CH-9101 Herisau/Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 E-Mail info@metrohm.ch http://www.metrohm.com 813 Compact Autosampler Program version 5.813.0010 Instructions for use 8.813.1003 06.
D. Möckli Teachware Metrohm Ltd. Oberdorfstr. 68 CH-9100 Herisau 1st Edition 2001 Copyright © 2001 by Metrohm Ltd. All rights reserved. This manual was carefully produced. Nevertheless the author does not warrant the information contained herein to be free of errors. The author appreciates your comments and feedback. © Metrohm Ltd.
Table of content 1 Introduction ......................................................1 1.1 Instrument description .................................................................................1 1.2 Parts and controls .........................................................................................2 1.3 Rear view........................................................................................................4 1.4 The keyboard ...............................................................
3 Operation ........................................................20 3.1 Keyboard functions .................................................................................... 20 3.2 Configuration .............................................................................................. 21 3.2.1 Course of configuration ...........................................................................23 3.3 RAM initialization...................................................................................
Table of Figures Fig. 1 Fig. 2 Fig. 3 Fig. 4 Fig. 5 Fig. 7 Fig. 8 Fig. 9 Fig. 10 Fig. 11 Fig. 12 Fig. 13 Fig. 14 Fig. 15 Fig. 16 Fig. 17 Side view ........................................................................................................ 2 Rear view........................................................................................................ 4 Keyboard ........................................................................................................
1 Introduction 1 Introduction 1.1 Instrument description The 813 Compact Autosampler can be used for automating different tasks, e.g. ion chromatographic determinations with the Metrohm IC system instruments or voltammetric determinations with the Metrohm 746 Trace Analyzer or 757 VA Computrace . The sample rack provided may hold up to 36 vials of 2.5 or 11 mL volume respectively. Sample tubes made of polypropylene are standard.
1.2 Parts and controls 1.2 Parts and controls 5 6 7 4 3 8 2 1 9 10 11 26 12 13 14 15 16 17 18 2 20 -240 V U NIQUE MENT AVE C FU SE S/EMP LOYE R U SE ONL Y WIT H 25 0V 1 00 -120 V D ES F USIB LES DE 250V Metrohm 25 24 23 19 22 21 20 Fig. 1 Side view Safety note: Never operate the instrument without splash protection and plug cover being mounted. The plug cover prevents any contamination of the connectors, caused by spilled solvents or chemicals.
1 Introduction 1 Splash protection 6.2751.040 14 Must be installed always in operation! 2 Needle PEEK needle 6.1835.020 or PEEK tube 6.1835.010 or 6.1835.030 15 Snap-action lever For releasing the tubing cartridge 3 Lift 16 Screw thread for splash protection 4 Steel holder 4.766.4330 attached (part of 6.2833.000 Needle holder) 17 PEEK capillary 6.1831.060 or 6.1822.410 (1 m or 1.2 m) For conveying the sample to e.g. an injection valve 5 PEEK compression fitting 4.766.
1.3 Rear view 1.3 Rear view 9 9 11 18 16 16 25 27 24 Type 1.813. 28 Keyboard Made by Metrohm Herisau Switzerland 20 Fig. 2 Rear view 9 4 Mounting screws for splash protection 24 Sample rack 6.2041.750 11 Tubing cartridge 6.2755.000 For 6.1826.0X0 pump tubing 25 PP sample tubes 6.2743.050 (can be sealed with 6.2743.060 PE caps) 16 Mounting screws for splash protection 27 Serial number 18 Tower 28 Keyboard connection 20 Plug cover 6.2752.
1 Introduction 1.4 The keyboard 813 Compact Autosampler HOLD • The key starts a sample series or continues an interrupted series. • The key terminates a sample series or resets (if pressed twice) the 813 Compact Autosampler (RESET). • The key interrupts the course of a sample series and establishes the 'HOLD' state. The green LED blinks. With the key the interrupted sample series can be continued. • The green LED indicates the status of the Autosampler.
2.1 Setting up the instrument 2 Installation 2.1 Setting up the instrument 2.1.1 Packaging The 813 Compact 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 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! 2.2.1 Setting the mains voltage Before switching on the 813 Compact Autosampler for the first time, check that the mains voltage set on the instrument (see Fig. 4) matches the local mains voltage.
2.2 Mains connection 220 – 240 V 100 – 120 V 22 0 - 24 0 V 10 0 - 12 0 V 22 0 - 24 0 V 23 10 0 - 12 0 V 21 Fuse holder 22 Mains connection plug 23 Mains switch 22 21 Fig. 4 Setting the mains voltage 2.2.2 Fuses One of the two fuses 0.5 A/slow-blow for 100…120 V or 0.
