 2-2, 3-46 ENT (Enter) ..........................
Page 583 Fluorometry/Features of Light Source ................2-17 Fluorometry/Notes on Fluorescence Analysis ..............2-11 Fluorometry/Principle of Fluorometry ................... 2-6 Fluorometry/Principle of Operation..................2-16 Fluorometry/Second-order and Third-order Radiation............2-14 Fluorometry/Temperature Dependency of Fluorescence Intensity........2-15 Frequency......................APPENDIX1-2 Fuse Replacement ......................5-20 GLP ........................2-4, 3-17, 4-22 Hg Lamp/Replace.......................
Page 584 Mobile Phase/Degassing and Removing Dust ..............3-61 Mobile Phase/Selection ...................... 3-53 NOISE/Measurement ......................4-10 NOISE/Noise Calculation ....................4-10 OFFSET ..........................3-8 Operation..........................3-1 Organic Solvents ........................ 3-56 Performance/Check......................4-1 Power/Turning On the Power ....................2-1 Power/Shutdown Procedure....................3-7 Power Supply/voltage..................APPENDIX1-2 PROCESSOR (option) ......................
Page 585 TIME CONSTANT ........................ 3-8 TIME PROGRAM/Setting of Time Program ............... 3-10 Troubleshooting........................4-31 Tubing....................... APPENDIX1-12 UI Pad (option) ........................2-1 UTILTY (Utility) ........................2-4 VERTICAL .......................... 5-12 WL (Wavelength)........................2-4 Wavelength/Accuracy Checking by using Hg Lamp ............ 4-2, 4-21 Wavelength/Calibration of Wavelength Accuracy............... 4-17 Wavelength/Setting ......................
Page 586: Appendix
If relocation of the instrument becomes necessary after delivery, please be sure to consult your dealer or nearest Hitachi High-Technologies authorized maintenance service agent in order to avoid possible trouble involved in relocation. APPENDIX 1 - 1...
Page 587: Installation Conditions
2. Installation Conditions Confirm that the following requirements are satisfied before installing the instrument. Power Supply Power supply voltage : 100 to 115/220 to 240 V AC Fluctuation should be within ±10% of the rated voltage. Frequency : 50 or 60 Hz Fluctuation should be within ±0.5 Hz of the rated frequency.
Page 588 WARNING Electric shock due to improper grounding! This instrument is designed in conformity with the specifications of Class I in Annex H of the IEC 61010-1 (International Electrotechnical Commission Standards) - Issue 1. To prevent an electric shock hazard, provide a proper grounding connection.
Page 589 (b) Grounding Connection when grounded 3P power outlet not available 2P power outlet (15A) Grounded 3P table tap Power cord (standard Chromaster 5440 accessory) Ground fluorescence detector terminal 750 mm or Grounding more resistance: Connector underground 100 Ω or less Ground wire (green) Screw diameter : M4 or larger...
Page 590: Installation Place
3. Installation Place For Chromaster Series system installation, it is required to provide a space of 540 mm in width, and 550 mm in depth at least. A space of 150 mm or more in width shall be provided on the rear side of the instrument, and a space of 100 mm or more in width shall be provided on each of the left and right sides of the instrument.
Page 591: Checking The Contents
Other Conditions (a) Avoid placing the instrument near a window where it would be exposed to direct sunlight. Exposure to sunlight may cause a degraded performance and/or discoloration of the painted surfaces. (b) Protect the instrument from drafts. (c) Do not allow the instrument to be exposed to any strong vibration or shock.
Page 592: Assembling
6. Assembling 6.1 Removal of Transport Screws There are three screws for transport installed on the bottom of the instrument. Remove the transport screws with a phillips screwdriver. Transport screw 3. (For lamp house fixing) Transport screw 1. Transport screw 2. (For the instrument (For the instrument fixing)
Page 593 Cathode nut Lamp house Xenon lamp Transport Cathode screw Appended Fig. 1-4 Transport Screws and Mounting Xenon Lamp Install the xenon lamp in the lamp house. And mount it to the instrument (see ⑧ to ⑪ in section 6.2.1 (2).) Adjust the position of the xenon lamp.
Page 594 • Power Supply The power cord is furnished together with the Chromaster 5440 fluorescence detector. Connect this power cord to the rear of the instrument. Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5440 fluorescence detector To AC power supply Chromaster 5310...
Page 595 • Wiring Arrangement In the Chromaster series, it is required to connect the e-Line cable between the instruments. On the left rear of each instrument, insert the e-Line cable into the e-Line connector. e-Line connector Rear side of the instrument Appended Fig.1-6 e-Line Connector on the Rear of Instrument...
Page 596 Isocratic System/Low-pressure Gradient System (stacked in two blocks) e-Line cable 1) Chromaster 5410/5420/ 5430/5450 detector e-Line cable 2) Chromaster 5440 fluorescence detector Chromaster 5310 column oven Chromaster organizer Chromaster 5210 autosampler Chromaster Interface control 5110 pump board Appended Fig. 1-7 e-Line Cable Connection Appended Table 1-2 Cables to be Used e-Line cable 1) (50 cm) P/N 890-6105 (attached to each unit)
Page 597 • System Tubing In the Chromaster series, the inlet tube up to the pump and drain tube are fastened to the right/left side face of each unit with tube clamps. And the tubes are connected from the pump to the autosampler, column and detector through the central hole of each module unit.
Page 598 Low-pressure Gradient System Chromaster 5440 fluorescence detector Detector cell Mobile phase Detergent Chromaster 5310 column oven Mixer Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump Four-way joint Degassing unit Proportioning valve Drain Appended Fig. 1-9 Piping Arrangement for Low-pressure Gradient System Connect the inlet tube of the mobile-phase container to the IN port of the degassing unit.
Page 599 • Drain Tubing Chromaster 5440 fluorescence detector T-joint Drain tube A1*3 Chromaster Chromaster 5310 organizer column oven Drain tube B1 Chromaster 5210 Drain tube *2 autosampler T-joint N1 Drain tube A1*1 Chromaster 5110 I-joint pump L-joint Drain tube *1 Drain tube A1*2 Appended Fig.
Page 600 • GUI Controller The GUI controller is a touch panel type operation panel. This operation panel alone enables the user to control the respective modules. For operation, refer to the instruction manual of the GUI controller. • Fastening between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips...
Page 601 • Assembly of Constant Temperature Flow Cell (Option) Chromaster 5440 fluorescence detector can incorporate the constant as an option. The temperature switching equipment installed in the constant temperature flow cell keeps constant the temperature of the mobile phase and the sample which is poured into the flow cell. Therefore, change in sensitivity caused by environment temperature change can be reduced.
Page 602: Appendix 2. Description On Contact Signal Communication
APPENDIX 2. Description on Contact Signal Communication 1. Outline The following two types of contact signals are used in the Chromaster series. Contact signals (START, ERROR, BUSY) entering the e-Line connector. These are contact signals having input/output functions 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.
Page 603 Connection with L-2000 Series Use the e-DIO cable (890-6145) for connection. ERROR START STOP e-Line connector To L-2000 To Chromaster series series instrument instrument e-Line connector BUSY 3-pin connector e-DIO cable e-DIO cable (890-6145) (890-6145) APPENDIX 2 - 2...
Page 604 Connection with Model D-2500 Use the e-DIO cable (890-6146) for connection. D-2500 START START EXTERNAL To Chromaster series instrument BUSY e-Line BUSY connector Connect the START L and G terminals of the e-DIO cable (890-6146) to the EXTERNAL-COM terminal of the Model D-2500.
Page 605: Individual Contacts Of Each Unit
3. Individual Contacts of Each Unit Contact Signal Input Terminals These are contact signal input terminals for control using contact signals from an external switch, relay etc. Any of the signals is activated by shorting the terminal for 0.1 second or longer. The input circuit is shown in Fig. 3. Contact signal Output Terminals These are contact signal input terminals for control using contact signals of an external unit.
Page 606 +5 V 320 Ω Max. 10 mA Chromaster series External unit unit Activated upon shorting contacts of external unit. Fig. 3 Contact Signal Input Circuit 0.1 A max. 30 V max. Chromaster series unit External unit Fig. 4 Contact Signal Output Circuit APPENDIX 2 - 5...
Page 607: Appendix 3. Glossary
APPENDIX 3. GLOSSARY Initial screen ........After power on, the initial screen appears upon completion of initialization. Auto zero [A/Z]....... Absorbance is electrically adjusted to zero to cancel insignificant parts of data. In common analytical practice, perform auto zero adjustment immediately before or after the start of operation.
Page 608 Scan ..........Means a sequential shifting operation of monochromator wavelength for spectral measurement. Stokes law ........The law states that the wavelength of a fluorescent emission is always longer than the excitation wavelength. Time Program........ Used to adjust such measurement parameters as detection wavelength according to measurement time.
Page 609 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. Ex (Excitation wavelength) .... Used for exciting a sample. Recorder (RECORDER)....
Page 610: Flowpath Figures
FLOWPATH FIGURES General flowpath figures are shown below. Please select a plumbing according to your system configuration and the purpose. :Stainless-steel pipe :Teflon tube Numbers :Inside diameter. 1. Isocratic System Chromaster 5440 FL Detector Detector cell 0.25 ST 0.33 TT Inlet tube Mobile phase Wash fluid...
Page 611 • Keep this manual in a safe place nearby so it can be referred to whenever needed. 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 3rd Edition, June 2011 Copyright C Hitachi High-Technologies Corporation 2011. 1st Edition, 2011 All rights reserved. Printed in Japan. Part No. 892-9320-2 HH-R (RG-HMS)
Page 612 NOTICE: 1. The Information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Technologies Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Technologies Corporation.
Page 613 PREFACE Thank you very much for purchasing Chromaster 5310 Column Oven. The Chromaster 5310 Column Oven is used in a liquid chromatograph system for maintaining the analytical column at a constant temperature, for the purpose of improving the separation of sample components according to temperature and the reproducibility of retention time.
Page 614 ABOUT THIS MANUAL This instruction manual describe how to use and maintain the Chromaster 5310 Column Oven. This instruction manual. consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 OVERVIEW (Outline of Chromaster 5310 Column Oven) Section 2 FUNCTIONS (Name and Function of Each Column Part, Specifications) Section 3 OPERATION (Basic Operation, UTLTY Setting, GLP and Preparation) Section 4 MAINTENANCE &...
Page 615 IMPORTANT Warranty on Product Limited Warranty The Chromaster 5310 Column Oven is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 616 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 617 (m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Technologies shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 618 (b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 619 In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 620 Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 621 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 622 Do not perform any operation or action other than described in these manuals. • On occurrence of any trouble in the instrument, notify the nearest sales service representative of Hitachi High-Technologies. • 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.
Page 623 Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Technologies. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 624 SAFETY SUMMARY WARNING precautions in the Manual WARNING 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 (Section 2.3, 3.6) • Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 625 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure turn off the power switch and unplug the power cord before proceeding to fuse replacement.
Page 626 SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Touching Hot Part Could Result in Burns! The column oven becomes very hot during operation and can severely burn you in case of contact with it. Before column replacement, open the column oven door and wait until the inside temperature of the column oven decreases down to room temperature.
Page 627 If any one of the warning labels becomes illegible due to deterioration, contact your local Hitachi High-Technologies Corporation sales representative or service office of Hitachi High-Technologies Corporation sales representative for replacement with a new one.
Page 628 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument Front View (2) Do Not Touch Hot Part (3) Explosion of Vapor from Flammable Chemicals SAFETY - 7...
Page 629 SAFETY SUMMARY NOTICE precautions Precautions on Use of Solvents • Fluororesin, PEEK, quartz and SUS316 materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials. • This instrument has internal parts made of materials that could be corroded by strongly acidic solutions, strongly alkaline solutions or organic solvents.
Page 630 SAFETY SUMMARY NOTICE precaution (Continued) Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally. If necessary, conduct measurement on a control sample. SAFETY - 9...
Page 631 CONTENTS PREFACE.......................1 ABOUT THIS MANUAL..................2 IMPORTANT..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users....IMPORTANT-4 Estimated Life Time of the Instrument........IMPORTANT-4 Caution on Disposal of Instrument .........IMPORTANT-5 Disposal of This Instrument and Its Parts ......IMPORTANT-5 Precautions on CE Conformity Marking .........IMPORTANT-5 Information for Users on WEEE (only for EU Countries) ..IMPORTANT-6 Other Precautions..............IMPORTANT-6...
Page 632 3.1.3 Temperature Setting................3-7 3.1.4 Setting of Temperature Ready Conditions ........3-8 3.1.5 Position Changeover for Selector Valve..........3-9 3.1.6 Closing Operation................3-9 UTLTY Setting....................3-10 3.2.1 Setting of Leak Sensor ..............3-10 3.2.2 Analog Temperature Output .............. 3-12 3.2.3 Setting of Error Out Contact ..............
Page 633 Replacement Parts ....................5-1 Consumables and Spare Parts ..............5-1 Parts Replacement Method ................5-3 5.2.1 Fuse Replacement ................5-3 5.2.2 Replacement of Seals for Selector Valve (option)......5-4 INDEX........................6-1 APPENDIX APPENDIX 1. INSTALLATION ............APPENDIX 1-1 Unpacking ................APPENDIX 1-1 Place for Installation ..............
Page 634 1. OUTLINE 1.1 Outline of Chromaster 5310 Column Oven The major features of the Chromaster 5310 column oven are as follows: Broad Temperature Control Range Temperature rising and cooling functions based on the principle of Peltier temperature control are provided in the standard version of the Chromaster 5310.
Page 635 1.1 Outline of Chromaster 5310 Column Oven Enhancement of Data Reproducibility by Means of Optimum Preheating A preheating method developed by Hitachi (FACTS: Flow Adapted Column Temperature Stability) is employed. This preheating method makes it possible to provide a stable peak retention time even if the ambient temperature varies and to minimize a dead volume for reducing possible peak diffusion.
Page 636 1.2.1 1.2 Configuration of Liquid Chromatograph System The liquid chromatograph system consists of a pump for feeding a mobile phase, a sample introducing section (autosampler, manual injector) for injecting a sample, a column for chromatographic separation of the injected sample, a column oven for maintaining the column at a constant temperature, and a detector section for detecting a signal of a separated component of the sample.
Page 637 1.2 Configuration of Liquid Chromatograph System An eluent is fed by the pump through the degassing unit. A sample is injected from the autosampler. The injected sample is separated through the column which is maintained at a constant temperature by the column oven. (4) Each component separated from the sample is then detected as a signal by the detector.
Page 638 1.2.2 Each of plural eluents is fed from the degassing unit to the low-pressure unit. In the low-pressure unit, the eluents are mixed at a pre- specified ratio. Through the mixer, the mixture eluent is delivered. A sample is injected by the autosampler. The injected sample is separated through the column which is maintained at a constant temperature by the column oven.
Page 639 2. FUNCTIONS 2.1 Name and Function of Each Part on Column Oven Front door (Left) Power switch UI pad Front door (Right) Fig. 2-1 Front Panel • Power switch : Turns power ON/OFF. • Front door (R/L) : The column oven has double doors. Opening the front door (R/L) allows you to access an internal space that protected with a black cover.
Page 640 2.1 Name and Function of Each Part on Column Oven Inside cover Drain tray Leak sensor Inside cover fixing tab Fig. 2-2 Inside the Panel • Inside cover : A column housing cover. It is fixed with four tabs. • Inside cover fixing tab : It locks the inside cover. For unlocking the cover, slide two upper side tabs downward and two lower side tabs upward.
Page 641 Analog output connector Power connector Ground terminals Wiring cover (e-Line connector is inside) Fig. 2-4 Rear Panel Ground terminals : Terminals for grounding connection (three terminals). Power connector : For connecting the power cable. Analog output connector A connector for analog output of a temperature indication.
Page 642 2.2 Name and Function of Each Part on UI Pad (Option) 2.2 Name and Function of Each Part on UI Pad (Option) A UI pad will be used when a chromatography data station or a GUI controller (option) is not used for module control. The UI pad is ineffective when either chromatography data station or a GUI controller (option) is connected with this column oven.
