Metrohm 750 Autosampler Instructions For Use Manual
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Metrohm 750 Autosampler Instructions For Use Manual

Metrohm 750 Autosampler Instructions For Use Manual

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CH-9101 Herisau/Switzerland
Tel.
++41 71 353 85 85
Fax
++41 71 353 89 01
Internet
www.metrohm.ch
E-Mail
info@metrohm.ch
750 Autosampler
2.750.0020 Instrument version
8.750.1023 Instructions for Use
23.02.2000 / dö

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  • Page 1 CH-9101 Herisau/Switzerland Tel. ++41 71 353 85 85 ++41 71 353 89 01 Internet www.metrohm.ch E-Mail info@metrohm.ch 750 Autosampler 2.750.0020 Instrument version 8.750.1023 Instructions for Use 23.02.2000 / dö...

  • Page 2: Table Of Contents

    2.1.2 Check ....................9 2.1.3 Location................... 9 Connection to IC system................10 2.2.1 750 Autosampler as "Master" ............10 2.2.2 732 IC Detector as "Master" ............11 2.2.3 Connection to 762 with «IC Net» ........... 12 2.2.4 Tubing connection ................ 14 Mains connection ..................15...
  • Page 3 Fig. 5: Rear of 750 Autosampler................... 5 Fig. 6: Connection of 750 Autosampler to 732/733 ........... 11 Fig. 7: Connection of 750 Autosampler to 732/733 and 762 ........13 Fig. 8: Keypad ......................20 Abb. 9: Manual sample filtering ................... 39 Fig.

  • Page 4: Introduction

    128 samples, which are transferred automatically into the sample loop of the 733 IC Separation Center. The 750 Autosampler performs up to four, fixed loop injections per vial at user-selectable time intervals. All operating parameters are entered from the front panel.

  • Page 5: Theory Of Operation

    Theory of operation Displacement principle The 750 Autosampler operates using the positive displacement princi- ple of sample transfer. This sample transfer process into the sample loop of the 733 IC Separation Center is illustrated in Fig. 2. When an in- jection is initiated, the hollow transfer needle 5 5 descends into the vial.

  • Page 6: Fig. 3: Displacement Volume Versus Needle Position

    1.2 Theory of operation Number of injections The number of injections per sample with the 750 Autosampler de- pends on the sample loop size. With sample loops > 10 µL max. 3, with sample loops ≤ 10 µL max. 4 injections are possible. Fig. 3 details the needle position and displacement volume at the sample delivery action.

  • Page 7: Control Elements

    FUNCTION SYSTEM TEMP REM/LOC RUN/STOP PRIORITY CLEAR ENTER Fig. 4: Front of the 750 Autosampler Display (LCD) Transfer needle comprising 4 lines each of 20 characters Keypad Holder for transfer tubing with function, numeric and cursor keys (details see chap. 3.1.2) Sample rack (6.2041.600)

  • Page 8: Fig. 5: Rear Of 750 Autosampler

    1.3 Control elements RS-232 INJECT LOAD IEEE PRINTER EXT PWR CONTROL Fig. 5: Rear of the 750 Autosampler Contact closure strip for valve Mains switch switch to switch the instrument on control details see chap. 5.2.1 and off: I = ON...

  • Page 9: Information On The Instructions For Use

    Information on the Instructions for Use Please read through these Instructions for Use carefully before you put the 750 Autosampler into operation. The Instructions for Use contain information and warnings which must be heeded by the user to assure safe operation of the instrument.

  • Page 10: Notation And Pictograms

    Caution This symbol marks important in- formation. First read the associ- ated directions before you con- tinue. Comment This symbol marks additional in- formation and tips. 750 Autosampler...

  • Page 11: Safety Notes

    Safety notes 1.5.1 Electrical safety While electrical safety in the handling of the 750 Autosampler is assured in the context of the specifications IEC 1010-1 (protection class 1, de- gree of protection IP20), the following points should be noted: • Mains connection...

  • Page 12: Installation

    Setting up the instrument 2.1.1 Packaging The 750 Autosampler is supplied together with the separately packed accessories in special packagings containing shock-absorbing foam linings designed to provide excellent protection. The actual instrument is packed in an evacuated polyethylene bag to prevent the ingress of dust.

  • Page 13: Connection To Ic System

    750 Autosampler is connected to the 733 IC Separation Cen- ter with the 6.2128.100 cable as shown in Fig. 6. In addition the 709 IC Pump can be connected to the 750 Autosampler in such a way that when the pump stops the Autosampler will also be automatically stopped (important for unattended continuous operation).

  • Page 14: 732 Ic Detector As "Master

    733 IC Separation Center with two cables as shown in Fig. 6. In addition the 709 IC Pump can be connected to the 750 Autosampler in such a way that when the pump stops the Auto- sampler will also be automatically stopped (important for unattended continuous operation).