2 Installation 2.2.4 Switching the instrument on/off The 813 Compact Autosampler is switched on and off using the mains switch 23. 2.3 Attaching the accessories For attaching the accessories at the 813 Compact Autosampler, proceed in the order described below. 2.3.1 Connecting the keyboard 1 2 Connecting the keyboard Connect the 6.2142.110 keyboard to the keyboard connection 28 "Keyboard". For disconnection, press the plug together slightly on both sides. Type 1.76 0.001 0 Nr.
2.3 Attaching the accessories 2.3.3 Installing the needle 1 Remove PEEK compression fitting 5 Remove PEEK compression fitting 5 screwed onto the needle holder 4. 2 Insert needle • Needle 2 (6.1835.010 PEEK needle or 6.1835.020 or 6.1835.010 PEEK tube) is inserted a short distance into the opening of steel holder 4. • Push PEEK round seal 29 over needle 2 from above. The smaller end of the seal must face upwards.
2 Installation 2.3.4 Installing the splash protection To avoid any danger of injury by the needle, the 6.2751.070 splash protection must always be installed when operating the 813 Compact Autosampler! 1 Remove holding screws Remove the holding screws 16 and the washer mounted on the screw threads 9 at tower 18 using the 6.2621.100 Allen key. 2 Remove protective film from splash protection Remove the plastic film glued on both sides of the splash protection 1.
2.3 Attaching the accessories 2.3.5 Placing the sample rack 1 Place sample rack Place sample rack 24 on the turntable of the 813 Compact Autosampler acc. to Fig. 8. 2 Initialize rack Press to move the rack to the home position, in which the magnetic code can be read (coding magnet 30). 30 Fig. 8 Sample rack placing 2.3.6 Adjusting the sample rack If a new sample rack is placed on the 813 Compact Autosampler for the first time, it must be adjusted.
2 Installation 3 Check needle position • Press until the needle 2 is about 1 cm above the upper level of the sample rack 24. • Check needle position: If the needle 2 cannot be lowered unhindered through the upper hole of the rack position 1, continue directly with point 4. • Press once and continue lowering the needle by pressing again until the needle 2 stops.
2.3 Attaching the accessories 2.3.7 Tubing connections Pump tubings are consumable material with a lifetime which depends on the contact pressure (see section 4.4 Maintenance and servicing). This is why the tubing cartridges should be raised completely by loosening snap-action lever 15 on the right-hand side if the pump is to remain switched off for a considerable length of time (the set contact pressure remains unchanged). The 6.1826.
2 Installation 7 6 31 8 32 11 13 15 32 31 6 17 Fig. 9 Installing the pump tubing 6 PEEK compression fitting 6.2744.010 15 Snap-action lever 7 PEEK capillary 6.1831.050 17 PEEK capillary 6.1831.060 or 6.1822.410 8 Pump tubing 6.1826.040 31 Coupling 6.2744.030 11 Tubing cartridge 6.2755.000 32 Stopper (black) 13 Contact pressure lever 2.3.8 Tubing connection to Metrohm 761 / 790 IC–Systems 3 Connection pump tubing – injection valve • Use a 6.2744.
2.3 Attaching the accessories 2.3.9 Tubing connection to a Metrohm 747 VA Stand 3 Connection Pumpschlauch – VA Stand 747 • Use a 6.2744.010 PEEK compression fitting and a 6.2744.030 coupling to tighten the 6.1831.060 PEEK capillary 17 to the pump tubing 8. To keep the dead volume as small as possible shorten the pump tubing to a suitable length.
2 Installation 2.4 Instrument connections 2.4.1 Remote interface External devices can be connected to the 25 pin remote connection (see Fig. 1). The remote line Input 2 (pin 22, see section 4.3 Technical description) allows the 813 Compact Autosampler to get synchronized with an other instrument. Connecting instruments to the 813 Compact Autosampler requires Metrohm cables. Otherwise a safe signal transmission may not be guaranteed.
2.4 Instrument connections Example for the interconnection of a modular Metrohm IC System: 732 6.2125.090 cable 733 6.2125.090 cable 6.2125.060 cable 752 753 709 813 6.2143.210 cable 6.2141.110 cable 6.2125.120 adapter 6.2143.200 cable Fig. 13 Interconnection with a modular Metrohm IC System 2.4.3 Interconnection with a Metrohm 746 VA Trace Analyzer The 813 Compact Autosampler is connected to a Metrohm 746 VA Trace Analyzer with 747 VA Stand using the 25 pin 6.2141.020 Remote cable.