Page 643 Table 2-2 Function of Each Key Function Remarks Upper limiter must be set at +5 °C or SET TMP Used for temperature setting. Sets temperature and also more above the set temperature. temperature upper limiter. (set temp) COND Used for condition setting upon Upon setting wait time of “0”, ready judging that temperature is ready.
Page 644 2.2 Name and Function of Each Part on UI Pad (Option) Table 2-1 Function of Each Key (continued) Function Remarks Deletes each step in time program editing. ▪ When a cursor is in an entry field of (delete) TIME, the step is deleted. ▪...
Page 645 2.3.1 2.3 Operating Principle and Functional Description 2.3.1 Temperature Control With the Chromaster 5310 column oven, analysis can be started when oven temperature is within a certain set range (temperature ready status). Parameters settable are Tolerance and Wait Time, and when the measured temperature of the oven is maintained within the set temperature ±...
Page 646 2.3 Operating Principle and Functional Description 2.3.2 Gas Leak Sensor WARNING 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.
Page 647 2.3.2 The interior of the Chromaster 5310 column oven is apt to reach a very high temperature through setting. If an organic solvent or the like were to leak in such a high temperature environment, it could lead to a serious hazard such as explosion. A leak sensor is thus equipped to detect organic solvent vapor.
Page 648 2.4 Specifications 2.4 Specifications Principle of Temperature Control Peltier heating/cooling control Temperature Setting Range 1 to 85 °C (in increments of 1 °C) Temperature Control Range [Ambient temperature - 15] to [Ambient temperature + 60] °C and within temperature setting range Temperature Setting Accuracy : ±1.0 °C (20 to 85 °C in preheating) Oven temperature...
Page 649 Columns Accommodated 300 mm columns × 3 pcs Operating Temperature Range 4 to 35 °C (10) Operating Humidity Range 25 to 85% RH (11) Dimensions 410 (W) × 440 (D) × 140 (H) mm (12) Weight Approx. 13 kg (13) Input/Output Common contacts : BUSY OUT (level) ERROR IN (level) ERROR OUT (level)
Page 650 2.4 Specifications (d) Number of steps storable Up to 100 steps in a total of nine files (15) GLP Functions Recording of the changeover number of times and exchange dates of the optional changeover valve. (16) Other Function Liquid leak sensor Temperature control is stopped upon detection of liquid leak.
Page 651 3. OPERATION The method of column oven operation using the optional UI pad is described here. CAUTION Fatigue due to Long-Hour Operation If you keep working with the display monitor in the same posture for long hours, your eyes and body will be fatigued. When working with the display monitor for a long time, take a break for 10 to 15 minutes per hour for health of your eyes and body.
Page 652 * LED indicates “OVEN” in blue light. (a) Startup screen Column Oven 8928130-00 (C) Hitachi High-Technologies Corp. 2010 Initializing, self-testing, and indicating a copyright are performed. The program No. and version will be confirmed on the startup screen. The first monitor screen will be indicated after initialize- processing is completed normally.
Page 653 3.1.1 (b) 1st Monitor Screen (Oven Temperature Indication) TEMP:MONITOR SET READY:RANGE WAIT [－] 25.1 39.5-40.5 Indication Description MONITOR Measured temperature of column oven Set temperature of column oven RANGE Range in which temperature becomes ready (set temperature ± tolerance) WAIT Waiting time until temperature ready is attained after entering RANGE (“–”...
Page 654 3.1 Basic Operation (d) 3rd Monitor Screen (Time Program Indication) TIME MONITOR SET VALVE 1 PROG[－] 25.0 Indication Description TIME Indication of an elapsed period (in minutes) in execution of a time program Indication of a preset temperature VALVE1 Indication of present position of selector valve (option) (“–”...
Page 655 3.1.2 3.1.2 Parameter input Method Described below are parameter input screen and program setup screen for the Chromaster 5310 column oven. Parameter Input Screen (a) Single numeric Parameter name Input range PROGRAM NO. (1 – 9) Input field (b) Plural numeric Input Item Parameter name VALVE1 SEAL CHANGE...
Page 656 3.1 Basic Operation Numerical Input (a) A cursor is indicated on the first character in the input field. Previous setup value is indicated in the input field. (b) Numerical and decimal (.) input are allowed up to the number of maximum character input. (c) Press the ENT key to register the input value, and move to the next item.
Page 657 3.1.3 3.1.3 Temperature Setting Carry out setting of the control temperature and temperature upper limit. SET TMP SET TEMP (°C) MAX LIMIT (°C) <1 - 85> Set the control temperature. 40 ENT SET TEMP (°C) MAX LIMIT (°C) <45 - 95> Set the temperature upper limit.
Page 658 3.1 Basic Operation 3.1.4 Setting of Temperature Ready Conditions Make the condition setting for the temperature ready status. Initial setting: TOLERANCE=1.0 °C, WAIT TIME=0 min. COND COND USE TOLERANCE (YES=1, NO=0) Specify whether or not to use tolerance setting. 1 ENT TOLERANCE (°C) WAIT TIME (min) <0.1 - 9.9>...
Page 659 3.1.5 3.1.5 Position Changeover for Selector Valve In an arrangement where the optional selector valve is connected, its position changeover can be made by keying on the UI pad. VALVE Indicates the current position number. VALVE1 POSITION (1 - 3) CURRENT 2 ENT Monitor screen...
Page 660 3.2 UTLTY Setting 3.2 UTLTY Setting 3.2.1 Setting of Leak Sensor Set the leak detection level for the gas leak sensor. SET UP UTLTY UTILITY (LEAK SENSOR=1, ANALOG OUT=2, ERROR OUT=3, CALIBRATION=4) 1 ENT SELECT SENSOR (GAS=1, LIQUID=2) 1 ENT LEAK GAS (MONITOR=1, SET LEVEL=2) Monitor the gas leak sensor output.
Page 661 3.2.1 NOTE: 1. Even if the sensor output exceeds the threshold on the gas leak sensor monitor screen, a leak error will not occur. 2. The gas leak sensor output may vary slightly according to the environment of the installation room even if a leak has not occurred.
Page 662 3.2 UTLTY Setting 3.2.2 Analog Temperature Output Set the output temperature for the analog output connector on the rear of the instrument. Output temperature conforms to the relational expression given below. Temperature [°C] = (output voltage [mV]/9.6) - 10 SET UP UTLTY UTILITY (LEAK SENSOR=1, ANALOG OUT=2, ERROR OUT=3, CALIBRATION＝4)
Page 663 3.2.3 3.2.3 Setting of Error Out Contact Specify whether or not to output an error contact signal to another instrument upon occurrence of an error in the column oven. When the other instrument receives the error contract signal, its operation is stopped. SET UP UTLTY UTILITY (LEAK SENSOR=1, ANALOG OUT=2,...
Page 664 3.2 UTLTY Setting SET UP UTLTY UTILITY (LEAK SENSOR=1, ANALOG OUT=2, Present setting is ERROR OUT=3, CALIBRATION=4) indicated. 4 ENT SELECT MODE (+OFFSET=1, -OFFSET=2) OFFSET (°C)=-1.0 Select either plus or minus side for deviation. 1 ENT SET +OFFSET (0.0 - 5.0) °C Set an offset value for the correction.
Page 665 3.3.1 3.3 GLP-Related Functions 3.3.1 Keylock Setting This function serves to lock the keys on the keyboard, and thus prevent erroneous activation of keys on the control panel. GLP (LOGBOOK=1, KEY LOCK=2) 2 ENT KEY LOCK (YES=1, NO=0) 1 ENT Monitor screen LOCK OFF Clicking the...
Page 666 3.3 GLP-Related Functions 3.3.2 Logbook Setting (Valve) When using the optional selector valve, information on the replacement date of the valve seal (a maintenance item) and number of valve switchings after the replacement is recorded in logbook form. GLP (LOGBOOK=1, KEY LOCK=2) 1 ENT Check the logbook information.
Page 667 3.4.1 3.4 Analysis Operation 3.4.1 Time Program Setting In the Chromaster 5310, a time program can be prepared for each of the temperature setting and selector valve position setting. PROG SET PROGRAM NO. (1 - 9) Enter a time program number. 1 ENT EDIT MODE (MODIFY=0，NEW=1) Select a mode.
Page 668 3.4 Analysis Operation NOTE: 1. If a valve is specified for “nonuse”, it is not indicated. 2. Just pressing the ENT key without inputting a numeric value results in retention of the previous setting. 3. In time programming, although a temperature level can be changed, a temperature rising time/cooling time cannot be specified.
Page 669 3.5.1 3.5 Setup 3.5.1 Valve Use/Nonuse Setting Specify whether or not to use an optional selector valve. Valve type is to be automatically recognized. SET UP POWER ON UTLTY SETUP: VALVE1 CONTRAST S.NO. SETUP monitor screen NO USE 02AB-111 ENT key SETUP ITEMS(USE VALVE=1, CONTRAST=2) Specify whether or not to use an optional...
Page 670 3.5 Setup 3.5.2 LCD Contrast Setting For LCD contrast setting on the UI pad, take the procedure shown below. SET UP UTLTY POWER ON SETUP: VALVE1 CONTRAST S.NO. SETUP monitor screen 02AB-111 ENT key SETUP ITEMS(USE VALVE=1, CONTRAST=2) Specify an LCD contrast level. 2 ENT LCD CONTRAST(1 - 7) 1 ENT...
Page 671 3.6 Before Performing Analysis 3.6 Before Performing Analysis This chapter describes the basic items to be careful about before starting analysis. WARNING 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.
Page 672 3.6 Before Performing Analysis WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 673 3.6.1 (b) When performing analysis with a UV detector in the short wavelength range or highly sensitive analysis with an RI detector, degassing the mobile phase before use is not enough, and the baselines may be fluctuated by the bubbles. In such a case, use a degassing unit which can degas mobile phase on-line.
Page 674 3.6 Before Performing Analysis Table 3-2 Reagents for Mobile Phase that may be Restricted Use is Possible If Use is Possible If Reagents Unsuitable Use is Possible 50% or Lower 10% or Lower for SUS316 Phosphoric acid Acetic acid Disodium phosphate Ammonium chloride Sodium phosphate Ammonium citrate...
Page 675 3.6.2 3.6.2 Characteristics of Organic Solvents Characteristics of organic solvents as mobile phase for liquid chromatograph are shown in Table 3-3. Use it for reference. WARNING 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.
Page 676 3.6 Before Performing Analysis WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 677 3.6.2 Table 3-3 Characteristics of Organic Solvents Polarity Viscosity Refractiv UV cut Flash Ignition point Vapor Boiling Specific (cP20 ° C) ° C e index off (nm) point density point gravity Lower Upper ( ° C) ( ° C) (Air: 1) (Water: 1) limit limit...
Page 678 3.6 Before Performing Analysis NOTICE: For Using Organic Solvents as Mobile Phase 1. When using organic solvents, be careful about UV cut off wavelength. *UV cut off wavelength: Light cannot be transmitted in the range shorter than this wavelength. For example: Cut off wavelength of chloroform is 245 nm.
Page 679 3.6.3 3.6.3 Cautions on Static Electricity WARNING Ignition of Flammable Chemicals by Static Electricity 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.
Page 680 3.7 Preparation 3.7 Preparation NOTE: When using Ultrasonic Cleaner etc., follow the instruction manual for it. 3.7.1 Degassing and Removing Dust from Mobile Phase Degas mobile phase before use without fail. Oxygen gas and nitrogen gas contained in mobile phase cause the following when used under high pressure.
Page 681 3.7.2 Remove cap Mobile phase container Ultrasonic cleaner (a) Set mobile phase container well stirred into ultrasonic cleaner. * When using a mixed mobile phase, stir it completely by using a stirrer, or else low repeatability or baseline drift may be caused. NOTE: Degas mobile phase of organic solvent by using ultrasonic cleaner with water.
Page 682 3.7 Preparation Devices to be prepared Ultrasonic cleaner (Put water in the bath without fail.) (ii) Aspirator with rubber stopper which fits the mouth of mobile phase container Rubber stopper should fit the mouth of container. Ultrasonic cleaner Mobile phase container Aspirator (a) Set mobile phase container* in ultrasonic cleaner after sufficient stirring.
Page 683 3.7.3 (h) Turn off the power of ultrasonic cleaner. Take mobile phase container out of ultrasonic cleaner, wipe the water from the container, and set it to liquid chromatograph. NOTE: Bubble generation depends on constitution of mobile phase. When mobile phase is a mixture with organic solvent (e.g.
Page 684 3.7 Preparation 3.7.4 Sample Pretreatment Filter samples without fail if they may contain fine dust. Dust can clog column and deteriorate it. Remove foreign matter from samples without fail. Foreign matter can lower the reliability of data, e.g. generating abnormal peaks etc. (a) Example of Filtering Samples Dust in sample can be removed easily as follows.
Page 685 3.7.4 NOTE: There are various ways of removing foreign matter from sample. Remove in the way suitable for the purpose of analysis. Cartridge of silica gel Clean sample after removing foreign matter. 3 - 35...
Page 686 4.1.1 4. MAINTENANCE & INSPECTION NOTICE: Make sure to request our authorized service agent for repair of the instrument in case it breaks down. Repair by anyone who has not received technical training by us is prohibited since it could be hazardous. 4.1 How to Check the Specifications and Performance 4.1.1 Items to Prepare in Advance •...
Page 687 4.1 How to Check the Specifications and Performance 4.1.3 Operational Check of Gas Leak Sensor The Chromaster 5310 column oven is equipped with a gas leak sensor for detecting an organic solvent gas on occurrence of liquid leakage. Note, however, that liquid leakage may not be detected correctly due to variations in environmental conditions or sensitivity of the leak sensor.
Page 688 4.1.4 4.1.4 Operational Check of Liquid Leak Sensor The Chromaster 5310 column oven is equipped with a liquid leak sensor for detecting liquid leakage. Note, however, that liquid leakage may not be detected correctly due to sensitivity of the leak sensor. To prevent this, perform periodic operation check for the liquid leak sensor as instructed below.
Page 689 4.1 How to Check the Specifications and Performance Cleaning of Leak Sensor <Item to be prepared> • Hexagonal wrench (P/N: N315003, size: B2.5) (a) Remove the leak sensor fastening screw with the furnished hexagonal wrench to separate the sensor from the drain tray. (b) Wipe moisture off the leak sensor and drain tray, and then fasten the sensor to the drain tray again.
Page 690 4.1.5 4.1.5 How to Check the Temperature Setting Accuracy Check the accuracy of the temperature indicated by the column oven in the procedure given below. <Item to be prepared> • Hexagonal wrench (P/N: N315005, size: B4) Open the front door of the Chromaster 5310 column oven to remove an inside cover.
Page 691 4.1 How to Check the Specifications and Performance Temperature sensor 35mm Detailed view Fig. 4-4 Attachment of Temperature Sensor NOTE: In cases where a non-specified temperature sensor is used as a substitute for the specified one, be sure to measure a surface temperature in the vicinity of the groove of the preheat base.
Page 692 4.1.5 4.1.6 How to Check the Temperature Control Accuracy Check the accuracy (stability) of temperature control at the set temperature in the following procedure. Set the thermocouple in place the same way as in steps (1) to (3) of the preceding section for checking the temperature setting accuracy, and connect the thermometer output to a recorder.
Page 693 4.1 How to Check the Specifications and Performance 4.2 Periodical Inspection Check Item Frequency Check Method Drain tray Daily Check the drain tray for any contamination or dust to be cleaned. Liquid leak from flow path Daily Check tubing and connections for any liquid leakage.
Page 694 4.3.1 Adjustment Procedure While monitoring the sensor output on the gas leak sensor monitor screen, inject 50 μL of methanol through the piping connection opening in the side of the main unit. Set the alarm level to about 80% of the maximum sensor output value.
