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.
Table of contents Table of contents 1 Introduction ............................................................................................1 1.1 Instrument description............................................................................. 1 1.2 Theory of operation .................................................................................. 2 1.3 Control elements ....................................................................................... 4 1.
Inhaltsverzeichnis 4 Notes – Maintenance – Faults ...................................... 39 4.1 Operating information............................................................................ 39 4.1.1 Loading sample vials.................................................................... 39 4.1.2 Sample preparation ...................................................................... 39 4.1.3 Operating parameters................................................................... 40 4.
1.1 Instrument description 1 Introduction 1.1 Instrument description The 750 Autosampler is a microcomputer-operated sampling/controller system designed to be used with the ion chromatographic instruments 732 IC Detector and 733 IC Separation Center. It has a capacity of up to 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.
1 Introduction 1.2 Theory of operation Displacement principle The 750 Autosampler operates using the positive displacement principle of sample transfer. This sample transfer process into the sample loop of the 733 IC Separation Center is illustrated in Fig. 2. When an injection is initiated, the hollow transfer needle 5 descends into the vial. The needle tip punctures the polyethylene cap of the sample vial.
1.2 Theory of operation Number of injections The number of injections per sample with the 750 Autosampler depends 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. Care should always be taken that the injection volume is at least three times greater than the volume of the sample loop.
1 Introduction 1.3 Control elements 750 Autosampler 1 METHOD MANUAL INJECTION 7 8 9 SYSTEM TEMP REM/LOC 4 5 6 F1 F2 F3 1 2 3 PRIORITY 0 . CLEAR ENTER RINSE FUNCTION RUN/STOP 2 3 4 8 7 6 5 Fig. 4: Front of the 750 Autosampler 4 1 Display (LCD) comprising 4 lines each of 20 characters 5 Transfer needle 2 Keypad with function, numeric and cursor keys (details see chap. 3.1.2) 6 Holder for transfer tubing 3 Sample rack (6.2041.
1.3 Control elements 9 10 11 BCD 12 RS-232 INJECT LOAD Switzerland IEEE PRINTER Type: Nr.: U: EXT PWR CONTROL f: V S: Hz VA 13 14 15 Fig. 5: Rear of the 750 Autosampler Contact closure strip for valve control details see chap. 5.2.1 13 Mains switch switch to switch the instrument on and off: I = ON 0= OFF 10 Contact closure strip for external control details see chap. 5.2.1 14 Mains connection plug mains connection see chap. 2.3 11 RS232 interface details see chap. 5.2.
1 Introduction 1.4 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. 1.4.1 Organization These 8.750.
1.4 Information on the Instructions for Use 1.4.2 Notation and pictograms The following notations and pictograms (symbols) are used in these Instructions for Use: Key "Run Time" Parameter or entry value 5 Control element of 750 (see chap. 1.
1 Introduction 1.5 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, degree of protection IP20), the following points should be noted: • Mains connection Setting the mains voltage, checking the mains fuse and the mains connection must be effected in accordance with the instructions in section 2.3.
2.1 Setting up the instrument 2 Installation 2.1 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. Please store all these special packagings as only they can assure damage-free transport of the instrument. 2.1.
2 Installation 2.2 Connection to IC system 2.2.1 750 Autosampler as "Master" When an IC system consisting of 732 IC Detector, 733 IC Separation Center, and 709 IC Pump is operated with the 750 Autosampler as "Master" the command to start the next injection after the analysis time "Run Time" has elapsed will be given by the Autosampler itself. In this case the 750 Autosampler is connected to the 733 IC Separation Center with the 6.2128.100 cable as shown in Fig. 6.
2.2 Connection to IC system 732 6.2125.090 Cable 732/Evaluation System (analog signal) 733 Evaluation system 6.2125.060 Cable 732/Evaluation system (start signal) 750 6.2128.100 6.2115.070 INJECT LOAD 709 6.2134.070 Fig. 6: Connection of 750 Autosampler at 732/733 2.2.
2 Installation • Connect one end of the 6.2115.070 cable (option) to the connections "EXTERNAL INJECT INPUT" and "GND" on the connector plug inserted in the contact closure strip 10. 10 • Connect the other end of the 6.2115.070 cable to the connections "Pos. Fill" on the terminal block 38 (valve A) or 46 (valve B) of the 733 IC Separation Center so that COM and GND are connected.