2 Installation 2.4.4 Interconnection with a Metrohm 757 VA Computrace You need a 6.2141.150 Remote cable to interconnect a 813 Compact Autosampler with a Metrohm VA Computrace 757, see below. 6.2141.080 cable 731 757 772 772 765 813 6.2141.150 cable Fig. 15 Interconnection with 757 VA Computrace 2.4.5 Interconnection with other instruments The Metrohm 813 Compact Autosampler can be connected to other Metrohm instruments or instruments of other equipment manufacturers.
3.1 Keyboard functions 3 Operation 3.1 Keyboard functions The 813 Compact Autosampler provides three keys and two LEDs, which may offer different functions depending on the current instrument status. After switching on the instrument the readyness of the 813 Compact Autosampler is displayed by lighting up of the green LED. Function of the keys START RESET Starts processing of a sample series. STOP Stops processing of a sample series or initializes the 813 Compact Autosampler (by pressing twice).
3 Operation 3.2 Configuration To select a method or to define the work position switch on the 813 Compact Autosampler while holding down the key. The green LED blinks once a second while you can enter the desired settings. Keyboard functions for configuration: (after Power on while depressed, green LED blinks) START HOLD RESET STOP Accepts the setting of a value and moves on to the next value. Selection of method or manual lift movement for the definition of the work position.
3.2 Configuration For setting the work position place a filled sample tube on the sample rack of the Autosampler on rack position 1. The needle should remain dipped in the sample solution during the aspiration interval or reach the bottom of the sample vial, depending on the application. Press to accept a setting. To cancel a setting press . Press twice to abort the configuration procedure.
3 Operation 3.2.1 Course of configuration Power on + Init Select method 1...4 Set work position (move lift) Init Ready Ready Fig. 16 Configuration If you just want to select a method: 1. Switch off Autosampler. 2. Press and simultaneously switch on Autosampler. The green LED blinks. 3. Press again, to select method 1. The red LED blinks slowly.
3.3 RAM initialization 4. Accept the selected method with . 5. To return to the basic state, press the key. If you just want to define the work position: 1. Switch off Autosampler . 2. Press and simultaneously switch on Autosampler. The green LED blinks. 3. Press . The green LED blinks twice. 4. Press to run the lift downward. The red LED slowly. Press again and again to set the work position exactly.
3 Operation 3.4 The methods All methods of the 813 Compact Autosampler make use of the built-in peristaltic pump to aspirate the sample and to fill the sample loop of the Ion chromatograph connected. The pump duration is controlled by the time program of the Ion chromatograph's PC software by sending Remote signals to the Autosampler. The number of samples to be processed is to be set in the sample queue of the control software. The Autosampler should be stopped manually after processing the last sample.
3.4 The methods Method 3 (detailed command sequence, see 4.2 Sequences) Double determination of each sample, no air gap, needle remains in sample after sample transfer. Sequence: 1. Await first Remote signal of the instrument. 2. Get sample tube and immerse needle. 3. On receiving second Remote signal, switch on the peristaltic pump. Sample is transferred. 4. Await third Remote signal. The instrument starts its determination. 5. Peristaltic pump is switched off after 12 s. 6.
3 Operation 3.5 The Metrohm IC control software To use the 813 Compact Autosampler with a 761 Compact IC or a 790 Personal IC one has to create a time program. First of all the IC has to send a Remote signal (Remote line 3) to synchronize the command sequence (first Remote signal) of the 813 Compact Autosampler. After that the injection valve is switched to 'Fill' position. Then a second Remote signal starts the filling of the sample loop.
3.6 Modular Metrohm IC System 732/733 3.6 Modular Metrohm IC System 732/733 The 813 Compact Autosampler can be controlled directly by a Metrohm 732 IC Detector or by a PC control software, such as the Metrohm IC Net 2.0 using the remote control lines of the 732 IC Detector. See the 732 IC Detector user manual for details or read the IC Net 2.0 documentation. 3.
3 Operation Sample method for the 746 VA Trace Analyzer: 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 Instructions t/s ------------- ----STIR PURGE SMPL/M SETCTRL 1.0 SETCTRL REM 30.0 SETCTRL 1.0 SETCTRL REM 300.0 SETCTRL 1.0 SETCTRL REM DOS>M PURGE 90.0 (ADD STIR PURGE 30.0 (REP SEGMENT REP)1 ADD>M ADD)2 RINSE SETCTRL 1.0 SETCTRL REM 20.0 SETCTRL 1.0 SETCTRL REM 300.0 SETCTRL 1.0 SETCTRL REM RINSE RINSE END Main parameters ------------------------Rot.