Page 695 4.3 Adjustment 4.3.2 Temperature Calibration If there is a difference between the indicated temperature and actual temperature (temperature measured by a calibrated thermometer) in the check on temperature setting accuracy, the difference can be corrected by temperature calibration setting. For instance, if the actual temperature as measured by calibrated thermometer is 39.5 °C when the indicated temperature of the column oven is 40.0 °C, then set a value of -0.5 °C (offset value) for correcting the difference.
Page 696 Erroneous operation of If error recurs after power is restored, PRESS “CL” KEY TO instrument or circuit board contact your nearest service office of CLEAR MESSAGE Hitachi High-Technologies Corporation sales representative. RAM ERROR PRESS “CL” KEY TO CLEAR MESSAGE PARAMETER ERROR...
Page 697 2. If error recurs after power is THEN CHECK MAX set at a level lower than restored, contact your nearest LIMIT ambient temperature.) service office of Hitachi High- Technologies Corporation sales 2. Temperature sensor representative. abnormal NOTE: 3. Circuit board faulty Pressing the CL key can clear this error indication.
Page 698 Turn on valve power again. If this PRESS “CL” KEY TO control circuit board error occurs repeatedly, notify your CLEAR MESSAGE nearest service office of Hitachi High-Technologies Corporation sales representative. VALVE IS NOT Valve connection error Correct valve setting (used/not CONNECTED used).
Page 699 5. REPLACEMENT PARTS Given below is a list of parts requiring periodic replacement in order to enable using the Chromaster 5310 column oven in the optimum conditions at all times. Most of these parts have a lifetime which varies substantially with usage of the instrument, etc.
Page 700 5.1 Consumables and Spare Parts Estimated Part No. Part Name Remarks Lifetime 893-3324 Pipe for AS to Union Option (preheat pipe kit accessory) 0.25 mm I.D. × 500 mm (Flexible SUS) 892-0824 Union Option (preheat pipe kit accessory) M790019 Option (preheat pipe kit Setscrew accessory) For preheat pipe inlet...
Page 701 5.2.1 5.2 Parts Replacement Method 5.2.1 Fuse Replacement WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure to turn off the power switch before proceeding to fuse replacement.
Page 702 5.2 Parts Replacement Method 5.2.2 Replacement of Seals for Selector Valve (option) NOTE: Be sure to halt the solvent delivery of the pump connected to the instrument prior to seal replacement. Take the following procedure for seal replacement. Items to prepare •...
Page 703 5.2.2 Rotor seal Positioning pin Stator ring Stator ring retaining screw Stator seal Stator seal Stator retaining screw Fig. 5-2 Replacement of Selector Valve Seals 5 - 5...
Page 704 6. INDEX 3-column selector valve (seal replacement)......5-4 3-column selector valve ..........2-12, 3-9 6-way 2-position valve (seal replacement)....... 5-4 6-way 2-position valve............. 2-12, 3-9 ALARM LEVEL............... 3-10 AMBIENT ................. 3-3 Accuracy ...............SAFETY-9 Alarm level ................4-7 Analog output connector ............2-3 Analog temperature output.............
Page 705 e-Line ..............APPENDIX1-8 Fuse ..................5-1 Fuse replacement ..............5-3 GLP key ................2-5, 3-15 Ground terminals..............2-3 Grounding .............. APPENDIX1-3 Ignition of flammable chemicals ....SAFETY-3, 2-8, 3-21 Ignition of flammable chemicals by static electricity ............. SAFETY-3, 3-29 Installation space ........... APPENDIX1-7 Instrument tipover ............SAFETY-5 Isocratic system ..........
Page 706 OVEN ..................3-12 Operation check of leak sensor..........4-3 Outline..................1-1 PROG key ................2-5 Packing list ............. APPENDIX1-7 Periodical inspection ..............4-7 Pipe (for Chromaster 5310)............5-1 Power connector ..............2-3 Power supply............APPENDIX1-8 Power switch ................2-1 Pre-heating plate..........APPENDIX1-14 Pre-heating tubing.....
Page 707 Troubleshooting (options) ............4-12 Tubing (option valves).......... APPENDIX1-24 Tubing (system) ........... APPENDIX1-17 Tubing connection of switching valve (option) ..APPENDIX1-24 UI pad..............2-1, 2-4, 2-12, 3-1 UTLTY key ..............2-5, 3-10 Unpacking .............. APPENDIX1-1 VALVE key ................2-5 VALVE1 SEAL ............... 3-16 Valve seal................
Page 708 If relocation of the instrument becomes necessary after delivery, consult your dealer or nearest Hitachi High- Technologies service representative in order to avoid possible trouble involved in relocation. 2. Place for Installation For installation of the instrument, select a place which meets the following conditions.
Page 709 Atmospheric gas (a) Adequate ventilation is required. (b) The room shall not be filled with highly corrosive gas of acid or alkali. (c) The room shall not be filled with gas of an organic solvent (particularly, benzine and paint thinner) which dissolves coating.
Page 710 3. Items to be Prepared by Customer 3.1 Power Supply Arrangement Power supply voltage: 100 to 115 V AC/220 to 240 V AC Fluctuation shall be ±10% of the rated voltage. Frequency: 50 or 60 Hz Fluctuation shall be ±0.5 Hz of the rated frequency. Power Capacity: 230 VA or more for a single unit, and 600 VA or more for the total system...
Page 711 WARNING Electric shock due to improper grounding This instrument is designed to meet the basic insulation stipulated in the international standard IE C61010-1. To prevent an electric shock hazard due to improper grounding, provide a proper grounding connection. Be sure to use the grounded 3P power cable, which is supplied as a standard accessory for the instrument.
Page 712 (a) Usual Grounding Connection (with grounded 3P power outlet) Grounded 3P power outlet (15 A) Grounded 3P table tap Power cord (attached to Chromaster 5310 instrument) column oven Ground resistance 750 mm or 100 Ω or less more below Connector ground Rear panel Grounding electrode...
Page 713 (b) Connection when Grounded Power Outlet is Unavailable 2P power outlet (15 A) 3P table tap with grounding wire Power cord (attached to Chromaster 5310 instrument) Grounding column oven terminal Ground 750 mm or resistance more below Connector 100 Ω or less ground Grounding wire (green) Rear panel...
Page 714 3.2 Installation Space For composing a liquid chromatograph system with the Chromaster series module units, a space of 540 mm wide (980 mm for stacking the units in two blocks) and 550 mm deep is required at least. Behind each unit, a space of 150 mm or more must be secured.
Page 715 5. Assembling NOTE: It is not permitted for the user to carry out installation at the time of delivery. For ensuring safety and high accuracy in operation of the instrument, installation of the instrument shall be carried out by or under supervision of qualified service personnel of the manufacturer or its authorized service agent.
Page 716 Isocratic System/Low-pressure Gradient System (stacked in one block) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump To AC power supply Appended Fig. 1-4 Power Cable Connection Diagram Appended Table 1-1 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer) Connector cable 2)
Page 717 Isocratic System/Low-pressure Gradient System (stacked in two blocks) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5440 fluorescence detector To AC power supply Chromaster 5310 column oven Chromaster 5210 autosampler Interface control Chromaster board 5110 pump Appended Fig. 1-5 Power Cable Connection Diagram Appended Table 1-2 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer)
Page 718 5.2 System Cabling In the Chromaster series, the module units are cabled by plugging the e-Line cable into the e-Line connector at the rear left of each unit. e-Line connector Rear panel of module unit Power connector Isocratic System/Low-pressure Gradient System Chromaster organizer e-Line cable 1)
Page 719 Isocratic System/Low-pressure Gradient System (stacked in two blocks) e-Line cable 1) Chromaster 5410/ 5420/ 5430/ 5450 detector e-Line cable 2) Chromaster 5440 fluorescence detector Chromaster 5310 column oven Chromaster organizer Chromaster 5210 autosampler Chromaster Interface control 5110 pump board Appended Fig. 1-7 e-Line Cable Connection Appended Table 1-4 Cables to be Used e-Line cable 1) (50 cm) P/N 890-6105 (attached to each unit)
Page 720 5.3 Assembling of Pre-heating Tubing Chromaster 5310 column oven has a pre-heating section for preliminary heating (Appended Fig. 1-8). The pre-heating section has nine grooves (lines) for accommodating the pre- heating tubing, and the optimum number of grooves to be used varies depending on the flow rate for the analysis to be used.
Page 721 Shown below is the assembling method of tubing for 1-line pre- heating, for example. Loosen the two hexagon bolts fastening the pre-heating plate where the pre-heating tubing is to be installed, using the hexagon screw wrench attached. Appended Fig. 1-9 Disassembling of Pre-heating Plate Prepare a tube of approx.
Page 722 With the tube set in the pre-heating base, re-attach the pre- heating plate and fasten it with the two hexagon bolts. NOTE: Before re-attaching the pre-heating plate, be sure to make sure that the tube is neatly installed in the grooves in the pre-heating base.
Page 723 Where a flow rate at higher than 1.51 mL/min is used, turn around the tube as shown in Appended Fig. 1-12 below. When turning around, install the tube to the next groove with one line of groove skipped. Turn around with one line of groove skipped Appended Fig.
Page 724 5.5 System Tubing In the Chromaster series, the inlet tube up to the pump and drain tube are fastened to the right/left side face of each unit with tube clamps. And the tubes are connected from the pump to the autosampler, column and detector through the central hole of each module unit.
Page 725 Chromaster 5440 fluorescence detector Detector cell Mobile- phase Chromaster 5310 liquid Detergent column oven Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump Degassing unit Drain Appended Fig. 1-14 Tubing Diagram of Isocratic System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to the IN port of degassing unit.
Page 726 Low-pressure Gradient System Detergent Mobile-phase liquid Chromaster organizer Chromaster 5410/5420/5430 detector Chromaster 5310 Injection valve column oven Syringe valve Chromaster 5210 autosampler Wash pump Low-pressure gradient unit/ proportioning valve Chromaster 5110 pump Degassing unit Drain Appended Fig. 1-15 Tubing Diagram of Low-Pressure Gradient System (stacked in one block) APPENDIX 1 - 19...
Page 727 Chromaster 5440 fluorescence detector Detector cell Mobile-phase liquid Detergent Chromaster 5310 column oven Mixer Column Chromaster Injection valve organizer Chromaster 5210 autosampler Chromaster 5110 pump Wash pump 4-way joint Degassing unit Proportioning Drain valve Appended Fig. 1-16 Tubing Diagram of Low-Pressure Gradient System (stacked in two blocks) Connect the inlet tube from the mobile-phase container to...
Page 728 Drain Tubing Drain tube A1 Chromaster organizer Chromaster 5410/ 5420/ T-joint 5430/ 5450 detector Chromaster 5310 column oven Drain tube A2 Chromaster 5210 autosampler Drain tube 4 Chromaster 5110 T-joint N1 pump Drain tube B1 Drain tube L-joint Appended Fig. 1-17 Tubing Diagram for Drain (when stacking module units in one block) Appended Table 1-6 Drain Tubes to be Used Drain tube A2...
Page 729 Chromaster 5440 fluorescence detector T-joint Drain tube A1*3 Chromaster Chromaster 5310 organizer column oven Drain tube B1 Chromaster 5210 Drain tube *2 autosampler T-joint N1 Drain tube A1*1 Chromaster 5110 I-joint pump L-joint Drain tube A1*2 Drain tube *1 Appended Fig. 1-18 Tubing Diagram for Drain (when stacking module units in two blocks) Appended Table 1-7 Drain Tubes to be Used...
Page 730 5.7 Fastening between Component Units CAUTION Prevention of Instrument Tipover Personal injury could be incurred if the instrument tips over. When installing the instrument, provide a proper means for preventing the instrument from tipping over accidentally. On the rear of each module unit, a cabling cover is attached. The adjacent models are fastened with each other by attaching the fastening plate between the cabling covers.
Page 731 6. Assembling of Optional Component Part (Switching Valve) 6.1 Type Chromaster 5310 column oven can incorporate one type of the switching valves shown below as option: 3-column selector valve, and 6-way 2-position valve. NOTE: It is not permitted for the user to carry out installation at the time of delivery.
Page 732 For 6-Way 2-Position Valve Chromaster 5310 column oven Pretreatment Detector column Analysis column Waste solution Injector Mobile phase 1 Pump 1 Pump 2 6-way 2-position valve Mobile Waste solution phase 2 Appended Fig. 1-21 Usage Example of 6-Way 2-Position Valve 7.
Page 733 7.2 Connection of Column Data Tags When the switching valve is mounted, the column management system updates the history data of the columns used in the analysis, interlocked with the switching valve, each time an analysis is completed, suspended and brought into an abnormal end.
Page 734 For 3-column Selector Valve Where the column management system is used in the Chromaster 5310 column oven which is set not to use a 3- column selector valve, the data on the tags which are connected to the relevant slot positions corresponding to the respective valve positions of the 3-column selector valve will be updated.
Page 735 APPENDIX 2 DESCRIPTION ON CONTACT SIGNAL COMMUNICATION 1. Outline The following two types of contact signals are used in the Chromaster series. Contact signals (START, ERROR, BUSY) entering the e-Line connector. These are contact signals having input/output functions 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.
Page 736 Connection with L-2000 Series Use the e-DIO cable (890-6145) for connection. ERROR START STOP e-Line connector To L-2000 To Chromaster series series instrument instrument e-Line connector BUSY 3-pin connector e-DIO cable e-DIO cable (890-6145) (890-6145) Connection with Model D-2500 Use the e-DIO cable (890-6146) for connection. D-2500 START START...
Page 737 3. Individual Contacts of Each Unit Contact Signal Input Terminals These are contact signal input terminals for control using contact signals from an external switch, relay etc. Any of the signals is activated by shorting the terminal for 0.1 second or longer. The input circuit is shown in Fig. 3. Contact signal Output Terminals These are contact signal input terminals for control using contact signals of an external unit.
Page 738 +5 V 320 Ω Max. 10 mA Chromaster series unit External unit Activated upon shorting contacts of external unit. Fig. 3 Contact Signal Input Circuit 0.1 A max. 30 V max. Chromaster series unit External unit Fig. 4 Contact Signal Output Circuit APPENDIX 2 - 4...
Page 739 APPENDIX 3 GLOSSARY 3-column selector ......A column selector valve that permits an analysis exchanging maximum three columns by switching incoming and outgoing flow paths connected on the column. 6-way 2-position valve ....A flow path switching valve applicable to the pre-treatment or similar processing.
Page 740 Gas leak sensor......A sensor that can detect a leakage of organic solvent in the column oven. Detection is made by means of the vapor emitted from organic solvent when a leakage occurs. Liquid leak sensor......A sensor that can detect a liquid leakage in the column oven.
Page 741 • Keep this manual in a safe place nearby so it can be referred to whenever needed. 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 3rd Edition, June 2011 Copyright C Hitachi High-Technologies Corporation 2011. 1st Edition, 2011 All rights reserved. Printed in Japan. Part No. 892-9122-2 HH-R (RG-LT)
Page 742 NOTICE: 1. The information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Technologies Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Technologies Corporation.
Page 743: Preface
PREFACE We thank you for purchasing the 6-channel degassing unit for Chromaster 5110 pump. This instrument is used to eliminate dissolved gas from wash fluid for mobile phase and the autosampler in HPLC analysis. This instrument is intended for use by persons having a basic knowledge of chemical analysis procedures.
Page 744: Important
IMPORTANT Warranty on Product Limited Warranty The 6-channel degassing unit for Chromaster 5110 pump is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the instrument is not used according to the instruction manual.
Page 745 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 746: Installation, Relocation And After-Sale Technical Service
(m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Technologies shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 747: Technical Seminars And Training Courses For Users
(b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 748 In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 749: Other Precautions
Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 750 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 751 SAFETY SUMMARY Prior to using the 6-channel degassing unit for Chromaster 5110 pump, read the following safety instructions carefully and understand the contents. The hazard warnings that appear on the warning labels on the product or in the manual have one of the following alert headings consisting of an alert symbol and a signal word WARNING or CAUTION.