2.2 Connection to IC system The four cable ends are appropriately inscribed with "LOAD NO" (green), "LOAD COM" (yellow), "INJECT NO" (brown) and "INJECT COM" (white). • Connect the other end of the 6.2128.100 cable to the connections "Ground", "Fill" and "Inject" on the terminal block 38 (valve A) or 46 (valve B) of the 733 IC Separation Center. The three cable ends are appropriately inscribed with "GND" (white), "FILL" (green) and "INJECT" (brown). 732 6.2128.130 733 6.2125.090 (732) 6.2115.070 750 6.
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: 1 Tubing connection 750 – injection valve • At the 733 IC Separation Center, loosen the rotary nipple screwed onto the interior side of connection 22 or 28. 28 • Take PTFE suction tubing 88 (see Fig. 16 and Fig.
2.3 Mains connection 2.3 Mains connection Follow the instructions below for connecting to the power supply. If the instrument is operated with the mains voltage set wrongly and/or wrong mains fuse there is a danger of fire! 2.3.1 Check fuses The selection of mains voltage (100, 120, 220 or 240 V) and mains frequency (50 or 60 Hz) is made automatically by the 750 Autosampler according to the mains voltage and frequency used.
2 Installation 2.3.2 Mains cable and mains connection Mains cable The instrument is supplied with one of three mains cables • 6.2122.020 with plug SEV 12 (Switzerland, …) • 6.2122.040 with plug CEE(7), VII (Germany, …) • 6.2133.070 with plug NEMA 5-15 (USA, …) which are three-cored and fitted with a plug with an earthing pin. If a different plug has to be fitted, the yellow/green lead (IEC standard) must be connected to protective earth (protection class 1).
2.4 Initial checkout 2.4 Initial checkout Initial checkout will prove the general operation of the instrument and show that no shipping damage or installation problem exists which would prevent normal operation. To carry out this checkout the 750 Autosampler must be connected to the 733 IC Separation Center as described in chap. 2.2 and correctly connected to the mains supply as described in chap. 2.3.
2 Installation 5 Start injection Press the key. The 750 Autosampler will make an injection from the vial at position 1. Afterwards the following display will appear: MANUAL INJECTION COMPLETED 6 Select "SYSTEM" Press the key ( + <4>). The following screen will appear: SYSTEM SETTINGS Park Needle Contact Closures Loop Size à 7 â Park needle Press the key.
3.1 Fundamentals of operation 3 Operation 3.1 Fundamentals of operation 3.1.1 Display and instrument dialog The LCD display 1 on the 750 Autosampler consists of 4 lines each with 20 characters. After the Autosampler has been switched on and initialized the following display appears: READY SELECT A FUNCTION This screen is called the main screen. It is always displayed any time the instrument is idle. Note that the line "SELECT A FUNCTION" flashes.
3 Operation ERROR Value out of range Enter value between # - ## where # and ## are the appropriate range limits. The error message will remain on the display until the key is pressed. Parameter lines which contain the characters "<" and/or ">" (e.g. "NONE>") on either side of the parameter value indicate that a selection must be made from a discreet menu of items. Pressing either the <à> or <ß> key allows scrolling through the selection list.
3.1 Fundamentals of operation Keys of 750 Autosampler Key Normal function Function with Function key • Selection of a function in combination with the corresponding numeric key. – Run/Stop key • If no method runs: Selection and start of a method. • If a method runs: Stop of the running method. – Key for priority sample • Interruption of a running method and injection of a priority sample. – PRIORITY – ENTER Enter key • Confirmation of entered parameter.
3 Operation Key F1 Function with Numeric entry 1 • Numeric entry of number "1". No function • The function is not available. Numeric entry 2 • Numeric entry of number "2". No function • The function is not available. Numeric entry 3 • Numeric entry of number "3". No function • The function is not available. 0 Numeric entry 0 • Numeric entry of number "0". Shipping position • Transfer needle is moved to the shipping position. . Point • Entry of decimal point ".".
3.2 System settings 3.2 System settings SYSTEM 4 By pressing the key ( + <4>) the system settings menu appears. The system settings are global parameters which affect the operation of the Autosampler, but are not required to be programmed for each sample or method.
3 Operation CLOSURE DURATIONS Injection 1 à 1…32000 s CLOSURE DURATIONS Event # 1 à 1…32000 s Contact closure time for "START" Input of contact closure time for the signal to be produced at output "START" when the injection valve is switched to the "INJECT" position. Contact closure time for "T1", "T2" or "T3" Entry of contact closure time for the signal to be produced at output "T#". The signal output is made according to the time laid down in the method "Event# Time".