4.1 Error Messages 4 Appendix 4.1 Error Messages An error occurring during a sample series is displayed by a blinking red LED. The number of flashes indicates the error number. If an error occurs during processing of a sample series, the changer will then be switched into the 'HOLD' state. The current method has to be halted by pressing . The list of possible error messages and their causes: 30 1* RAM defect Call Metrohm-Service.
4 Appendix 4.2 Sequences The available Autosampler methods are described briefly in section 3.4 The following listings explain the sequences in detail. Method 1 Single determination with air gap after each run, needle lifted after sample transfer. 813 Compact Autosampler 813.
4.2 Sequences Method 2 Single determination, no air gap, needle remains in sample after sample transfer. 813 Compact Autosampler 813.0010 ¬ Program version parameters method 813_2 number of samples: ¬ Method name * ¬ Number of samples unlimited 1 ¬ First rack position >start sequence 1 SAMPLE: = >sample sequence 1 SCN:Rm: 2 MOVE *****1** 1 3 LIFT: 1 : : work mm 4 SCN:Rm: 5 PUMP 1.1 *****1** : 6 WAIT on 5 s 7 SCN:Rm : 8 WAIT 9 PUMP sample *****1** 12 s 1.
4 Appendix Method 3 Double determination of each sample, no air gap, needle remains in sample after sample transfer. 813 Compact Autosampler 813.0010 ¬ Program version parameters method 813_3 number of samples: ¬ Method name * ¬ Number of samples unlimited 1 ¬ First rack position >start sequence 1 SAMPLE: = >sample sequence 1 SCN:Rm: 2 MOVE *****1** 1 3 LIFT: 1 : : work mm 4 SCN:Rm: 5 PUMP 1.1 *****1** : 6 WAIT : 8 WAIT 1.1 : off *****1** 11 WAIT 5 s 12 SCN:Rm: 1.
4.2 Sequences Method 4 Triple determination of each sample, no air gap, needle remains in sample after sample transfer. 813 Compact Autosampler 813.0010 ¬ Program version parameters method 813_4 number of samples: ¬ Method name * ¬ Number of samples unlimited 1 ¬ First rack position >start sequence 1 SAMPLE: = >sample sequence 1 SCN:Rm: 2 MOVE *****1** 1 3 LIFT: 1 : : work mm 4 SCN:Rm: 5 PUMP 1.1 *****1** : 6 WAIT : 8 WAIT 1.1 : 5 s 12 SCN:Rm: 1.
4 Appendix 4.3 Technical specifications Dimensions Weight Material Lift path Lift Turntable Pump Height: 0.50 m, Width: 0.28 m, Depth: 0.49 m 12.3 kg (incl. sample rack) Housing: Metal case, multiple enameling Splash protection: Polymethylmethacrylate (PMMA) Sample rack: Polypropylene (PP) ca. 125 mm Load: Stroke speed: Rotational speed: Pump type ca. 30 N 12 mm/s 20 angular degrees/s 1-channel peristaltic pump with rotational speed of 20 /min (with water, without counterpressure) with 6.1826.
4.3 Technical specifications Temperatures Nominal operating range 5...40 °C at 20...80 % atmospheric humidity Storage, transport –20...+60 °C 60 °C at atmospheric humidity 50 °C " " 40 °C " " <50% <85% <95% Mains connection Voltage 100...120 V, 220...240 V Frequency 50...60 Hz Power consumption 40 VA Fuse 0.5 AT (110 V), 0.
4 Appendix 4.4 Maintenance and servicing 4.4.1 Maintenance by Metrohm service is best done as part of an annual service performed by specialists from the Metrohm company. If work is frequently performed with caustic and corrosive chemicals, it may be necessary to shorten the interval between servicing. The Metrohm service department is always willing to offer expert advice on the maintenance and servicing of all Metrohm instruments 4.4.
4.4 Maintenance and servicing To replace a pump tubing proceed as follows: 1 Remove old pump tubing • Press contact pressure lever 11 on the tubing cartridge down as far as it will go. • Release tubing cartridge 11 from holding clamp 14 by pressing down snap-action lever 15 and remove from mounting pin 10 at the 813 Compact Autosampler (see Fig. 1). • Remove old pump tubing. 2 Insert new pump tubing • Insert the new pump tubing 8 (6.1826.040) in the tubing cartridge as shown in Fig. 9.
4 Appendix 4.5 Warranty and conformity 4.5.1 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 this case, 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.