Page 752 SAFETY SUMMARY ● Prior to using chemicals such as reagents, be sure to check data (MSDS etc.) related to the properties and handling of such substances and handle them correctly. ● If a problem occurs with the instrument or if you have any question concerning the instruction manual, contact our service representative nearest you.
Page 753 SAFETY SUMMARY COMMON SAFETY PRECAUTIONS Given below are safety precautions that do not appear in the manual. WARNING ● Failure due to continued use in faulty condition! ■ Continuing use of the instrument in a faulty condition could cause an electric shock or fire hazard.
Page 754 SAFETY SUMMARY WARNING INDICATIONS APPEARING IN MANUAL The warning indications that appear in this manual and their locations are given below. 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.
Page 755 CONTENTS PREFACE.......................1 ABOUT THIS MANUAL..................1 IMPORTANT..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users....IMPORTANT-4 Estimated Life time of the Instrument........IMPORTANT-4 Caution on Disposal of Instrument .........IMPORTANT-5 Disposal of This Instrument and Its Parts ......IMPORTANT-5 Precautions on CE Conformity Marking .........IMPORTANT-5 Information for Users on WEEE (only for EU Countries) ..IMPORTANT-6 Other Precautions..............IMPORTANT-6...
Page 756 1. OVERVIEW The 6-channel degassing unit for Chromaster 5110 pump is used for online degassing of solvents. This instruction manual has been compiled basically for the case where the 6-channel degassing unit is built in the Chromaster 5110 pump and used in combination with other system components/units of your liquid chromatograph.
Page 757: Functions
2. FUNCTIONS 2.1 Front Panel 6-channel degassing unit Monitor lamp Flow path inlet of degassing chamber Flow path outlet of degassing chamber Fig. 2-1 Front View of Pump Monitor Lamp Listed below are status indications of the monitor lamp. The lit-state color of this lamp changes in response to the status of vacuum pump.
Page 758: Specifications
2.2 Specifications 2.2 Specifications Number of Flow Paths 6 (paths) Standard throughput 3 mL/min (when using distilled water. Applicable range varies with the kind of mobile phase to be used. Note that, if momentary maximum flow exceeds 3 mL/min, the degassing performance given in (3) below may not be attained.) Degassing Performance UV absorbance change at wavelength 210 nm shall be...
Page 759 (c) At occurrence of pressure sensor error * Active status (error detected) can be checked from the Chromato Data Station (CDS) or GUI controller. Material of Wetted Parts TEFLON-AF (degassing membrane), glass fiber-reinforced PPS (connector) Power Supply 24 V DC (10) Power Consumption Max.
Page 760: Operation
3. OPERATION 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.
Page 761 3.2 Operating Procedure Table 3-1 Typical Solvents Restricted for Use as Mobile Phase Solvent Remarks Hexafluoroisopropanol (HPIF) 60% hexane If replacement of hexane with other solvent in the same chamber is repeated, the chamber might be damaged. Hydrogen fluoride solvents Perfluoro solvents CFC solvents Acid...
Page 762 Error status can be released by turning on power supply to the Chromaster 5110 pump again. NOTE: If the error recurs despite restart of the pump, be sure to consult your dealer or nearest Hitachi High-Technologies service representative. 3 - 3...
Page 763 3.4 Caution on Handling 3.4 Caution on Handling Caution on Solvent Replacement (substitution) For solvent replacement, make sure the old and new solvents will be dissolved in each other. If the old solvent will not be dissolved in the new one to be used, first replace the old solvent with an intermediary solvent which will be dissolved in both the old and new solvents, and then replace the intermediary solvent with the new one.
Page 764 Caution on Storage When you intend to use the degassing unit the next day though the pump was stopped after completion of analysis, instrument power supply may not be turned off. However, before a long-time stop of the degassing unit, turn off the power supply, wash adequately with ion-exchanged water, run methanol or the like, replace the flow paths with the air, etc., and then plug the tubes securely.
Page 765 4. TROUBLESHOOTING Table 4-1 directs troubleshooting of the degassing unit. If abnormality occurs, reference should be made to this table. Table 4-1 Troubleshooting of Degassing Unit Symptom Possible Cause Countermeasure Monitor lamp a. Power supply to the pump or a. Turn on power supply to the does not light.
Page 766 If relocation of the instrument becomes necessary after delivery, consult your dealer or nearest Hitachi High- Technologies service representative in order to avoid possible trouble involved in relocation. 1.1 Check against Packing List Exterior Check of Package First of all, check the exterior of product package.
Page 767 APPENDIX 2. PLACE FOR INSTALLATION 2.1 Installation Conditions Power Supply Line voltage: 24 V DC (supplied from the PC board at the rear of pump unit) Installation Location In Chromaster 5110 pump. 2.2 Ambient Conditions Operating Temperature 4 to 35 °C For measurement under the most stable condition, it is recommended to install this product in an air-conditioned room at 20 to 25 °C.
Page 768 (d) Shall be away from strong electric field generating equipment (such as electric welder, high frequency electric furnace and pole transformer). (e) Shall be free from excessive dust. (Performance degradation might be caused.) Power supply to motor-driven equipment (such as stirrer and vibrator) without a noise suppressor shall not be turned ON/OFF frequently on the same power supply line as that of this instrument.
Page 769 For solenoid valve A For solenoid valve B For solenoid valve C For solenoid valve D Appended Fig. 2-1 Tubes Attached to Chromaster 5110 Pump 6-channel degassing unit Low-pressure gradient unit (proportioning valve) Appended Fig. 2-2 Tubing between 6-channel Degassing Unit and Proportioning Valve Tube for port 1 Tube for port 2...
Page 770 Port 1 Port 2 Wash port Appended Fig. 2-4 External View of Chromaster 5210 Autosampler Aspiration of Eluent Eluent should be aspirated with the aspiration syringe attached to the pump. The total internal volume (per flow path) of the tubes for pump and the degassing chamber of 6-channel degassing unit is about 5 mL.
Page 771 • Keep this manual in a safe place nearby so it can be referred to whenever needed. 24-14, Nishi-Shimbashi 1-chome, Minato-ku, Tokyo, Japan 4th Edition, June 2011 Copyright C Hitachi High-Technologies Corporation 2011. 1st Edition, 2011 All rights reserved. Printed in Japan. Part No. 892-9220-3 HH-R (GG-HMS)
Page 772 NOTICE: 1. The Information contained in this document is subject to change without notice for improvement. 2. This manual is copyrighted by Hitachi High-Technologies Corporation with all rights reserved. No part of this manual may be reproduced, transmitted or disclosed to a third party in any form or by any means without the express written permission of Hitachi High-Technologies Corporation.
Page 773: Preface
PREFACE Thank you very much for purchasing Chromaster 5210 Autosampler. The Chromaster 5210 Autosampler is specifically designed for automatic analysis in a liquid chromatograph system. Note that physiologically or biologically active samples are not applicable to the Chromaster 5210 Autosampler because of possible infection with bacteria or viruses. This product is intended for use by persons having a basic knowledge of chemical analysis.
Page 774: About This Manual
ABOUT THIS MANUAL This instruction manual describe how to use and maintain the Chromaster 5210 Autosampler. This instruction manual consists of the following sections. IMPORTANT (Warranty, Installation, Relocation, After-sale Technical Service, etc) SAFETY SUMMARY (collected and summarized) Section 1 OUTLINE (Isocratic System, Low-Pressure Gradient System) Section 2 FUNCTIONS (The Instrument Keypad) Section 3 OPERATION (Basic Operation, Measuring Operation) Section 4 MAINTENANCE (Checking the Performance and Specifications)
Page 775: Important
IMPORTANT Warranty on Product Limited Warranty The Chromaster 5210 Autosampler is warranted to be free from defects in material or workmanship under normal use within the product specifications indicated in this manual and under conditions given below. This warranty is void if the software is not used according to the instruction manual.
Page 776 Warranty Limitations and Exclusions Disclaimer of Warranty THE MANUFACTURER MAKES NO WARRANTIES, EITHER EXPRESS OR IMPLIED, EXCEPT AS PROVIDED HEREIN, INCLUDING WITHOUT LIMITATION THEREOF, WARRANTIES AS TO MARKETABILITY, MERCHANTABILITY, FOR A PARTICULAR PURPOSE OR USE, OR AGAINST INFRINGEMENT OF ANY PATENT. IN NO EVENT SHALL THE MANUFACTURER BE LIABLE FOR ANY DIRECT, INCIDENTAL OR CONSEQUENTIAL DAMAGES OF ANY NATURE, OR LOSSES OR EXPENSES RESULTING FROM ANY DEFECTIVE PRODUCT OR THE USE OF ANY PRODUCT.
Page 777: Installation, Relocation And After-Sale Technical Service
(m) Failure due to a life-limited part that has exceeded the end of its useful lifetime. Limitations of Liability Hitachi High-Technologies shall not be liable in contract or in tort (including, without limitation, negligence, strict liability or otherwise) for claims by third parties (other then for bodily injury or...
Page 778: Technical Seminars And Training Courses For Users
(b) A maintenance & service contract is available for servicing the instrument after the warranty period has ended (service available at charge). (c) Maintenance parts and consumables will be supplied during the useful life of this instrument (7 years). And even though parts and/or units (when available) will continue to be supplied after the specified useful life has ended (for up to 10 years), they are not intended to extend the useful life of the instrument.
Page 779: Caution On Disposal Of Instrument
In the present design, this instrument does not use materials that would directly cause environmental harm. Note, however, that the environmental protection laws and regulations may be revised or amended. Therefore, be sure to consult with your local Hitachi High-Technologies sales or service representative when planning disposal of this instrument or its parts and accessories.
Page 780: Information For Users On Weee (Only For Eu Countries)
Information for Users on WEEE (only for EU Countries) This symbol is in compliance with the Waste Electrical and Electronic Equipment directive 2002/96/EC (WEEE). This symbol on the product indicates the requirement NOT to dispose of the equipment as unsorted municipal waste, but use the return and collection systems available.
Page 781 Disturbance by Electromagnetic Wave This instrument conforms to Class A in the EN standards EN61326 (first edition 2002-02). Avoid installing this instrument near equipment whose data will be affected by electromagnetic noise within the permissible range of this standard. Also, data of this instrument may be affected by electromagnetic noise or the instrument itself may malfunction.
Page 782 Do not perform any operation or action other than described in these manuals. • On occurrence of any trouble in the instrument, notify the nearest sales service representative of Hitachi High-Technologies. • 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.
Page 783: Warning
Disconnect the power cord plug from the power outlet. Then, after providing proper safety measures as required, contact the nearest service representative of Hitachi High-Technologies. Using the instrument in such an abnormal condition could result in an electric shock or fire.
Page 784 SAFETY SUMMARY WARNING precautions in the Manual WARNING 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 (Section 3.4) • Beware of ignition hazard when using flammable chemicals such as organic solvents. Do not bring a heat or flame source near the instrument.
Page 785 SAFETY SUMMARY WARNING precautions in the Manual(Continued) WARNING Electric Shock due to Improper Grounding This instrument is designed in conformity with the specifications of Class I in Annex H of the IEC 61010-1 (International Electrotechnical Commission Standards) – Issue 1. To prevent an electric shock hazard, provide a proper grounding connection.
Page 786: Caution
SAFETY SUMMARY CAUTION Precautions in the Manual CAUTION Heavy Instrument This instrument is as much as 24 kg (29 kg with the optional cooling unit equipped). When carrying this instrument, exercise care not to incur injury by dropping it off accidentally.
Page 787 If any one of the warning labels becomes illegible due to deterioration, contact your local Hitachi High-Technologies Corporation sales representative or service office of Hitachi High-Technologies Corporation sales representative for replacement with a new one.
Page 788 SAFETY SUMMARY WARNING and CAUTION Labels on Instrument (4) Injury of Hand by Needle or Internal Mechanism Left side view (5) Electric Shock due to Contact with Inside of Instrument (when equipped with optional cooling unit) Rear Panel SAFETY - 7...
Page 789 SAFETY SUMMARY NOTICE precautions Precautions on Use of Solvents • Stainless steel (SUS316), Vespel®, fluorine resin, polypropylene (PP), ethylene-propylene rubber (EPDM) and perfluoroelastomer materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials. •...
Page 790 SAFETY SUMMARY NOTICE precaution (Continued) Accuracy and Precision of Measured Values Carry out periodic inspection and check whether the system is operating normally. If necessary, conduct measurement on a control sample. SAFETY - 9...
Page 791 CONTENTS PREFACE.......................1 ABOUT THIS MANUAL..................2 IMPORTANT..................IMPORTANT-1 Warranty on Product ..............IMPORTANT-1 Installation, Relocation and After-sale Technical Service ..IMPORTANT-3 Technical Seminars and Training Courses for Users....IMPORTANT-4 Estimated Life time of the Instrument........IMPORTANT-4 Caution on Disposal of Instrument .........IMPORTANT-5 Disposal of This Instrument and Its Parts ......IMPORTANT-5 Precautions on CE Conformity Marking .........IMPORTANT-5 Information for Users on WEEE (only for EU Countries) ..IMPORTANT-6 Other Precautions..............IMPORTANT-6...
Page 792 3.1.2 Parameter setting ................3-4 Measuring Operation ..................3-6 3.2.1 Basics of Operation ................3-6 3.2.2 Analyzing Operation ................3-12 Shutdown Operation ..................3-58 Before Performing Analysis ................. 3-59 3.4.1 Selection of Mobile Phase and Cautions on Handling ...... 3-61 3.4.2 Degassing of Mobile Phase and Wash Fluid........
Page 793 Discharge of Air Bubbles from Syringe ............5-12 Replacing the Injection Valve Seal .............. 5-16 Replacing the Syringe Valve Seal..............5-18 Purging the Wash Pump................5-20 5.10 Discharge of Air Bubbles from Wash Pump ..........5-21 5.11 How to Wash Solvent Filter ................5-23 5.12 How to Replace Fuse (in the optional thermostat)........
Page 794: Outline
1. OUTLINE The liquid chromatograph system consists of a pump for feeding a mobile phase, a sample introducing section (autosampler, manual injector) for injecting a sample, a column for chromatographic separation of the injected sample, a column oven for maintaining the column at a constant temperature, and a detector section for detecting a signal of a separated component of the sample.
Page 795: Low-Pressure Gradient System
A mobile phase is fed by the pump through the degassing unit. A sample is injected from the autosampler. The injected sample is separated through the column which is maintained at a constant temperature by the column oven. Each component separated from the sample is then detected as a signal by the detector.
Page 796 Each of plural mobile phases is fed from the degassing unit to the low-pressure unit. In the low-pressure unit, the mobile phases are mixed at a pre-specified ratio. Through the mixer, the mixture mobile phase is delivered. A sample is injected by the autosampler. The injected sample is separated through the column which is maintained at a constant temperature by the column oven.
Page 797: Functions
2. FUNCTIONS 2.1 The Instrument Keypad 2.1.1 Name and Function of Each Part on Autosampler Main switch UI pad Window Door (left) Door (right) Fig. 2-1 Front View (A) Main switch : Turns on/off power supply. UI Pad (Option) : A keypad required for operating the autosampler independently.
Page 798 Door lock mechanism Syringe Sample rack Injection valve 3-way switching valve, Wash pump Wash port Syringe valve Degassing Drain tray unit Port 1 (Solvent 1) Port 2 (Solvent 2) Wash pump Fig. 2-2 Front View (B) Sample rack : Accommodates sample vials. Injection valve : Switches the flow path for delivering a sample and mobile phase to the column.
Page 799 Wash port : A port in which the needle is washed. Drain tray : A pan for receiving the leaking fluid if any. 3-way switching valve : A valve for switching flow path of wash fluid1 and wash fluid2. Wash pump : A pump for delivering wash fluid.
Page 800 Needle : Aspirates a sample. : Move right to left (X direction), back and forth (Y direction), and up and down (Z direction). Leak sensor : Detects fluid leakage. Injection port : A port into which the needle is inserted to inject a sample into the sample loop.