  • Page 15: Connection To 762 With "Ic Net

    When a modular IC system consisting of 732 IC Detector, 733 IC Separation Center, 709 IC Pump, and 762 IC Interface is operated with the PC software «IC Net» as "Master" the 750 Autosampler sample change procedure will be started by a signal from the 733 IC Separa- tion Center.

  • Page 16: Fig. 7: Connection Of 750 Autosampler To 732/733 And 762

    46 (valve B) of the 733 IC Separation Center. The three cable ends are appropriately inscribed with "GND" (white), "FILL" (green) and "INJECT" (brown). 6.2128.130 6.2125.090 (732) 6.2115.070 6.2128.100 6.2134.100 INJECT LOAD 6.2134.090 6.2134.000 Fig. 7: Connection of 750 Autosampler at 732/733 and 762 750 Autosampler...

  • Page 17: Tubing Connection

    2 Installation 2.2.4 Tubing connection For transferring the sample from the 750 Autosampler to the injection valve of the 733 IC Separation Center the following tubing connections must be made: Tubing connection 750 – injection valve • At the 733 IC Separation Center, loosen the rotary nipple...

  • Page 18: Mains Connection

    (50 or 60 Hz) is made automatically by the 750 Autosampler according to the mains voltage and frequency used. Nevertheless, be- fore the 750 Autosampler is switched on for the first time a check should be made as to whether the correct fuses for the intended mains supply have been inserted in the instrument.

  • Page 19: Mains Cable And Mains Connection

    Plug the mains cable into mains connection plug 14 14 of the 750 Auto- sampler (see Fig. 5). 2.3.3 Switching the instrument on/off The 750 Autosampler is switched on and off using mains switch 13 When the instrument is switched on display 1 1 lights up. 750 Autosampler...

  • Page 20: Initial Checkout

    1 of sample rack 3 3 ; then proceed step by step as follows: Switch on 750 Autosampler Switch on 750 Autosampler with mains switch 13 13. The following screen will be displayed after powerup and initialization:...
  • Page 21 2 Installation Start injection Press the <ENTER> key. The 750 Autosampler will make an injection from the vial at position 1. Afterwards the following display will appear: MANUAL INJECTION COMPLETED Select "SYSTEM" Press the <SYSTEM> key (<FUNCTION> + <4>). The fol-...

  • Page 22: Operation

    Fundamentals of operation 3.1.1 Display and instrument dialog The LCD display 1 1 on the 750 Autosampler consists of 4 lines each with 20 characters. After the Autosampler has been switched on and initial- ized the following display appears: READY SELECT A FUNCTION This screen is called the main screen.

  • Page 23: Overview Of Key Functions

    Cursor keys Fig. 8: Keypad The keypad of the 750 Autosampler contains 4 main function keys, 12 numerical keys (incl. <CLEAR>) and 4 cursor keys. In the basic condi- tion the functions given above the numbers can also be activated by pressing the <FUNCTION>...
  • Page 24 3.1 Fundamentals of operation Keys of 750 Autosampler Normal function Function with <FUNCTION> Function key – • Selection of a function in combi- FUNCTION nation with the corresponding numeric key. Run/Stop key – • If no method runs: RUN/STOP Selection and start of a method.
  • Page 25 Cursor key <ß> – • Decrements numerical parameter values. • Moves the display one selection item to the left. Cursor key <à> – • Increments numerical parameter values. • Moves the display one selection item to the right. 750 Autosampler...

  • Page 26: System Settings

    SYSTEM SETTINGS Contact Closures à On the 750 Autosampler there is the possibility of producing four signals in the form of a contact closure on contact closure strip 10 for controlling external instruments: Automatic contact closure at output "START" for every Injection injection triggered by the Autosampler.
  • Page 27 (see section 1.2): POS1,POS2,POS3,POS4 310 µL 590 µL POS1 POS3 450 µL 730 µL POS2 POS4 If sample vessels closed with 6.2743.030 filter stoppers are used then immersion depth " " must not be selected. POS4 750 Autosampler...
  • Page 28 " ", and " " or " ". Month Injection valve SYSTEM SETTINGS Injection Valve à Without function for 750 Autosampler. Status display SYSTEM SETTINGS Status à By pressing <ENTER> the following screen is displayed: Status display Validated 709/50 S/N 03029...

  • Page 29: Manual Rinsing

    Position of sample vial MANUAL INJECTION Sample Vial à Entry of the sample vial position on the sample rack for the desired sample to be injected. 1…128 750 Autosampler...
  • Page 30 MANUAL INJECTION When the injection has been completed the transfer needle COMPLETED remains in the sample vial. Further injections can now be started from the same sample vial, for which a new immer- sion depth must be selected. 750 Autosampler...