4.5 Warranty and conformity 4.5.2 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: System software: Name of manufacturer: Technical information: 813 Compact Autosampler stored in ROMs Metrohm Ltd.
4 Appendix Ionenanalytik • Analyse des ions • Ion analysis • Análisis iónico 813 Compact Autosampler EU Declaration of conformity The METROHM AG company, Herisau, Switzerland hereby certifies that the in-strument: 813 Compact Autosampler meets the requirements of EC Directives 89/336/EWG and 73/23/EWG.
4.6 Standard equipment 4.6 Standard equipment Subject to changes! All dimensions are given in mm. The following parts are included: 2.813.0010 Compact Autosampler (for IC applications) Quant. Order No. 2 6.1826.040 1 2 6.1831.050 6.1831.060 Description Pump tubing made of PVC (Tygon); with 2 firmly attached black-black stoppers; i.d. = 0.76 mm, e.d. = 2.27 mm 150 400 PEEK Capillary Length = 40 cm 0.5 1.59 PEEK Capillary Length = 100 cm 0.5 1.59 1 6.2041.
4 Appendix Quant. Order No. 1 6.2621.100 Description Allen key 3 mm For Allen screws on sample rack and for splash protection 1 6.1835.010 PEEK needle For aspiration of solutions from sealed sample tubes 1 6.2743.057 PP Sample tubes (11 mL) For 6.2041.750 sample rack set of 200 1 6.2743.077 PE Caps For sealing the 6.2743.057 sample tubes set of 200 1 6.2744.010 PEEK Compression fitting For the connection of 6.1831.0X0 PEEK capillaries or 6.1803.
4.6 Standard equipment 2.813.0020 Compact Autosampler (for VA applications) Quant. Order No. 2 6.1826.020 1 1 6.1831.050 6.1822.410 Description 150 Pump tubing made of PVC (Tygon); with 2 firmly attached black-black stoppers; i.d. = 0.76 mm, e.d. = 2.27 mm 400 PEEK Capillary Length = 40 cm 0.5 1.59 PEEK Capillary 1x M6 Length = 120 cm 0.5 1.59 1 6.2041.750 Sample rack for 36 sample tubes 6.2743.050 (11 mL) or 6.2743.040 (2,5 mL) 1 6.2122.
4 Appendix Quant. Order No. Description 1 6.2743.057 PP Sample tubes (11 mL) For 6.2041.750 sample rack set of 200 1 6.2744.010 PEEK Compression fitting For the connection of 6.1831.0X0 PEEK capillaries or 6.1803.0X0 PTFE capillaries; set of 5 26 1 6.2744.030 PEEK Coupling Connection between 6.2744.010 PEEK compression fitting and 6.1826.0X0 pump tubing set of 4 1 6.2751.070 Splash protection Must be installed at the tower of the 813 Compact Autosampler. 1 6.2752.
4.7 Optional accessories 4.7 Optional accessories Order No. Description 6.1835.020 PEEK needle For aspiration of solutions from open sample tubes 6.1835.000 PEEK needle For aspiration of solutions from open sample tubes 1.5 150 6.2624.000 1.5 Steel needle For aspiration of solutions from sealed sample tubes 150 6.1831.040 6.2833.000 PEEK capillary Length = 15 cm 0.5 1.59 Needle holder (1/8") for PEEK needle 6.1835.010 and 6.1835.020 6.2833.010 Needle holder (1/16") For steel needle 6.
4 Appendix 6.2743.050 PP Sample tube (11 mL) For sample rack 6.2041.750 set of 2000 6.2743.077 PE Caps For sealing the 6.2743.057 sample tubes set of 200 6.2743.060 PE Caps For sealing the 6.2743.0x0 sample tubes set of 1000 6.2125.120 Adaptor for remote connection with 5 connections for remote cables 6.2141.150 6.1826.
4.7 Optional accessories 5 Index key ..................... 5 key .................... 5 key.................... 5 6.1835.010 PEEK needle Insertion ......................... 10 6.1835.020 PEEK tube Insertion ......................... 10 6.2141.020 Remote cable Connection..................... 18 6.2141.130 Remote cable Connection..................... 17 746 VA Trace Analyzer Interconnection .............. 18 A Abort the configuration procedure..................... 22 Accept setting.....
5 Index Installation ...................... 10 Needle guide Figure ............................... 3 Needle holder Figure ............................. 10 Needle installation.......... 10 Ordering designation ..... 46 Needle position................. 13 Pump tubing Connection to needle..... 14 Figure ......................... 3, 15 Installation ...................... 14 Life time.......................... 37 Ordering designation42, 44 Replacement.................. 37 Pump tubing 6.1826.020 ..