Page 801: Name And Function Of Each Part On Ui Pad (Option)
Name Content WAIT OFF IN Releases a wait state for injection valve changeover according to the external signal input. START OUT The injection valve outputs a start signal after switching to INJECT from LOAD. ALL END OUT Outputs the ALL END signal when the ALL END time is reached under the condition of ALL END OUT setting.
Page 802 Display Function WASH Delivers wash fluid with the wash pump to rinse out flow paths. PAUSE Puts an analysis sequence to pause. Releases pause when pressed again. UTLTY Sets the basic operating conditions. SET UP Keep pressing the wash button and the main switch at the same time until a setup screen is displayed.
Page 803: Application
2.2 Application The autosampler is combined with a liquid chromatograph and used for injecting a sample. 2.3 Operating Principle and Functional Description 2.3.1 Configuration of Flow Path The configuration and the flow path of the Chromaster 5210 autosamplers are shown in Fig. 2-5 and 2-6. Sample vials are placed in the form of a rack.
Page 804 Buffer tube Needle Syringe valve Injection valve Injection port Rack Loop Sample Waste Waste solution solution Plunger Wash Wash pump from Pump to Column Syringe 3-way solenoid valve Degassing unit Wash Wash fluid1 fluid2 Fig. 2-6 Flow Path of Autosampler 2 - 8...
Page 805: Sample Injection Method
2.3.2 Sample Injection Method Description of each method Select a sample injection method for the Chromaster 5210 autosampler from the following three methods. Table 2-1 Injection Methods Cut Injection Method All Volume Injection Full Loop Method (Standard) Injection Method Summary The amount of sample The entire sample The sample loop is filled...
Page 806 Operating suggestions are indicated below. Cut Injection Method When applying the cut injection method, the loop capacity more than the injection volume is required. Select loop capacity within the area indicated in the following figure. The sample introduction volume is selected within the shadow area of the following figure.
Page 807 Loop Capacity [µl] Fig. 2-8 All Volume Injection Method Full Loop Injection Method When applying Full loop injection method, the sample introduction volume more than quintuple loop capacity (injection volume) is required (amount of sample necessity). Select sample introduction volume within the area indicated in the following figure.
Page 808 Wash fluid selection and use examples The Chromaster 5210 autosampler uses two kinds of wash fluid. Refer to the following table. Table 2-2 Isocratic Analysis One Fluid Wash <standard> Two Fluids Wash (for Cut injection method, (for All volume injection method, Low carry over analysis) Full loop injection method) Wash fluid 1...
Page 809: Sample Injection Procedure
*3) Higher sample solubility solvent is used. (Some types of samples are dissolved with 100% organic solvent.) NOTE: Stainless steel (SUS316), Vespel®, fluorine resin, polypropylene (PP), ethylene-propylene rubber (EPDM) and perfluoroelastomer materials are used for the wetted parts of the instrument. Never use solvents that would corrode these materials.
Page 810 Idle status The mobile phase is flowing to the column from the pump via the loop of the injection valve. The wash fluid1 is connected to the syringe via the 3-way solenoid valve, the wash pump, and the port3 of the syringe valve.
Page 811 Aspiration of the wash fluid1 The syringe aspirates the dead volume (:vd, inside parameter) of fluid1. Switch the syringe valve to the wash port side (port1) after aspiration of the wash fluid1. When [wash before sample aspiration] is set, refer to the following operation.
Page 812 Sampling The syringe aspirates one-half of the air volume (:va/2) while needle is moving to the sample vial. The syringe aspirates [vr + vi + vl : Rear volume + Injection volume + Lead volume] after the needle has moved into the sample vial.
Page 813 Wash of the needle outer wall with the wash fluid1 The syringe aspirates one-half of the air volume (:va/2) while needle is moving to the wash port. Deliver the wash fluid1 via the wash pump to wash the needle outer wall. Buffer tube Needle Syringe valve...
Page 814 Movement of the needle and discharge of the lead volume After the needle has moved into the injection port, the injection valve is switched to inject the sample. Buffer tube Needle Syringe valve Injection valve Injection port Loop Rack Sample Waste Waste solution...
Page 815 Pressure release (LOAD switch) Switch the injection valve to the LOAD side to release pressure in the loop. Buffer tube Needle Injection valve Injection port Loop Rack Sample Waste Waste solution solution Plunger Wash wash Degassing unit Wash port pump From Pump To Column 3-way solenoid valve...
Page 816 Sample loading Deliver the sample into the sample loop. Buffer tube Needle Injection valve Syringe valve Injection port Rack Loop Sample Waste Waste solution solution Plunger Wash wash Degassing unit pump Wash port From Pump To Column 3-way solenoid valve Degassing unit Syringe...
Page 817 Sample injection (INJECT switch) Switch the injection valve to the INJECT side to load the sample into the flow path. Move the syringe to the top dead point after switching the injection valve. Buffer tube Needle Injection valve Syringe valve Injection port Rack Loop...
Page 818 Wash of the injection port flow path with the wash fluid1 Switch the syringe valve to the needle side (Port2). Deliver the wash fluid1 via the needle to the injection port with the wash pump to wash the flow path of the buffer tube and the injection valve.
Page 819 (10) [When two wash fluids are used] Wash of the injection port flow path with the wash fluid2. Switch the 3-way solenoid valve to the wash fluid2 side. Deliver the wash fluid2 via the needle to the injection port with the wash pump to wash the flow path of the buffer tube and the injection valve.
Page 820 (11) Return to idle status Switch the syringe valve to the syringe side (Port3). Move the needle to the home position. Switch the 3-way solenoid valve to the wash fluid1 side. Buffer tube Needle Syringe valve Injection valve Injection port Loop Rack Sample...
Page 821 (12) [When the plunger wash is applied] Wash the pump plunger with the wash fluid2. Switch the 3-way solenoid valve to the wash fluid2 side. Switch the syringe valve to the plunger wash side (port 4). Deliver the wash fluid2 to the pump plunger with the wash pump (specified time).
Page 822 All Volume Injection Method Procedure The all volume injection method, the injection volume, the feed volume, and the air volume are restricted by the following relational expression. A stroke of the syringe capacity can’t be used all. <175 µL of Standard syringe > vi + vf + va ≦...
Page 823 Idle status The mobile phase is flowing to the column from the pump via the loop of the injection valve. The wash fluid1 is connected to the syringe via the 3-way solenoid valve, the wash pump, and the port3 of the syringe valve.
Page 824 Aspiration of the wash fluid1 The syringe aspirates [vf + vd :Feed volume + Dead volume (inside parameter)] of fluid1. Switch the syringe valve to the wash port side (port1) after aspiration of the wash fluid1. When [wash before sample aspiration] is set, refer to the following operation.
Page 825 Sampling The syringe aspirates one-half of the air volume (:va/2) while needle is moving to the sample vial. The syringe aspirates [vi :Injection volume] after the needle has moved into the sample vial. Buffer tube va/2 Needle Syringe valve Injection valve Injection port Loop Rack...
Page 826 Wash of the needle outer wall with the wash fluid1 The syringe aspirates one-half of the air volume (:va/2) while needle is moving to the wash port. Deliver the wash fluid1 via the wash pump to wash the needle outer wall. Buffer tube va/2 Needle...
Page 827 Movement of the needle Move the needle into the injection port. Buffer tube Needle Syringe valve Injection valve Injection port Loop Rack Sample Waste Waste solution solution Plunger wash Wash pump Wash port From Pump To Column 3-way solenoid valve Degassing unit Syringe...
Page 828 Pressure release (LOAD switch) Switch the injection valve to the LOAD side to release pressure in the loop. Buffer tube Needle Syringe valve Injection valve Needle Injection port Loop Rack Sample Waste Waste solution solution Plunger wash Degassing unit Wash pump Wash port From Pump To Column 3-way solenoid valve...
Page 829 Sample loading Deliver the sample into the sample loop. The syringe discharges [vf + vi + va + vd : Feed volume + Injection volume + Air volume + Dead volume (inside parameter)], and delivers a sample into the loop. Buffer tube Needle Syringe valve...
Page 830 Sample injection (INJECT switch) Switch the injection valve to the INJECT side to load the sample into the flow path. Buffer tube Needle Syringe valve Injection valve Injection port Rack Loop Sample Wash Wash solution Plunger solution wash Degassing unit Wash pump Wash port From Pump To Column...
Page 831 Full Loop Injection Method Procedure The full loop injection method, the injection volume, the west volume, and the air volume are restricted by the following relational expression. A stroke of the syringe capacity can’t be used all. <175 µL of Standard syringe > vi + vw + va ≦...
Page 832 Idle status The mobile phase is flowing to the column from the pump via the loop of the injection valve. The wash fluid1 is connected to the syringe via the 3-way solenoid valve, the wash pump, and the port3 of the syringe valve.
Page 833 Aspiration of wash fluid1 The syringe aspirates [vd :Dead volume (inside parameter)] of fluid1. Switch the syringe valve to the wash port side (port1) after aspiration of the wash fluid1. When [wash before sample aspiration] is set, refer to the following operation: Washing of the needle outer wall and the injection port flow path.
Page 834 Sampling The syringe aspirates one-half of the air volume (:va/2) while needle is moving to the sample vial. The syringe aspirates [vw + vi :Waste volume + Injection volume] after the needle has moved into the sample vial. Buffer tube va/2 Needle Syringe valve...
Page 835 Wash of the needle outer wall with the wash fluid1 The syringe aspirates one-half of the air volume (:va/2) while needle is moving to the wash port. Deliver the wash fluid1 via the wash pump to wash the needle outer wall. Buffer tube Needle Syringe valve...
Page 836 Movement of the needle Move the needle into the injection port. Buffer tube Needle Syringe valve Injection valve Injection port Rack Loop Sample Waste Waste solution Plunger solution wash Wash pump Wash port From Pump To Column 3-way solenoid valve Degassing unit Syringe...
Page 837 Pressure release (LOAD switch) Switch the injection valve to the LOAD side to release pressure in the loop. Buffer tube Needle Syringe valve Injection valve Injection port Rack Loop Sample Waste Waste solution Plunger solution wash Wash port Wash pump From Pump To Column 3-way solenoid valve Degassing...
Page 838 Sample loading Deliver the sample into the sample loop. The syringe discharges [va/2 + vw/2 + vi + vd : one-half of the Air volume + one-half of the Waste volume + Injection volume + Dead volume (inside parameter)], and delivers a sample into the loop.
Page 839 Sample injection (INJECT switch) Switch the injection valve to the INJECT side to load the sample into the flow path. Move the syringe to the top dead point after switching the injection valve. Buffer tube Needle Injection port Syringe valve Injection valve Rack Loop...
Page 840: Specifications
2.4 Specifications 2.4.1 Main Unit Maximum number of samples 120 (1.5 mL) (4 mL) (option) 195 (1 mL) (option) 192 (96-holes microplate × 2) (option) 768 (384-holes microplate × 2) (option) Sample injection method Cut injection method All volume injection method Full loop injection method Syringe capacity 175 µL (standard)
Page 841 (11) Minimum injection operating time Approx. 20 s (stand-alone) (12) Minimum cycle time Approx. 30 s (stand-alone) (13) Injection mechanism X, Y, Z directions: Needle movement (14) Washing method Fluid2 wash with a dedicated pump (15) Vial detecting function Provided (16) Pressure resistance 40 MPa (17) Material of liquid-contacting parts...
Page 842 (24) Weight Approx. 24 kg (Approx. 29 kg with thermostat) (25) Ambient temperature 4 to 35 °C (non-condensing) (26) Ambient humidity 25 to 85% (27) Other functions Liquid leak sensor, Door lock (28) Power supply 24 V DC, 4 A *1) Performance specification should be checked in the following combination.
Page 843: Thermostat (Option)
2.4.2 Thermostat (option) Temperature setup range* 1 to 45 °C (in increments of 1 °C) Temperature control range* [ambient temperature – 21 °C] to [ambient temperature + 25 °C] and within the setup range (humidity 60 %, sample vial 1.5 mL, 4 mL, 1 mL) [ambient temperature –...
Page 844 Ambient temperature 4 °C to 35 °C Ambient humidity 25 to 85% Cooling system Peltier effect-based thermoelectronic cooling type Safety countermeasure Overheat prevention system by the thermal protector (75 °C) (10) Power supply AC 100 V to 240 V ± 10% (50/60 Hz), 110 VA *1) An acceptable temperature range for the thermostat is from 1 to 45 °C.
Page 845: Operation
3. OPERATION The method of the Chromaster 5210 autosampler operation using the optional UI pad is described here. CAUTION Fatigue due to Long-Hour Operation If you keep working with the display monitor in the same posture for long hours, your eyes and body will be fatigued. When working with the display monitor for a long time, take a break for 10 to 15 minutes per hour for health of your eyes and body.
Page 846 (a) Startup screen Auto Sampler 8928120-00 (C) Hitachi High-Technologies Corp. 2010 Initializing, self-testing, and indicating a copyright are performed. The program number and version will be confirmed on the startup screen. (b) 1...
Page 847 (c) 2 monitor screen This screen indicates information about the thermostat (option). TEMP RANGE 35.0 30.0 – 40.0 Indication Description TEMP Present temperature of thermostat (“-” is indicated when the thermostat is not under control.) RANGE Temperature range in which temperature ready status is assumed (set temperature ±...
Page 848: Parameter Setting
3.1.2 Parameter setting Carry out setting of the parameter and program. (1) Parameter setup screen (a) Single numeric Parameter name Input range PROGRAM NO. (1 – 9) Input field (b) Plural numeric Input Item Parameter name INJ. PORT SEAL CHANGE YYYY) <...
Page 849 (b) Numerical and decimal (.) input are allowed up to the number of maximum character input. (c) Press the ENT key to register the input value, and move to the next item. When the input value is error, the cursor is set up in the first character of the input field while indicating the previous input value, and waits for retype.
Page 850: Measuring Operation
3.2 Measuring Operation WARNING Injury of Hand by Needle or Internal Mechanism Never touch the inside of the autosampler during operation, as your hand or finger may be seriously injured by the needle or internal mechanism. 3.2.1 Basics of Operation Handling sample rack For taking out the sample rack, slightly lift its gripping section, and then pull it out toward you.
Page 851 NOTES: 1. Mount the sample rack at the correct position. If the rack is mounted at a wrong position, the instrument may be caused to malfunction. 2. Be sure to use both hands for handling the sample rack. Avoid hooking your fingers onto sample vials for handling the rack.
Page 852 Pull out the sample rack while keeping it in parallel position t the rack holder. Sample rack Rack holder Locating pin Handle Fig. 3-3 Handling of Thermostat Rack 3 - 8...
Page 853 Take care not to flaw these surfaces. Put it in until a sample vial touches the bottom of a sample rack. 1. Exercise care not to drop off the sample rack NOTES: accidentally. 2. Take care not to flaw the contacting surfaces of the sample rack and cooling rack holder.
Page 854 Setting of standard sample rack Orient the septum as shown below. Cap with hole White (silicone rubber) Septum Brown (Teflon) Sample vial (1.5 mL) 3 - 10...
Page 855 Operation flow chart The flow chart is shown in the figure below. Each frame is used as follows. : Indicates a key operation. : Indicates a status. IDLE Sequential program IDLE key input POWER ON stops. awaited STOP START Measurement Sequential program continues till end of Initialization...
Page 856: Analyzing Operation
3.2.2 Analyzing Operation Routine analysis operation Make sure the pump, column, detector, data processing unit, etc. are correctly connected, and then set the mobile phase and detergent. Check that the waste bottle is not filled with waste solution. Start the pump and wait until the flow path is filled with the mobile phase.
Page 857 Sequential program setting (a) Setting method As a method of setting a sequential program, the setting procedure is shown below on the following conditions; analysis time 5 minutes and injection of 120 samples of 10 μL each sequentially once. STEP RACK VIAL VOL(µL) TIME 10.0...
Page 858 (continued) STEP RACK VIALS VOL(µL) TIME 1-120 10.0 Input the number of injections from each vial. 1 ENT STEP RACK VIALS VOL(µL) TIME 1-120 10.0 Input a cycle time (min). 5 ENT STEP RACK VIALS VOL(µL) TIME Repeat input by the same method as for STEP1. When pressing the ESC key, the monitor screen reappears.