  • Page 31: Methods

    METHOD By pressing the <METHOD> key (<FUNCTION> + <7>) the method menu appears. For the 750 Autosampler a method is understood as being a program defined by the operator which proceeds automatically after being started. A maximum of 10 methods with up to 128 program steps each can be stored in the Autosampler.
  • Page 32 The sample series will be skipped. SKIP The sample vials are only used for RINSE rinsing. If sample vials sealed with 6.2743.030 filter stoppers are used then a maximum of only 3 injections per sample vial can be carried out. 750 Autosampler...
  • Page 33 The follow- NONE,EVEN,ODD, QR_E,QR_O ing options can be selected with the < > and à à < > cursor keys: ß ß No rinses. The vials are used as pro- NONE grammed. 750 Autosampler...
  • Page 34 Entry of the number of the program step after Enter Step Number which the new program step is to be inserted. After <ENTER> is pressed a menu with the 10 editable parameters for the program step ap- pears (see under " "). Edit Step à à 750 Autosampler...
  • Page 35 Copy TO Method with the selected source method. After confirmation with <ENTER> the method will be copied provided that the 1…10 target method is empty. If the target method already contains program steps then the following safety inquiry will appear: 750 Autosampler...
  • Page 36 1 2 3 4 5 6 7 8 9 10 method memory is shown. The characters have the following P - - - - - - - - - meaning: Memory place occupied by programmed method. Memory place free. – 750 Autosampler...

  • Page 37: Method Procedure

    <RUN/STOP> key; the transfer needle remains in <FUNC-7> to Edit its position and the display shown alongside appears. The three following possibilities now exist: Continue method run. <RUN/STOP> Abort method. <ENTER> Edit the current method, then re- <FUNC-7> turn to this selection. 750 Autosampler...

  • Page 38: Priority Sample

    Run time for priority sample RTIME When the priority sample has been completed the Auto- sampler returns to the running method and carries on with the program step which would have followed had the priority sample not interrupted the method run. 750 Autosampler...

  • Page 39: Remote Control

    Entry of parity Select Parity Entry of parity for the RS232 interface. The value entered <None here must also be set on the external controller. After the parity has been confirmed with <ENTER> the following Even,Odd,None display appears: 750 Autosampler...
  • Page 40 <REM/LOC> key is pressed. Remote control via the RS232 interface is carried out with the commands described in the following table. 750 Autosampler...
  • Page 41 21…40 = 2 line; @MSG ## "$$$" 41…60 = 3 line; 61…80 = 4 line) on the LCD display the message "$$$...". Return to normal operation (LOCAL). @LOC # = digit 0 … 9; $ = any character 750 Autosampler...

  • Page 42: Notes - Maintenance - Faults

    All samples should be filtered therefore prior to filling the vials. This can be accom- plished using a hand filtration device with a 0.45 µ µ m membrane filter shown in Fig. 9. Manual sample filtering Fig. 9: 750 Autosampler...

  • Page 43: Operating Parameters

    " between individual injections must be sufficiently Run Time long so that all substances are eluted before the next sample is in- jected. Moreover, it may be necessary to include further time for base- line analysis and evaluation with the evaluation system. 750 Autosampler...

  • Page 44: Maintenance And Servicing

    Maintenance and servicing 4.2.1 General information The 750 Autosampler was designed for years of maintenance-free use. The X,Y,Z sample tray assembly is equipped with bushings and bear- ings made from materials chosen to minimize the need for lubrication. The needle drive carriage position is recalibrated at powerup and with the start of each method.

  • Page 45: Sample Preparation

    For example, this can be achieved by filling several (e.g. 5) sample vials in sequence with distilled water after each sample and programming them as rinsing samples without run time. This procedure also avoids corrosion damage to the injection needle and the crystallization of salts. 750 Autosampler...

  • Page 46: Remedying Malfunctions

    In the second pattern, larger peak heights on the 750 Autosampler...

  • Page 47: Missed Injections

    1 and to set the Needle Depth to " " or " " using POS1 POS2 the system settings key. Should this latter suggestion fail to provide satisfactory results, an alternative sample filtering procedure should be used. 750 Autosampler...

  • Page 48: Error Messages

    733 IC Separation Center and operate the injection valve manually by means of the <FILL> and <INJECT> keys. Please inform Metrohm service if the valve can only be rotated with these keys or not rotated at all.
  • Page 49 "Priority Sample currently running." An attempt was made to begin a priority sample while a priority was already running. 750 Autosampler...