3.2 System settings NEEDLE SETUP Pressure Low> à Low,High Pressure for needle lowering The needle can be lowered either with "Low" pressure or with "High" pressure. If sample vessels closed with 6.2743.030 filter stoppers are used then pressure "High" must be selected.
3 Operation 3.3 Manual rinsing RINSE This command allows the rinsing of the transfer needle, transfer tubing and injection valve. When the key ( + <9>) is pressed, the following screen appears: 9 Enter Rinse Vial # 1 1…128 3.4 Position of rinsing solution Entry of position of the rinsing solution on the sample rack. After confirmation with the transfer needle moves to the given rinsing vial and sinks down to its lowest position "POS4".
3.4 Manual injection Needle depth Entry of the position to which the transfer needle is lowered at the injection of the sample. The positions correspond to the following displacement volumes (see also section 1.2): MANUAL INJECTION àNeedle Depth POS4 POS1 POS2 310 µL 450 µL POS3 POS4 590 µL 730 µL If sample vessels closed with 6.2743.030 filter stoppers are used then immersion depth "POS4" must not be selected..
3 Operation 3.5 Methods METHOD 7 By pressing the key ( + <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.
3.5 Methods Edit program step Allows an already existing program step to be called up and edited. The following display will appear after entering : EDIT METHOD # N Edit Step à Enter Step Number #M 1…128 METHOD N STEP Start Vial à M 1 1…128 METHOD N STEP Final Vial à M 1 1…128 Select program step Entry of the number M of the program step which is to be edited.
3 Operation METHOD N Run Time à STEP M 3.0 0.0,0.1…999.9 min METHOD N STEP M Event1 Time 0.0 à 0.0…999.9 min METHOD N STEP M Event2 Time 0.0 à 0.0…999.9 min METHOD N STEP M Event3 Time 0.0 à 0.0…999.9 min METHOD N STEP M Rinse Type NONE> à NONE,EVEN,ODD, QR_E,QR_O 30 Run time Selects the run time (chromatographic analysis time) between switching the injection valve to the "INJECT" position and the start of a new injection with the same or the next sample. The minimum run time is 0.1 min.
3.5 Methods EVEN ODD QR_E QR_O METHOD N Next Step STEP M à Next program step Changes to next program step in the method. If no further program step exists the following display appears: At end of method. Add another step? for Yes for No , METHOD N STEP Previous Step M à Add new program step Decision as to whether a new program step is to be added: Add a new program step. Return to program step menu.
3 Operation Delete program step Allows program steps to be deleted. After is pressed the following display appears: EDIT METHOD # N Delete Step à DELETE A STEP Enter Step Number #N Delete Step # N? to Delete to Abort Select program step Entry of the number of the program step which is to be deleted. After is pressed the following display appears: Confirmation of deletion process Delete selected program step N. Abort deletion process.
3.5 Methods Method # contains a program to Overwrite to Abort , Overwrite confirmation The selected target method already contains a program. Overwrite confirmation. Return to method menu. Delete a method Allows a method to be deleted. After is pressed the following display appears: METHOD MENU Delete Method à Select method Entry of the method number N which is to be deleted.
3 Operation 3.6 Method procedure RUN/STOP A previously programmed method can be started by pressing the key or (as already described in chap. 3.5) by selection of the menu item "Run Method" in the method menu. In both cases the following display appears: Enter Method Number # N 1…10 METHOD STEP METHTIME NN MM XXX.X VIAL INJ RTIME nnn m xxx.x Select method Entry of the method number N which is to be started. After confirmation with the selected method is started.
3.7 Priority sample 3.7 Priority sample PRIORITY By pressing the key a running method can be interrupted so that a single priority sample can be processed. The priority sample can be assigned its own parameters independently from those of the current method. The priority sample has priority before the next sample, i.e. it will be processed as soon as all injections from the current sample vial have been completed.
3 Operation 3.8 Remote control REM/LOC 6 By pressing the key (key + <6>) the menu for switching between normal operation (Local) and remotecontrolled operation via the RS232 interface (Remote) appears. The key opens the following menu: REMOTE/LOCAL Local RS-232 IEEE-488 Exit Remote control/Normal operation Normal operation Remote control via RS232 Remote control via IEEE-488 Return to standby mode The individual menu points are selected by pressing the <á> and <â> keys.