Page 859 (c) STEP inserting method A new STEP can be inserted in a sequential program. STEP RACK VIALS VOL(µL) TIME 1- 1 10.0 Display a step where an insertion is desired and press the INSERT key. STEP RACK VIALS VOL(µl) TIME A new step is inserted.
Page 860 (e) Editing of under execution For editing a sequential program under execution, set the PAUSE status, and then editing will be allowed. However, a step which has already been executed or under execution cannot be edited. This is indicated by an asterisk “∗” appearing under the initial character S of STEP.
Page 861 Operating condition setting Use the UTLTY key to set it. STEP RACK VIAL VOL(µL) TIME 10.0 UTILTY UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTHERS=4) Under this display, a parameter is selectable and its contents are settable as you desire. 3 - 17...
Page 862 (a) Sequential parameter The sequential parameter is settable in the following procedure. UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTHERS=4) 1 ENT SEQ PARAM (START STEP=1, ALL END=2, OPERATION=3, INJ TIMING=4) 1 ENT START STEP (1-100) Input the start step (for start from a halfway step in a sequential program).
Page 863 (continued) 1 ENT USE ERROR OUT (YES=1, NO=0) The ALL END signal will be output in ERROR OUT on the e-Line. When ALL END “YES” is set, the ALL END signal is output to the option input/output circuit board irrespective of this setting. For output in ERROR OUT, select “1”...
Page 864 (continued) 2 ENT INJ.METHOD (CUT=1, ALL=2, LOOP=3) Select an injection method. 1 ENT LEAD VOLUME (0.0-300.0) µL 30.0 Input a lead volume. 30 ENT REAR VOLUME (0.0-300.0) µL 30.0 Input a rear volume. 30 ENT Monitor screen reappears. 2 ENT FEED VOLUME (0.0-500.0) µL 30.0 Input a feed volume.
Page 865 (continued) 3 ENT APL PARAM (SYR SPD=1, NEEDLE SPD=2, SYR VOL=3, AIR VOL=4) Select an operation condition. 1 ENT ASP SYRINGE SPEED (1-5) Set a syringe speed to aspirate a sample according to the sample viscosity. Set a slow syringe speed for a high-viscosity sample.
Page 866 (continued) 2 ENT NEEDLE DOWN SPEED (SLOW=1, FAST=2) Input a needle lowering speed. Usually, set “FAST.” For using a hard septum, “SLOW” should be set. Needle Down Speed Speed SLOW 30 mm/s FAST 150 mm/s NOTE: When the slow needle down speed is selected, the needle is apt to be broken due to a strong falling force.
Page 867 (continued) 4 ENT INJ TIMING (NO USE=0, USE=1) Sample injection timing can be synchronized with pump action. Reproducibility on retention time can be enhanced. 1. For using this function, it is required to NOTES: combine the autosampler with the Chromaster 5110 pump. If the autosampler is combined with any other model of pump, the INJECTION TIMING error will be issued.
Page 868 (b) Rack parameter Set the shape of the applied rack as a parameter. Contents of rack parameters Rack Parameter X1 : X coordinate of first vial within 55.0 to 180.0 mm Y1 : Y coordinate of first vial within 0.0 to 155.0 mm X2 : X coordinate of last vial within 55.0 to 180.0 mm...
Page 869 Sampling order Pattern code: 2 Pattern code: 3 Pattern code: 4 pattern code: 1 Pattern code: 5 Pattern code: 6 Pattern code: 7 Pattern code: 8 NOTE: The coordinate position indicated in the fig.3-5 determines rack parameters for X1 (X coordinate of first vial), Y1 (Y coordinate of first vial), X2 (X coordinate of last vial), Y2 (Y coordinate of last vial).
Page 870 (ii) Rack parameter setting procedure The rack parameter is settable in a numerical input method or in the robotic mode where the needle is actually moved for adjustment. UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTERS=4 2 ENT RACK CODE (1-16) 1 ENT Input the code of the rack which parameter is to be set.
Page 871 (continued) Y2 (0.0-155.0) mm 148.5 Input the Y2 coordinate. 148.5 ENT Ny (1-40) 12 ENT Z (0.0-53.0) mm 34.0 34 ENT PATTERN CODE (1-8) 5 ENT Monitor screen reappears 2 ENT Nx (1-40) Input an Nx value. 10 ENT Ny (1-40) Input an Ny value.
Page 872 (continued) RACK SET (X1=57.1, Y1=0.0) mm ∗X=57.1 Y=0.0 Z=0.0 Adjust the leading vial position in the following way. The needle moves to the X1/Y1 position of the specified rack code. The Z position is relocated at the uppermost point. (ii) Move “∗” to X by the SELECT key and adjust X by moving the needle using arrow keys.
Page 873 (continued) RACK SET (X2=178.6, Y2=148.5) mm ∗X=178.6 Y=148.5 Z=0.0 Adjust the last vial position in the following way. The needle moves to the X2/Y2 position of the specified rack code. The Z position is relocated at the uppermost point. (ii) Move “∗”...
Page 874 (c) Wash parameter Manual wash time UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTHERS=4) 3 ENT WASH PARAM (MANUAL WTIME=1 INJ WTYPE=2, INJ WTIME=3) MANUAL WTIME : Setting the washing time to be arranged by pressing the WASH key. INJ WTYPE : Setting the washing conditions during execution of a sequential program.
Page 875 (continued) 3 ENT PUMP PLUNGER WASH TIME (1-999) s Input a pump plunger wash time 15 ENT Monitor screen reappears Injection wash type UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTHERS=4) 3 ENT WASH PARAM (MANUAL WTIME=1 INJ WTYPE=2, INJ WTIME=3) MANUAL WTIME : Setting the washing time to be arranged by pressing the WASH key.
Page 876 iii) Injection wash time UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTHERS=4) 3 ENT WASH PARAM (MANUAL WTIME=1 INJ WTYPE=2, INJ WTIME=3) MANUAL WTIME : Setting the washing time to be arranged by pressing the WASH key. INJ WTYPE : Setting the washing conditions during execution of a sequential program.
Page 877 (continued) Select the pump plunger 3 ENT PUMP PLUNGER WASH TIME (1-999) s Input a pump plunger wash time 15 ENT Monitor screen reappears (d) Others UTILITY (SEQ=1, RACK=2, WASH PARAM=3, OTHERS=4) 4 ENT OTHERS (LEAK SENSOR=1, VIAL SENSOR=2 ERROR OUT=3, BUZZER=4, INJ 1 ENT LEAK SENSOR (OFF=0, ON=1) ON is selected when restart the instrument...
Page 878 (continued) In execution of a sequential program, it is terminated without indication of “NO TUBE” on the UI pad. (In cases where ALL END OUT is set to “1” (YES), the ALL END processing is carried out.) Only in cases where ALL END OUT is set to “1” (YES) and ERROR OUT is set to “1”...
Page 879 Confidence-level reporting This autosampler incorporates the confidence-level reporting function for analysis to be carried out while checking data reliability. For using this function, press the GLP key. STEP RACK VIAL VOL(µL) INJ TIME [I] 10.0 GLP (LOGBOOK=1, KEY LOCK.=2) Input “LOGBOOK” for selecting a logbook which records maintenance information or “KEY LOCK”...
Page 880 (continued) 2 ENT INJ. PORT SEAL CHANGE (MM DD YYYY) <1–12> 2000 Input the month of replacement. 6 ENT INJ. PORT SEAL CHANGE (MM DD YYYY) <1–31> 2 2000 Input the date of replacement. 2 ENT INJ. PORT SEAL CHANGE (MM DD YYYY) <2000-2100>...
Page 881 (continued) 2 ENT INJ. VALVE SEAL CHANGE (MM DD YYYY) <1-12> 2000 Input the month of replacement. 6 ENT INJ. VALVE SEAL CHANGE (MM DD YYYY) <1-31> 1 2000 Input the date of replacement. 2 ENT INJ. VALVE SEAL CHANGE (MM DD YYYY) <2000-2100>...
Page 882 (continued) 2 ENT SYRINGE CHANGE (MM DD YYYY) <1-12> 2000 Input the month of replacement. 6 ENT SYRINGE CHANGE (MM DD YYYY) <1-31> 1 2000 Input the date of replacement. 2 ENT SYRINGE CHANGE (MM DD YYYY) <2000-2100> 2000 Input the year of replacement. Upon completion of all the inputs up to year, the logbook is reset.
Page 883 (continued) 2 ENT S.VALVE SEAL CHANGE (MM DD YYYY) <1-12> 2000 Input the month of replacement. 6 ENT S.VALVE SEAL CHANGE (MM DD YYYY) <1-31> 1 2000 Input the date of replacement. 2 ENT S.VALVE SEAL CHANGE (MM DD YYYY) <2000–2100>...
Page 884 (continued) 2 ENT WASHING PUMP CHANGE (MM DD YYYY) <1-12> 2000 Input the month of replacement. 6 ENT WASHING PUMP CHANGE (MM DD YYYY) <1-31> 1 2000 Input the date of replacement. 2 ENT WASHING PUMP CHANGE (MM DD YYYY) <2000–2100>...
Page 885 Functions Each mechanism can be moved for maintenance such as replacement of the needle or injection port seal. (a) TUBE The needle can be moved to the vial position, injection port, wash port and needle replacement position. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC...
Page 886 (continued) TUBE (RACK CODE VIAL NO.) <0-2> Input a vial number. 0: Wash port 1: Injection port 2: Needle replacement position 2 ENT Wash port and Injection port is MOVING WAIT! The needle moves to the specified position. PRESS FUNC KEY OR IDLE KEY FUNC IDLE MOVING...
Page 887 NOTE: When the input value of vial number exceeds the “n” value set as a rack parameter, an error of [CHECK VIAL NO.] will occur, even if it is in the input range of 1 to 500. (b) MOVE The needle can be moved to the specified coordinates. STEP RACK VIAL VOL(µL) INJ TIME 10.0...
Page 888 (c) HEIGHT The needle can be moved to the specified height. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC FUNC (TUBE=1, MOVE=2, HEIGHT=3, SYR=4, VALVE=5, SVALVE=6, SPURGE=7, WPUMP=8) 3 ENT HEIGHT SPEED) <0.0-53.0> Input a desired height. e.g.) 14.5 ENT HEIGHT SPEED) <1-2>...
Page 889 (d) SYR The syringe can be moved to the specified volume position. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC FUNC (TUBE=1, MOVE=2, HEIGHT=3, SYR=4, VALVE=5, SVALVE=6, SPURGE=7, WPUMP=8) 4 ENT SYRINGE (VOLUME(µL) SPEED) <0-690.0> Input a desired volume up to which the syringe is to be moved.
Page 890 NOTE: When an input value of VOLUME exceeds the syringe capacity set as SYRINGE VOL in UTILIITY, an error of [CHECK TOTAL VOL.] will occur. NOTE: The syringe moves to the specified volume position. The syringe valve position will be switched over automatically according to the syringe movement.
Page 891 (e) VALVE The injection valve can be operated. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC FUNC (TUBE=1, MOVE=2, HEIGHT=3, SYR=4, VALVE=5, SVALVE=6, SPURGE=7, WPUMP=8) 5 ENT VALVE (INJECT=0, LOAD=1) Select an injection valve position. 1 ENT MOVING WAIT! Injection valve position is now shifted. PRESS FUNC KEY OR IDLE KEY FUNC IDLE...
Page 892 SVALVE The syringe valve position can be switched. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC FUNC (TUBE=1, MOVE=2, HEIGHT=3, SYR=4, VALVE=5, SVALVE=6, SPURGE=7, WPUMP=8) 6 ENT SVALVE (RINSE PORT=1, NEEDLE=2, SYRINGE=3, PUMP PLUNGER=4) Select a port to which the syringe valve is to be switched.
Page 893 (g) SPURGE Syringe purging can be performed. The wash fluid a syringe aspirated is discharged to the port4 side of the syringe valve. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC FUNC (TUBE=1, MOVE=2, HEIGHT=3, SYR=4, VALVE=5, SVALVE=6, SPURGE=7, WPUMP=8) 7 ENT SYRINGE PURGE (STROKES SPEED)
Page 894 (h) WPUMP The wash pump can be operated. STEP RACK VIAL VOL(µL) INJ TIME 10.0 FUNC FUNC (TUBE=1, MOVE=2, HEIGHT=3, SYR=4, VALVE=5, SVALVE=6, SPURGE=7, WPUMP=8) 8 ENT WPUMP PURGE (OFF=0, SOLV1=1, SOLV2=2) Select the purging state of a wash pump. 0: OFF 1: Wash fluid1 is purged 2: Wash fluid2 is purged.
Page 895 Setup Processing You can select use or nonuse of the thermostat (option), and set LCD contrast of the UI pad. (a) Selection of use or nonuse of thermostat (option) UTLTY POWER ON （SET UP） Turn on power supply with the UTLTY key held down. SETUP: THERMO UNIT CONTRAST S.NO.(A/S) NO USE 02AB-111...
Page 896 (b) Setting of LCD contrast of UI (pad) UTLTY POWER ON （SET UP） Turn on power supply with the UTLTY key held down. SETUP: THERMO UNIT CONTRAST S.NO.(A/S) NO USE 02AB-111 Indicates a serial No. (product No.). SETUP ITEMS (THERMO UNIT=1, CONTRAST =2) 2 ENT LCD CONTRAST (1-7) Enter a contrast level.
Page 897 Thermostat Conditions need to be set when the thermostat (option) is connected. NOTE: THERMO key operation is ineffective when the thermostat is not connected or its use is not set. (a) Temperature setting A set temperature can be input. STEP RACK VIAL VOL(µL) INJ TIME 10.0 THERMO...
Page 898 (b) Temperature calibration If there is a difference between the indicated temperature of the thermostat and the actual temperature of the liquid in a sample vial, it can be corrected by setting of temperature calibration. In case the indicated temperature of the thermostat is 10.0 °C and the actual temperature of the liquid in a sample vial as measured with a calibrated thermometer is 10.5 °C, the difference correction value...
Page 899 1. Be sure to measure the liquid temperature with a NOTES: calibrated thermometer before execution of a temperature calibration. 2. A difference from the liquid temperature in a sample vial varies slightly with the set temperature. For temperature calibration, it is recommended to determine the difference at the set temperature to be used most frequently.
Page 900 (c) Selection of tolerance setting (USE TOLERANCE) Condition for reaching the temperature ready status can be set. STEP RACK VIAL VOL(µL) INJ TIME 10.0 THERMO THERMO UNIT (SET TEMP=1, CALIBRATION=2, TOLERANCE=3, SERIAL NO.=4) 3 ENT USE TOLERANCE (YES=1, NO=0) 0 ENT 1 ENT TOLERANCE (2-15) °C Set the tolerance range.
Page 901 (d) Display of program No. and serial No. The program No. and serial No. (product No.) of the thermostat can be indicated. STEP RACK VIAL VOL(µL) INJ TIME 10.0 THERMO THERMO UNIT (SET TEMP=1, CALIBRATION=2, TOLERANCE=3, SERIAL NO.=4) 4 ENT THERMO UNIT: PROGRAM NO.
Page 902: Shutdown Operation
3.3 Shutdown Operation (1) In the following cases, the autosampler will carry out a shutdown operation, and returns to the idle state. ▪ Analyses of all specified vial numbers have completed. ▪ A vial is not detected while the vial detector is in the ON state.
Page 903: Before Performing Analysis
3.4 Before Performing Analysis This chapter describes the basic items to be careful about before starting analysis. WARNING Ignition of Flammable Chemicals This instrument is not explosion-proof. In unattended operation, do not use organic solvents having a flash point below 70 °C. Be aware of ignition hazard when using flammable chemicals such as organic solvents.