  • Page 50: System Error Messages

    "Vial # already used in this Method." The vial # mentioned has already been programmed in a previ- ous step in the same method. With the 750 Autosampler a sam- ple vial can only be used once for injections. 4.4.2 System error messages "Cannot determine vial position."...

  • Page 51: Remote Control Error Codes

    4.4.3 Remote control error codes If the remote control for the 750 Autosampler is switched on via the RS232 interface then each error will produce a corresponding error code. For each of the errors listed below information is provided as to whether the error can be remedied (R) or if it is a fatal system error (F).

  • Page 52: Appendix

    230/240 V: 1.25 A (rapid-action, with low rupturing capacity, 5 × 20 mm) Interfaces Contact closure strips Outputs for control of external devices, inputs for remote control (see section 5.2.1) RS232 interface Data communication in accordance with RS232C (see section 5.2.2) 750 Autosampler...
  • Page 53 Diagnostic tests Self-diagnostic test Automatic self-diagnosis when instrument switched on User diagnostic test Built-in diagnostic program (see section 4.5) Housing Material Aluminum, enamelled Dimensions Width 324 mm Height 335 mm Depth 548 mm Weight 13.0 kg (incl. accessories) 750 Autosampler...

  • Page 54: Interfaces

    6 (normally closed) according to the time laid down in the method " ". The contact closure time can be set under " Event1 Time SYSTEM " between 1…32000 s. This signal SETTINGS /Contact Closures/Event 1 can be used for controlling external instruments. 750 Autosampler...
  • Page 55 The "Ready" signal provided at connection 18 is internally set to "high". If it is set to "low" by an externally connected instrument then the current Autosampler actions will be interrupted until the signal is reset to "high". 750 Autosampler...

  • Page 56: Rs232 Interface

    1, 2 (selectable, see section 3.8) A 1:1 RS cable with a male 9-pole plug is required as a connection ca- ble (e.g. 6.2134.000 Metrohm cable 9-pol/9-pol). Remote operation of the Autosampler is carried out with the ASCII commands described in chap. 3.8. An example of the use of these commands in a RS232 control program, which is programmed in Mi- crosoft Basic, is given below.

  • Page 57: Standard Equipment

    = 0.3 mm, e.D. = 1.5 mm, length = 1 m 6.2041.600 Sample rack For 128 sample vials 6.2128.100 Connecting cable Connecting cable 750 Autosampler– 733 IC Separation Center 6.2140.010 Connector plug With 19 connections, plugs into contact closure strip 10 6.2140.020 Connector plug With 8 connections, plugs into contact closure strip 9 9 "...

  • Page 58: Optional Accessories

    Set of 1000, with 1000 stoppers (transparent) and 100 stoppers (colored) made of polyethylene 6.2743.010 Polyethylene (PE) stoppers Set of 1000, transparent 6.2743.020 Polyethylene (PE) stoppers Set of 1000, colored ™ 6.2743.030 Filter stoppers (FilterCaps Set of 100, for automatic sample filtering 750 Autosampler...

  • Page 59: Warranty And Conformity

    Lack of an official damage report releases Metrohm from any liability to pay compensation. If any instruments and parts have to be returned, the original packaging should be used if at all possible.

  • Page 60: Eu Declaration Of Conformity

    5.5 Warranty and conformity 5.5.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies, that the in- strument: 750 Autosampler meets the requirements of EC Directives 89/336/EWG and 73/23/EWG. Source of the specifications:...

  • Page 61: Certificate Of Conformity And System Validation

    The features of the system software are documented in the instruc- tion manual. Metrohm Ltd. is holder of the SQS-certificate of the quality system ISO 9001 for quality assurance in design/development, production, installation and servicing. Herisau, November 8, 1996 Dr.

  • Page 62: Index

    Event1 Time 732 IC Detector as "Master" ....11 Contact closure time for "T2" ....24 ..........30 Event2 Time 750 Autosampler as "Master" ....10 Contact closure time for "T3" ....24 ..........30 Event3 Time Contact closure times ....23,51,52 ............19...
  • Page 63 Remote control mode......37 Mains connection Open-end spanner (6.2621.020)..54 Remote-controlled operation....36 Procedure ........15 Opening the 750 Autosampler ....8 Safety notes ........8 Reset ........... 22 Technical data ......... 49 Operating information ......39 Retention time ........40 Mains connection plug 14 Operating parameters ......
  • Page 64 Sampling ..........49 System error messages ...... 47 Seals............ 43 System parameters ......21 ......19 SELECT A FUNCTION Warning..........7 System settings........23 ........36 Select Baud Rate Warranty..........56 ......23 SYSTEM SETTINGS Waste container ........14 Weight ..........50 Width ............50 750 Autosampler...
  • Page 65 5 Appendix 750 Autosampler...

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