3.8 Remote control Select Data Bits 8 5,6,7,8 Select Stop Bits 1 1,2 REMOTE MODE RS-232 750 Autosampler Entry of data bits Entry of data bits for the RS232 interface. The value entered here must also be set on the external controller. After the data bits have been confirmed with the following display appears: Entry of stop bits Entry of stop bits in bits/s for the RS232 interface. The value entered here must also be set on the external controller.
3 Operation Summary of the remote control commands Command Description @GTV ### Go to vial position ### : 0 Rest position at left front 1 … 128 Vial position on sample tray @LDL # Fill sample loop: The transfer needle is lowered to position # (1 … 4). @VLV LD/INJ Switch injection valve: LD LOAD (switch injection valve to FILL position) INJ INJECT (switch injection valve to INJECT position) @RNP Read needle position: The position (1 … 4) is put out.
4.1 Operating information 4 Notes – Maintenance – Faults 4.1 Operating information 4.1.1 Loading sample vials Load the vial with sample to within ≈ 6 mm (1/4 in.) of the top and push the polyethylene cap (cup side down) into the vial. The cap has two sealing rings on its periphery. The cap should be pushed into the vial so that both rings engage and remain so. The maximum volume of sample is 800 µL, the minimum volume of sample is 300 µL using a loop size > 20 µL and 150 µL using a loop size ≤ 20 µL.
4 Notes – Maintenance – Faults A further possible way of filtering samples is by means of the optional 6.2743.030 filter stoppers. These filter stoppers, which contain a built-in filter unit, are fitted to the sample vials just like normal stoppers. The way they work is shown in Fig. 10. To injection valve Filtered sample Unfiltered sample Fig. 10: Sample filtering with FilterCaps FilterCaps were designed to free the chromatographer from the timeconsuming task of hand filtering samples.
4.2 Maintenance and servicing 4.2 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 bearings 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.
4 Notes – Maintenance – Faults PEEK compression fitting 18 16 Ferrule Nut 19 Holder 20 17 Needle holder Connection screw 21 Clamping ring 22 5 Transfer needle Holder 23 Centering sleeve 24 Fig. 11: Transfer needle replacement 4.2.3 Sample preparation Experience has shown that most problems are caused by solids in the sample solutions. Such particles can block the needle, transfer tubing and the sample loop and also permanently damage the surfaces of the injection valve seals.
4.3 Remedying malfunctions 4.3 Remedying malfunctions 4.3.1 Non-reproducible injections Non-reproducible injections are usually due to problems such as fitting leaks, plugged tubing, poorly swaged fittings, or submerged waste tubes. In some instances, non-reproducibility may appear to be injector related when, in fact, it is caused by other components in the chromatographic system.
4 Notes – Maintenance – Faults first injection followed by smaller but equal peak heights for the second two injections are observed. Observation of either pattern requires complete replacement of the loop. The correct way to mount seals is described in detail in chap. 2.5 of the 732/733 Instructions for Use. When using a previously swaged steel capillary, be sure to use it with the fitting in which its ferrules were originally set.
4.4 Error messages Malfunctioning injection valve If samples are only injected sometimes or not injected at all the injection valve of the 733 IC Separation Center must be checked. This is done by carrying out several injections with the 750 Autosampler while keeping the valve under observation. If the valve rotates perfectly but still no sample is injected then either a leak or a blockage is present (further procedure see chap. 4.3.1).
4 Notes – Maintenance – Faults "Cannot execute! Autosampler is currently running." An attempt was made to begin an operation while the Autosampler is currently running an operation. For example, if a manual injection is running and an attempt was made to run a method. "Final vial # must be greater than or equal to start vial." An attempt was made to program the final vial in a program step to a value less than the start vial. The final vial must always be ≥ the start vial.
4.4 Error messages "Source Undefined" An error occurred but the origination is unclear or unknown. This error should not occur. If it does, then a problem probably exists with the ROM or RAM. Inform the Metrohm service. "Unable to execute command while Method is running." An attempt was made to select an operation that is not allowed to execute while a method is in operation, e.g. a manual injection or a manual rinse. "Value out of range.
4 Notes – Maintenance – Faults 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). The Autosampler remains ready for operation with R-errors and the operator can enter a new command. With F-errors it is no longer possible to use the Autosampler.
5.1 Technical data 5 Appendix 5.1 Technical data Sampling Method Positive displacement principle Capacity 128 sample vials of 730 µL each Number of injections per vial max. 4 with sample loops ≤ 10 µL max. 3 with sample loops >10 µL Max. loop size 50 µL with 3 injections per sample 100 µL with 2 injections per sample 300 µL with 1 injection per sample Carryover < 0.25 % without rinsing < 0.