Page 904 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 905: Selection Of Mobile Phase And Cautions On Handling
3.4.1 Selection of Mobile Phase and Cautions on Handling Be careful about restriction on use due to characteristics and temperature of mobile phase to be used. (See Table 3-5 Characteristics of Organic Solvents) Mobile phase (a) When performing high sensitivity analysis with a UV detector, use solvents whose UV absorption characteristics are especially small.
Page 906 (b) Two types of wash fluids are applied to the autosampler. Select a wash fluid according to Table 3-3 for Isocratic analysis, and Table 3-4 for Gradient analysis. (c) When using one wash fluid that fills the washing requirements, the wash fluid1 side must be used. (Can’t use the wash fluid2 only) In this case, when an aqueous solvent is applied to the wash fluid2 side, it can be used as a plunger seal washing of the mobile...
Page 907 Table 3-2 Reagents for Mobile Phase that may be Restricted Usable reagents Usable, if it is 50% Usable, if it is 10% or Unusable reagents for or lower lower SUS316 Phosphoric acid Acetic acid Disodium phosphate Ammonium chloride Sodium phosphate Ammonium citrate Ammonium formate Potassium chloride...
Page 908: Degassing Of Mobile Phase And Wash Fluid
3.4.2 Degassing of Mobile Phase and Wash Fluid NOTE: For using an ultrasonic cleaner or the like, refer to the instruction manual of each instrument. For attaining the full performance of the autosampler, perform constant online degassing for the mobile phase and wash fluid by using a degassing unit.
Page 909: Removing Dust From Mobile Phase And Wash Fluid
3.4.3 Removing Dust from Mobile Phase and Wash Fluid There are various ways to remove dust from mobile phase. Remove dust in the way suitable for the purpose of use. Example of Filtering of Mobile Phase by Using Membrane Filter Removing dust and degassing can be performed simultaneously by filtration with a 0.45 μm membrane filter.
Page 910: Characteristics Of Organic Solvents
3.4.4 Characteristics of Organic Solvents Characteristics of organic solvents as mobile phase for liquid chromatograph are shown in Table 3-5. Use it for reference. WARNING Ignition of Flammable Chemicals This instrument is not explosion-proof. In unattended operation, do not use organic solvents having a flash point below 70 °C.
Page 911 WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 912 Table 3-5 Characteristics of Organic Solvents Polarity Viscosity Refractiv UV cut Flash Ignition point Vapor Boiling Specific (cP20 ° C) e index off (nm) point density point gravity ° C Lower Upper ( ° C) ( ° C) (Air: 1) (Water: 1) limit limit...
Page 913 NOTE: For using organic solvents as mobile phase 1. When using organic solvents, be careful about UV cut off wavelength. UV cut off wavelength: Light cannot be transmitted in the range shorter than this wavelength. e.g) Cut off wavelength of chloroform is 245 nm. Chloroform cannot be used in the range shorter than 245 nm (e.g.
Page 914: Cautions On Static Electricity
3.4.5 Cautions on Static Electricity WARNING Ignition of Flammable Chemicals by Static Electricity 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. Since flammable organic solvents are used for the High Speed Liquid Chromatograph, be careful about heat and fire.
Page 915: Preparatory Operations
3.5 Preparatory Operations 3.5.1 Cautions on Measurement (Handling) Cautions on displacement of mobile phase/wash fluid Before attempting to exchange the mobile phase/wash fluid with a different kind of mobile phase/wash fluid, make sure that the liquid currently used and the liquid to be used are mutually soluble.
Page 916: Sample Pretreatment
condition as salt precipitation or development of algae or microbes. To prevent this condition, be sure to carry out the above procedure before leaving the autosampler unused for a long time. While the autosampler is stopped, air will dissolve into the residing solution through the Teflon material of the connection tubing.
Page 917: Preparatory Operations Of Autosampler Proper
(b) Example of Removing Foreign Matter from Sample For example, when analysis is performed with a reversed phase column (e.g. ODS column), foreign matter can be removed as follows. Take sample into a syringe, attach a normal phase cartridge, and perform filtering.
Page 918 Start the pump to fill the flow paths in the pump and autosampler with liquid. Before a new connection to the column, fill the flow path with the mobile phase, and then connect a tube in order to prevent air bubbles from entering the column.
Page 919: Precautions On Handling
3.6 Precautions on Handling Solvent Displacement and Washing in Flow Path For displacement in the flow path, mutually soluble solvents should be used. (Be sure to perform solvent displacement in the detector cell and sample injector flow path also.) For washing in the flow path, take the same procedure. If a rapid replacement is made, salt precipitation may occur to cause clogging.
Page 920 solvent before use. For measurement, select a wavelength having less absorption. It is recommended to use a solvent specifically prepared for high-speed liquid chromatography. (b) Be sure to be deaerated when an organic solvent is used. Ultrasonic cleaner Aspirator Absorbance Wavelength Cleaning of Micro-syringe (a) After and before sampling, wipe off the needle of a...
Page 921 resulting in an adverse effect on operation. When securing the Teflon tube and SUS pipe, observe the following instructions. (a) Finger-tighten the setscrew (made of resin). (b) Referring to 6.2, fasten the setscrew (made of SUS) so that liquid leakage will not occur. Setscrew Finger-tighten the (made of resin)
Page 922: Maintenance
4. MAINTENANCE 4.1 Checking the Performance and Specifications Performance checking method is explained here. 4.1.1 Preparation of Items The following items are required for performance check. Component Units of Liquid Chromatography System • Pump (Chromaster 5110 or equivalent) • Detector (Chromaster 5410 or equivalent) •...
Page 923: Preparation Of Operation
NOTE: Be sure to use the sample vials, caps and septa recommended by Hitachi High-Technologies (refer to 6.3) If other parts are used, the instrument may malfunction or its original performance may not be available.
Page 924 Detector (wavelength 265 nm, time constant 0.1 s) Oven (40 °C) Waste solution bottle Load resistance coil of stainless pipe 0.25 mm ID × 20 m Autosampler (Injection valve) （注入バルブ） (Wash pump) Pump Waste solution bottle Mobile Wash phase fluid Degassing unit...
Page 925 After confirmation of the above steps, connect the mobile phase to the pump, and the detergent to the autosampler. Be sure to use the mobile phase and detergent of the same production lot. Start the pump to fill each flow path in the pump and autosampler with liquid.
Page 926: Reproducibility Check
(13) Input the following contents as instrument conditions. RACK CODE:1 SYRINGE SPEED:1 RACK PARAM:RACK CODE = 1 X1 = 57.1 X2 = 178.6 Nx = 10 Y1 = 0.0 Y2 = 148.5 Ny = 12 Z = 34 P = 5 INJ.METHOD: CUT LEAD VOLUME: 30.0 REAR VOLUME: 30.0...
Page 927 Press the WASH key of the autosampler, and select NEEDLE side to fill the needle and the injection port with wash fluid1. (When two wash fluids are used, replace the wash fluid2 side with fresh one). Fill the buffer tube with deaerated wash fluid while flushing the needle and the injection tube.
Page 928 NOTE: Close the front door (refer to Fig. 2-1, (L) and (R)) when a sample vial is set. Avoid rapid changes in ambient temperature, and not exposed to drafts such as an air conditioner. These may influence the analysis result which reproducibility with high precision required.
Page 929: Periodic Maintenance
4.2 Periodic Maintenance Estimated periodic maintenance is based on full operation of 8 hours daily and 20 days monthly with standard assay. Check Item Frequency Procedure Liquid leak check Daily Refer to 4.2.1 Washing the flow path As required Refer to 4.2.2 Cleaning As required Refer to 4.2.3...
Page 930 When using a saline solvent When a saline solvent is used as a mobile phase, salt may precipitate in the flow path to clog it or scratch the seal face of valve. After using such a solvent, wash the flow path adequately with distilled water.
Page 931 Leak sensor operation check To check the operation of the leak sensor, drip a droplet of water (H O) to the leak sensor tip in contact with the drain reservoir. Leak sensor Leak sensor set screw Drip a droplet Fig. 4-2 Leak Sensor NOTE: Refer to the following for more information about the leak sensor.
Page 932: Drain Tray
4.2.6 Drain tray WARNING Inflammation or Injury due to Toxic, Corrosive or Stimulative Solvent When using a toxic, corrosive or stimulative solvent, be careful not to incur a physical inflammation or injury. For details of the properties of each solvent and how to handle it, refer to the relevant Material Safety Data Sheets (MSDS).
Page 933: Positioning The Mechanism
4.3 Positioning the Mechanism 4.3.1 Cleaning and positioning the wash port After wash port cleaning, adjust it to the correct location. Turn on power supply to the autosampler. Fig. 4-3 Front View Using the MOVE command on the UI pad, move the needle so that the wash port can be removed easily.
Page 934 Wash port cover Retaining screw 2 Retaining screw 1 Fig. 4-4 Remove of the Wash Port Loosen the retaining screws 1 and 2, and remove the wash port. Other screws should not be loosened. Replace it with a new wash port. Or carry out ultrasonic cleaning.
Page 935 Using the HEIGHT command, lower the needle by about 5 mm. FUNC ENTER ENTER ENTER Retaining screw 1 Retaining screw 2 Retaining screw 1 Fig. 4-5 Height Adjustment of Needle 4 - 14...
Page 936 Check that the wash port is located just below the needle. When it is not correct location, return to the procedure (2) to readjust the wash port and fix it temporarily. (10) When the wash port is located just below the needle, move the needle once again (refer to (2)) and fix the washing port.
Page 937: Troubleshooting
4.4 Troubleshooting 4.4.1 Troubleshooting Table If an abnormal phenomenon is encountered, reference should be made to the following table. Table 4-2 Troubleshooting Symptom Cause Remedy Error is a. Improper measuring a. Perform correct operation indicated on the conditions are entered or according to the message display.
Page 938 Table 4-2 Troubleshooting (continued) Symptom Cause Remedy Reproducibility h. The detergent bottle is h. Wash the bottle and replace of analytical contaminated. the detergent. result is poor. i. The sample vial or septum is i. Replace the vial or septum. contaminated.
Page 939 Table 4-2 Troubleshooting (continued) Symptom Cause Remedy Carryover a. The flow path is a. Wash the flow path. occurs. contaminated. b. The injection port seal leaks. b. Check the lock nut and retighten if loose. Or replace the seal. c. The detergent bottle is c.
Page 940: Error Messages
Remedy ROM ERROR PC board malfunctions. Turn on power supply again. If the same error is indicated RAM ERROR again, contact your nearest LOG_INFORMATION service office of Hitachi High- ERROR Technologies Corporation sales EEPROM ERROR representative. PARAMETER ERROR COMMUNICATION Communication is abnormal.
Page 941 (Note: In execution of 2. The clearance between 2. Contact your nearest service a sequential program, the top face of sample vial office of Hitachi High- it is terminated and the detection lever is Technologies Corporation without indication of inappropriate. Or the sales representative.
Page 942 3. Remove the obstacle. the moving route of syringe (vertically). 4. The electric system 4. Contact your nearest service malfunctions. office of Hitachi High- Technologies Corporation sales representative. ERROR-SVALVE 1. The syringe valve seal has 1. Replace the seal. worn out.
Page 943: Thermostat (Option) Errors
THERMO UNIT ROM PC board malfunctions. Turn on power supply again. ERROR If the same error is indicated again, contact your nearest THERMO UNIT RAM service office of Hitachi High- ERROR Technologies Corporation sales THERMO UNIT representative. PARAMETER ERROR THERMO UNIT TIME Communication is Turn on power supply again.
Page 944: Parts Replacement
5. PARTS REPLACEMENT 5.1 Consumables and Spare Parts 5.1.1 Consumables The following parts are consumables. They must always be on hand. The amount of consumption of each item is based on the assumption that the autosampler is operated 240 days per year, 8 hours per day, and 15 minutes per analysis.
Page 945: Spare Parts
Table 5-1 Consumables (continued) Location Standard Part No. Name Form / Specification (Estimated Life) Life 893-0812 Injection Injection valve 10,000 valve seal (One year) switchings φ12 893-0813 Syringe valve Syringe valve 40,000 stator (Two years) switchings φ34 893-0814 Syringe valve Syringe valve 20,000 seal...
Page 946: Fastening Of Sus Pipe
5.2 Fastening of SUS Pipe Item to be prepared: Wrench (1/4 inches) In connection of the SUS pipe, fasten it in the following manner. Attach the SUS setscrew and screw it in with your hand until it is finger-tight. Using a wrench (1/4 inches), re-tighten the SUS setscrew (with a tightening torque of 4 [N•m]) so that it will be secured firmly.
Page 947: Replacement Of Injection Port Seal
5.3 Replacement of Injection Port Seal The injection port seal should be replaced periodically every about 10,000 sample injections as a standard. Items to be prepared: Injection port seal (P/N 893-0810) Seal remover (P/N 893-2115) Loosen the injection port with your hand. And remove it from the injection valve.
Page 948 Put a new injection port seal into the injection port. Attach it to the injection valve, and tighten it up with your hand. Injection port Injection port seal Turn the taper part of the injection port seal to the injection side when attach it.
Page 949: Needle Replacement
5.4 Needle Replacement Items to be prepared: Wrench (5/16 inch, 12 mm) Flange needle (P/N 893-0816) Detach a sample rack from the rack tray. Using the UI pad, move the needle to the replacement position. FUNC ENTER ENTER ENTER (Refer to 3.2.2 Analyzing Operation (5) Functions (a) TUBE for details.) Using a wrench (5/16 inch) to remove the flange needle while holding the screw on the needle joint side with wrench...
Page 950 Pull out the needle downward with your hand. Attach a new flange needle to the needle joint with your hand temporarily. Using a wrench (5/16 inch) to attach the flange needle while holding the screw on the needle joint side with wrench (12 mm).
Page 951: Syringe Replacement
5.5 Syringe Replacement Items to be prepared: Hypodermic syringe A tube between a syringe and a syringe valve Syringe, Beaker, Distilled water, Wash fluid Syringe (175 µL) (P/N 893-0815) Syringe (70 µL) (P/N 893-0817)(option) Remove the sealing screw connected to the port 4 of the syringe valve.
Page 952 Connect the provided hypodermic syringe to the port4. Hypodermic syringe Fig. 5-7 Connecting the Hypodermic Syringe (or Tube) Using the SYR command, aspirate 175 µL of wash fluid. FUNC ENTER ENTER ENTER (Refer to 3.2.2 Analyzing Operation (5) Functions (d) SYR for details.) NOTE: When 70 µL optional syringe is used, using the SYR command, aspirate 70 µL of wash fluid.
Page 953 Before mounting a new syringe, put distilled water (or wash fluid) into it. Avoid air bubbles in the plunger. Plunger Fill the syringe with distilled water by pulling the plunger. Syringe Distilled water (or wash fluid) Beaker Fig. 5-8 Filling with Distilled Water Mount the syringe (secure the top screw after engaging the plunger groove with the hook).
Page 954 2. If the syringe is not filled with liquid, it lacks lubricity. Therefore, the syringe may not move normally. 3. Securely screw the syringe manually to the valve. Incomplete screwing may deteriorate joint sealing and cause poor performance. 4. During replacement of the syringe, do not move the hook forcedly.
Page 955: Discharge Of Air Bubbles From Syringe
5.6 Discharge of Air Bubbles from Syringe Items to be prepared: Hypodermic syringe A tube between a syringe and a syringe valve Remove the sealing screw from port5 of the syringe valve. Syringe valve Sealing screw Fig. 5-10 Syringe Valve Connect the hypodermic syringe (furnished plastic injector) to port4.
Page 956 Using the PWASH command, aspirate 500 µL of wash fluid and discharge it though port 5. FUNC ENTER ENTER (Refer to 3.2.2 Analyzing Operation (5) Functions (g) SPURGE for details.) In the use of the hypodermic syringe (plastic injector), press the syringe with your finger to apply proper pressure when wash fluid is discharged through port4.
Page 957 When the plunger of the syringe moves Syringe valve upward, press the hypodermic syringe with your finger to exert proper pressure onto the inside of the cell for a moment and then release it immediately. Hypodermic syringe Fig. 5-12 Discharge of Air Bubbles from Syringe with Hypodermic Syringe The hypodermic syringe can be stored in the wall of the autosampler using the provided pipe holder.