5 Appendix Safety specifications Construction / testing According to IEC 1010 / EN 61010 / UL 3101-1, protection class 1, degree of protection IP20 Safety notes The Instructions for Use include information and warnings which must be heeded by the user to assure safe operation of the instrument.
5.2 Interfaces 5.2 Interfaces 5.2.1 Contact closure strips The contact closure strip 9 can be used for external control of an injection valve. The allocation of the 4 connections is shown in Fig. 12. The output signals are emitted as contact closures between two connections. REMOTE INJ. VALVE 8 7 6 5 4 3 2 1 INJECT LOAD LOAD (output signal for switching the Fig.
5 Appendix T2 (output signal for freely programmable event) Contact closure between connections 7 and 8 (normally open) and 7 and 9 (normally closed) according to the time laid down in the method "Event2 Time". The contact closure time can be set under "SYSTEM SETTINGS /Contact Closures/Event 2" between 1…32000 s. This signal can be used for controlling external instruments.
5.2 Interfaces 5.2.2 RS232 interface The RS232 interface 11 is used for complete control of the 750 Autosampler by an external computer. The interface is wired as DCE device (DCE: Data Communication Equipment) and has the following technical data: Baud rate: Data bits: Parity: Stop bit: 300…38400 (selectable, see section 3.8) 5…8 (selectable, see section 3.8) even, odd, none (selectable, see section 3.8) 1, 2 (selectable, see section 3.
5 Appendix 5.3 Standard equipment Subject to changes ! The 2.750.0010 Autosampler includes the following parts: Quant. Order No. Description 1 6.1803.000 PTFE Microcapillary tubing Transfer tubing for connection of transfer needle with injection valve; i.D. = 0.3 mm, e.D. = 1.5 mm, length = 1 m 1 6.2041.600 Sample rack For 128 sample vials 1 6.2128.100 Connecting cable Connecting cable 750 Autosampler– 733 IC Separation Center 1 6.2140.
5.4 Optional accessories 5.4 750 Autosampler Optional accessories Order No. Description 6.2134.000 RS Connecting cable length = 2 m; plug = 9-pol male / 9-pol female 6.2115.070 Connecting cable 750 – 733 length = 1.4 m 6.2134.070 Connecting cable 750 – 709 length = 2 m 6.2620.130 Transfer needle Replacement needle, assembly see chap. 4.2.2 6.2413.000 Borosilicate glass sample vials Set of 1000, with 1000 stoppers (transparent) and 100 stoppers (colored) made of polyethylene 6.2743.
5 Appendix 5.5 Warranty and conformity 5.5.1 Warranty The warranty on our products is limited to defects that are traceable to material, construction or manufacturing error which occur within 12 months from the day of delivery. In such cases the defects will be rectified in our workshops free of charge. Transport costs are to be paid by the customer. For day and night operation the warranty is limited to 6 months. Glass breakage in the case of electrodes or other parts is not covered by the warranty.
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 instrument: 750 Autosampler meets the requirements of EC Directives 89/336/EWG and 73/23/EWG.
5 Appendix 5.5.3 Certificate of conformity and system validation Certificate of Conformity and System Validation This is to certify the conformity to the standard specifications for electrical appliances and accessories, as well as to the standard specifications for security and to system validation issued by the manufacturing company. Name of commodity: 750 Autosampler Name of manufacturer: Metrohm Ltd.
5.6 Index 5.6 Index 7 732 IC Detector as "Master" ................ 11 750 Autosampler as "Master" .............. 10 A Accessories ......................................... 54 Acoustic signal .................................... 25 Ambient temperature........................... 50 Analysis time ....................................... 30 Append program step ......................... 31 Append Step ......................................... 31 Appendix .............................................
5 Appendix Insert program step ............................. 31 Insert Step ............................................ 31 Installation ............................................. 9 Installation problems ........................... 17 Instructions for Use (8.750.1023) ..... 6,54 Instrument description........................... 1 Instrument dialog................................. 19 Interfaces ........................................ 49,51 Introduction............................................
5.6 Index RS232 interface 11 Connection to 762 ........................... 12 Description ...................................... 53 Figure ................................................ 5 Remote control ................................ 36 Run Injection ........................................ 27 Run Method .......................................... 32 Run Time .............................................. 30 .................................... 34 Run/Stop key .................................
5 Appendix 62 750 Autosampler