Page 958 Fit in the body of the hypodermic syringe to the pipe holder. Put the tube from syringe valve port 4 to the downside, and the piston to the upper side. Fig. 5-14 Fitting the Hypodermic syringe 5 - 15...
Page 959: Replacing The Injection Valve Seal
5.7 Replacing the Injection Valve Seal NOTE: Before proceeding to replacement of the injection valve seal, be sure to stop the back flush pump. Items to be prepared: Hexagonal wrench (9/64 inch, This wrench is attached to P/N 893-0812) Wrench (1/4 inch) Injection valve seal (P/N 893-0812), Using a wrench (1/4 inch), disconnect the tubes and pipes from the injection valve port 1 to 5.
Page 960 Detach the injection valve seal from the unit. Unit Injection valve seal Injection valve stator Stator ring Stator setscrew Fig. 5-16 Removal of Injection Valve In the reverse order of removal, attach a new injection valve seal, the stator ring, and the injection valve stator. Then tighten the stator setscrews.
Page 961: Replacing The Syringe Valve Seal
5.8 Replacing the Syringe Valve Seal Items to be prepared: Hexagonal wrench (9/64 inch, This wrench is attached to P/N 893-0814) Syringe valve seal (P/N 893-0814) Disconnect the tubes from the syringe valve with your hand. Port 1 : Tube SV1 Port 2 : Buffer tube Port 3 : Tube SV3 Port 4 : Sealing screw...
Page 962 Detach the injection valve seal from the unit. Unit Injection valve seal Injection valve stator Stator ring Stator setscrew Fig. 5-18 Removal of Syringe Valve Stator In the reverse order of removal, attach a new syringe valve seal, the stator ring, and the syringe valve stator. Then tighten the stator setscrews.
Page 963: Purging The Wash Pump
5.9 Purging the Wash Pump Using the WPUMP command, deliver wash fluid1 for about 3 minutes to replace the fluid of the flow path between the solvent filter and the wash port with the wash fluid1. FUNC ENTER ENTER (Refer to 3.2.2 Analyzing Operation (5) Functions (h) WPUMP for details.) NOTES: To suspend delivering of the wash pump, select...
Page 964: Discharge Of Air Bubbles From Wash Pump
5.10 Discharge of Air Bubbles from Wash Pump Items to be prepared: Hypodermic syringe A tube between a hypodermic syringe and a syringe valve Syringe, Beaker, Distilled water, Wash fluid Remove a setscrew from the port1 of the syringe valve with your hand.
Page 965 Connect the provided hypodermic syringe to the port1. Hypodermic syringe Fig. 5-18 Connecting the Hypodermic Syringe (or Tube) Using the WPUMP command, deliver wash fluid1 to replace the fluid of the flow path between the solvent filter and the wash port with the wash fluid1. FUNC ENTER ENTER...
Page 966: How To Wash Solvent Filter
5.11 How to Wash Solvent Filter The solvent filter (filter for wash fluid bottle) should be washed in the following procedure. Items to be prepared: Beaker, Wash fluid (2-propanol) Ultrasonic cleaner, Distilled water Loosen the cap of the wash fluid bottle. Inlet tube Wash fluid bottle Pull out the inlet tube from the wash fluid bottle.
Page 967 Fill a beaker with wash fluid (e.g. 2-propanol), and put the solvent filter in it. Perform ultrasonic cleaning for approx. 5 to 6 minutes. Solvent filter Beaker Wash fluid Distilled water Ultrasonic cleaner Then, replace the wash fluid with distilled water, and perform additional ultrasonic cleaning for approx.
Page 968: How To Replace Fuse (In The Optional Thermostat)
5.12 How to Replace Fuse (in the optional thermostat) WARNING Electric Shock due to Contact with Inside of Instrument When replacing the fuse with a new one, be careful not to receive an electric shock. To prevent this, be sure to turn off the power switch before proceeding to fuse replacement.
Page 969: Accessories
6. ACCESSORIES A wide variety of accessories are available for the Chromaster 5210 Autosampler to meet the specific requirements of the laboratory. 6.1 Thermostat This unit is capable of cooling 120 sample vials (1.5 mL each) within a temperature range from (room temperature - 21) °C to (room temperature + 25) °C, or a setting range.
Page 970: Sample Racks
6.2 Sample Racks Table 6-2 and 6-3 describes the sample racks that can be used with the Chromaster 5210 Autosampler. For using an optional sample rack, rack parameters should be set so as to match that rack. (For details, refer to 3.2.2 (3) (b) and the instruction manual for the optional sample rack.) 6.2.1 Standard Used when a thermostat is unused.
Page 971: Vials
NOTE: Be sure to use the sample vials, caps and septa recommended by Hitachi High-Technologies (indicated in Table 6-4 to 6-11). If other parts are used, the instrument may malfunction or its original performance may not be available.
Page 972 Screw top Vials Table 6-4 Vials 080-3704 855-2351 080-3710 080-3711 080-3595 080-3705 080-3596 890-3674 890-3675 1.5 mL 890-3676 Applicable Part No. Name Specification/Standard Remarks Rack 080-3595 1.5 mL sample vial, Manufactured by Chromacol, Ltd. 892-0230 With blue 500 pcs Vial type: 2-SV, 892-0240 mark φ12 ×...
Page 973 Table 6-5 Vials 080-3704 855-2351 080-3710 080-3711 080-3706 1.1 mL Applicable Part No. Name Specification/Standard Remarks Rack 080-3706 1.1 mL sample vial, Manufactured by Chromacol, Ltd. 892-0230 500 pcs contained Vial typel: 1.1-STVG, 892-0240 φ12 × 32 mm, Pointed-bottom type 855-2351 Septum (Si-TEF), With slit (-)
Page 974 Table 6-6 Vials 080-3702 080-1863 080-3707 080-3701 4 mL Applicable Part No. Name Specification/Standard Remarks Rack 080-3707 4 mL sample vial, Manufactured by Chromacol, Ltd. 892-0232 500 pcs contained Vial type: 4-SV, 892-0242 φ15 × 46 mm 080-3701 4 mL sample vial Manufactured by Chromacol, Ltd.
Page 975 Crimp top Vials Table 6-7 Vials 080-3712 080-3597 080-3768 080-3598 1.5 mL Applicable Part No. Name Specification/Standard Remarks Rack 080-3597 1.5 mL crimp-top Manufactured by Chromacol, Ltd. 892-0230 With blue sample vial, 500 pcs Vial type: 2-CV, mark 892-0240 φ12× 32 mm contained 080-3768 1.5 mL crimp-top...
Page 976 Table 6-8 Vials 080-3712 080-3700 1.1 mL Part No. Applicable Name Specification/Standard Remarks Rack 080-3700 1.1 mL crimp-to Manufactured by Chromacol, Ltd. 892-0230 sample vial, 500 pcs Vial type: 1.1-CTVG, 892-0240 φ12 × 32, contained Pointed-bottom type 080-3712 Crimp cap (with Manufactured by Chromacol, Ltd.
Page 977 Crimp-top Vials A septum is placed in the aluminum crimp cap which is sealed to the vial using the dedicated crimper tool. To remove the cap, use the decapper. Crimper Part No. Name Remarks 080-3232 Crimper CR-8 For sealing of 080-3226 080-3233 Crimper CR-11 For sealing of 080-3227...
Page 978 Neckless Vials Table 6-9 Vials 890-3663 890-3662 890-3665 Applicable Part No. Name Specification/Standard Remarks Rack 890-3661 1 mL neckless Manufactured by 892-0234 With sample vial National Scientific Company, polyethylene 892-0244 (transparent), C4015-96 φ8 × 40 mm 200 pcs contained 890-3664 1 mL neckless Manufactured by With...
Page 979 Table 6-10 Vials 080-3712 Applicable Part No. Name Specification/Standard Remarks Rack 080-1869 Neckless sample Manufactured by 892-0230 With vial (transparent), FUJIMOTO SCIENCE, silicone 892-0240 φ12 × 32 mm set of 100 vials rubber cap 805-2236 Neckless sample Manufactured by Without vial (transparent), FUJIMOTO SCIENCE, silicone...
Page 980 Snap Vials Table 6-11 Vials 890-3670 890-3671 890-3669 890-3687 0.3mL Applicable Part No. Name Specification/Standard Remarks Rack 890-3672 0.3 mL snap-top La-Pha-Pack® 892-0230 With snap sample vial, cap set, 11190933, 892-0240 100 pcs contained 11150637 having φ12 × 32 mm, polypropylene septum (Si-PTFE, without...
Page 981 Otherwise, the instrument performance may be degraded without the microplate seal. NOTE: Be sure to use the microplate recommended by Hitachi High-Technologies. If other microplates are used, its original performance may not be available. 6 - 13...
Page 982: Optional Syringes
6.4 Optional Syringes Table 6-14 shows a list of the optional syringes for the Chromaster 5210 Autosampler. Refer to 5.5 Syringe Replacement for setting of 70 µL syringes. Table 6-14 Optional Syringes Part No. Part Name Remarks 892-0250 70 µL syringe kit Syringe 6.5 Degassing Unit 2ch degassing unit for the Chromaster 5210 Autosampler is...
Page 983: Index
7. INDEX ALL END ..............3-11, 3-18, 4-6 Accessories................6-1 Ambient humidity............2-46, 4-48 Ambient temperature............. 2-46, 4-48 Analysis operation..............3-12 Arm.................. 2-4, 4-20 Assembly.............. APPENDIX1-12 CL (clear) ................. 2-6 Cable connection, Cabling ..APPENDIX1-16, APPENDIX1-18 Cleaning ................... 4-9 Consumables ................5-1 DEL (delete) ..............
Page 984 INSERT ................2-6, 3-15 Idle ..................2-6, 3-2 Initial screen ..........3-2, 3-5, APPENDIX3-1 Injection port .............. 2-4, 2-7, 5-4 Injection port seal ..............5-4 Injection valve ..............2-2, 5-16 Injection valve seal............5-2, 5-16 Isocratic system ..........1-1, APPENDIX1-16 LED ...................
Page 985 RACK PARAM (rack parameters) .......... 3-24 RACK CODE..............3-13, 3-24 Rack holder ............... 3-6, 6-1 Remedy.................. 4-16 Relative Standard Deviation(RSD)........... 4-6 Replacement ................5-1 Reproducibility check ............... 4-5 Reproducibility of injection volume......... 2-44 Routine analysis operation............. 3-12 START ..................2-6 START STEP .................
Page 986 WASH ................ 2-6, 4-4, 5-5 Wash port..............2-3, 2-7, 4-12 Washing condition..............3-30 Waste solution tube ..........3-73, 4-8, 44-9 Weight ..................2-46 Wiring cover, Cable cover ......2-4, APPENDIX1-28 7 - 4...
Page 987: Appendix
If relocation of the instrument becomes necessary after delivery, consult your dealer or nearest Hitachi High- Technologies’s authorized maintenance service agent in order to avoid possible trouble involved in relocation.
Page 988: Appendix 1.2 Place For Installation
Appendix 1.2 Place for Installation For installation of the instrument, select a place which meets the following conditions. Operating temperature: Within 15 to 35 °C and with minimum temperature variation during measurement (±2 °C/h). Utmost care should be used for preventing condensation. Operating humidity: 25 to 85% Atmospheric Gas (a) Adequate ventilation is required.
Page 989 Shall be free from excessive dust. Otherwise, performance degradation might be caused. (g) Shall be free from a sudden change of power supply voltage. Otherwise, noise might be caused. (h) Power supply to motor-driven equipment (such as stirrer and vibrator) without a noise suppressor shall not be turned ON/OFF frequently on the same power supply line as that of this instrument.
Page 990: Appendix 1.3 Items To Be Prepared By Customer
Appendix 1.3 Items to be Prepared by Customer Appendix 1.3.1 Power Supply Arrangement Confirm that the following requirements are satisfied before installing the instrument. Power Supply Power supply voltage : 100 to 240 V AC Fluctuation shall be within ±10% of the rated voltage.
Page 991 WARNING Electric shock due to improper grounding! This instrument is designed in corformity with the specifications of Class I in Annex H of the IEC 61010-1 (International Electrotechnical Commission Standards), Issue 1. To prevent an electric shock hazard, provide a proper grounding connection.
Page 992 (i) Usual grounding connection (with grounded 3P power outlet) Grounded 3P power outlet (15 A) Grounded 3P table tap Chromaster 5210 autosampler Ground resistance 750 mm or 100 Ω or less more below Organizer or ground AC adapter (option) Connector Rear panel Grounding electrode (underground section)
Page 993 (ii) Connection when grounded power outlet is unavailable 2P power outlet (15 A) 3P table tap with grounding wire Chromaster 5210 Grounding autosampler terminal 750 mm or Ground Organizer or more below resistance AC adapter (option) ground 100 Ω or less Connector Grounding wire (green) Rear panel...
Page 994 (b) For the Instrument Provided with Thermostat (i) Usual grounding connection (with grounded 3P power outlet) Grounded 3P power outlet (15 A) Grounded 3P table tap Power cord (attached to instrument) Thermostat Ground resistance 100 Ω or less Connector Grounding electrode (underground section) Chromaster 5210 Grounding construction...
Page 995 (ii) Connection when grounded power outlet is unavailable Grounded 2P power outlet (15 A) Grounded 3P table tap Power cord (attached to Grounding instrument) terminal Thermostat Ground resistance 100 Ω or less Connecto Grounding wire (green) Screw diameter : M4 or larger Turn count 3 or more Grounding electrode...
Page 996 Power outlet with 3P-2P adapter grounding terminal Power cord (attached to the instrument) Thermostat Grounding terminal Connecto Grounding wire (green) Screw diameter : M4 or larger Turn count 3 or more Wire thickness 1.25 mm Chromaster 5210 autosampler Power outlet with grounding terminal 3P-2P adapter Grounding...
Page 997: Appendix 1.3.2 Installation Space
Appendix 1.3.2 Installation Space For composing a liquid chromatograph system with the Chromaster series module units, a space of 540 mm wide (980 mm for stacking the units in two blocks) and 550 mm deep is required at least. Behind each unit, a space of 150 mm or more must be secured.
Page 998: Appendix
Appendix 1.5 Assembling NOTE: It is not permitted for the customer to carry out installation at the time of delivery. For ensuring safety and high accuracy in operation of the instrument, installation of the instrument shall be carried out by qualified service personnel trained by the manufacturer or its authorized maintenance service agent.
Page 999 Fixing bracket Retaining screws Appended Fig. 1-5 Removal of Fixing Brackets APPENDIX 1 - 13...
Page 1000: Appendix 1.5.2 Attachment Of Waste Solution Tube
Appendix 1.5.2 Attachment of Waste Solution Tube Attach the waste solution tube to the waste solution tube mounting port. Waste solution mounting port (a) Before attachment T joint Drain tube A1 I joint Drain tube (b) After attachment Appended Fig. 1-6 Mounting of Waste Solution Tube APPENDIX 1 - 14...
Page 1001: System Power Supply
Appendix 1.5.3 System Power Supply For the Chromaster series, the organizer unit has been prepared. To the organizer (available at option), one Chromaster 5110 pump, one Chromaster 5210 autosampler, one Chromaster 5410/5420/5430/5450 detector and one IFC board can be connected. For the Chromaster 5310 column oven and Chromaster fluorescence detector, the power cord needs to be connected to the column oven unit.
Page 1002 Isocratic System/Low-pressure Gradient System (stacked in one block) Chromaster 5410/5420/ 5430/5450 detector Chromaster 5310 column oven Chromaster 5210 autosampler Interface control board Chromaster 5110 pump To AC power supply Appended Fig. 1-8 Power Cable Connection Diagram Appended Table 1-1 Cables to be Used Connector cable 1) P/N 892-6909 (attached to organizer) Connector cable 2)

Hitachi CHROMASTER 5160 Instruction Manual

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Section 3

Section 4

Section 5

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