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 754 Dialysis Unit 754 Dialysis Unit Metrohm POWER REMOTE PUMP ON ON OFF OFF 8.754.1003 Instructions for Use 19.01.
Table of contents Table of contents 1 Introduction ............................................................................................ 1 1.1 Instrument description............................................................................. 1 1.2 Parts and controls..................................................................................... 2 1.3 Information about the Instructions for Use .......................................... 4 1.3.1 Organization .................................
Table of contents 4 Malfunctions – Maintenance .......................................... 29 4.1 Malfunctions and their rectification..................................................... 29 4.2 Maintenance and servicing ................................................................... 30 4.2.1 Handling dialysis membranes .................................................... 30 4.2.2 Care of the unit............................................................................ 30 4.2.
1.1 Instrument description 1 Introduction 1.1 Instrument description The 754 Dialysis Unit is a unit for on-line sample preparation in ion chromatography permitting the use of automatic sample dialysis directly before sample injection. It consists of a dual-channel peristaltic pump for conveying the sample and acceptor solutions, and the actual dialysis cell in which the ions from the flowing sample solution are enriched in the resting acceptor solution and then injected directly into the IC system.
1 Introduction 1.2 Parts and controls 3 4 5 754 Dialysis Unit Metrohm POWER 2 REMOTE PUMP ON ON OFF OFF 1 10 9 8 7 6 Fig.
1.2 Parts and controls 11 12 13 14 Type 1.754.0010 Nr. f=50-60 Hz S=12 VA Remote Fuse 115V: 110-120V: 0,2A(T) 230V: 220-240V: 0,1A(T) Pump WARNING - Fire Hazard - For continued protection replace only with the same type and rating of fuse S Made by Metrohm Herisau Switzerland 16 15 Fig. 2: Rear of the 754 Dialysis Unit 11 Fuse holder Changing the fuses, see section 2.
1 Introduction 1.3 Information about the Instructions for Use Please read through these Instructions for Use carefully before operating the 754 Dialysis Unit. The Instructions for Use contain information and warnings to which the user must pay attention in order to assure safe operation of the instrument. 1.3.1 Organization These 8.754.
1.4 Support documentation Hazard This symbol draws attention to a possible danger to life or injury if the associated directions are not followed correctly. Warning This symbol draws attention to possible damage to instruments or instrument parts if the associated directions are not followed correctly. Caution This symbol marks important information. Read these directions before continuing. Comment This symbol marks additional information and tips. 1.
1 Introduction 1.5 Safety notes 1.5.1 Electrical safety While electrical safety in the handling of the 754 Dialysis Unit is assured in the context of the specifications IEC 1010-1 (protection class I, degree of protection IP40), the following points should be noted: • Mains connection Set the mains voltage and check the mains fuse and mains connection in accordance with the instructions in section 2.2.
2.1 Setting up the instrument 2 Installation 2.1 Setting up the instrument 2.1.1 Packaging The 754 Dialysis Unit 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 754 Dialysis Unit for the first time, check that the mains voltage set on the instrument (see Fig. 3) matches the local mains voltage.
2.2 Mains connection 115 11 100 – 120 V 11 Fuse holder 230 12 220 – 240 V 13 12 Voltage selection insert with display of voltage 13 Mains switch 16 16 Mains connection plug Fig. 3: Setting the mains voltage 2.2.2 Fuses Two fuses 0.2 A/slow-blow for 100…120 V or 0.1 A/slow-blow for 220…240 V are installed in the fuse holder 11 of the 754 Dialysis Unit as standard.
2 Installation 2.3 Attaching the accessories 2.3.1 Electrical connection to the 732 IC Detector In order to allow remote operation of the pump via the 732 IC Detector, connection 15 of the 754 Dialysis Unit must be connected to the "Remote" connection of the 732 IC Detector by means of the 6.2143.200 cable as per Fig. 4. The switch 2 on the front of the 754 Dialysis Unit must additionally be set to "ON" to permit remote operation. If you wish to connect a second, additional unit (e.g.
2.3 Attaching the accessories 754 Dialysis Unit 2 Connect new feedthrough • Using a wrench or a spanner, unscrew the nut on the interior side of feedthrough 27 and remove the feedthrough. • Insert new 6.2756.000 tubing feedthrough in the hole and retighten the nut. 3 Attach tubing to valve A • Screw 6.1825.210 PEEK sample loop (20 µL) to connections "3" and "6" of valve A 18 using the enclosed 6.2744.010 PEEK compression fittings. • Screw PEEK capillary 19 (6.1831.
2 Installation 20 21 19 22 18 23 24 25 17 STEP FILL INJECT 21 22 INJECT FILL A B 27 41 28 Fig. 5: Interior of the 733.0020 IC Separation Center 12 17 PEEK sample loop (6.1825.210; 20 µL ) 24 PEEK capillary (6.1831.050; 40 cm) 18 Injection valve A 25 PEEK capillary (6.1831.050; 40 cm) 19 PEEK capillary (6.1831.060; 1 m) 21 Connection for syringe 20 PEEK capillary (6.1831.040; 15 cm) 22 Feedthrough 21 PEEK capillary (6.1831.
2.3 Attaching the accessories 2.3.3 Attaching the accessories to the 754 Dialysis Unit Attach the tubing cartridges with the pump tubings to the 754 Dialysis Unit. Proceed as follows (see Fig. 5 and Fig. 8): 754 Dialysis Unit 9 Attach pump tubings • Loosen both tubing cartridges 4 from the holding clamp 7 by pressing down snap-action lever 8 and remove from mounting pin 10 on 754 Dialysis Unit (see Fig. 1). • Press contact pressure lever 5 on both tubing cartridges down as far as it will go.
2 Installation 26/27 28 29 30/31 32 4 5 8 32 29 28 23/33 Fig. 6: Installing pump tubings 4 Tubing cartridge 28 PEEK compression fitting (6.2744.010) 5 Contact pressure lever 29 Coupling (6.2744.030) 8 Snap-action lever 30 Pump tubing (6.1826.040) for conveying the sample 23 PEEK capillary (6.1831.050) for conveying the acceptor solution to valve B 31 Pump tubing (6.1826.030) for conveying the acceptor solution 26 PTFE capillary (6.1803.
2.3 Attaching the accessories Pump tubings are consumable material with a lifetime which depends on the contact pressure. This is why the tubing cartridges should be raised completely by loosening snap-action lever 8 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 6.1826.0X0 pump tubing is made of PVC and must not be used for rinsing with solutions which contain acetone.
2 Installation 4 Close dialysis cell • Place top part 38 on bottom part 35 so that both parts lie flush. • Using the 6.2621.070 Allen key, screw the 5 screws 39 right in and tighten up. 5 Attach dialysis cell • Insert the assembled dialysis cell 34 in the cell holder 6 of the 754 Dialysis Unit. 34 40 35 41 36 42 37 38 43 39 44 40 Fig. 7: Assembling the dialysis cell 16 34 Dialysis cell (6.2729.
2.3 Attaching the accessories 2.3.5 Connecting the dialysis cell To connect the dialysis cell to the IC system proceed as follows (see Fig. 8): 1 Tubing connections for acceptor solution • Mount a PVDF compression fitting 50 (6.2744.000) on the end of PEEK capillary 24 projecting from feedthrough 27 (see Fig. 5). • Screw PEEK capillary 24 to inlet opening 42 of the bottom part 35 of the cell (see Fig. 7). • Mount a PVDF compression fitting 50 (6.2744.
2 Installation 733 20 21 17 27 A 26 19 23 24 25 B Column 45 46 47 Eluent 48 754 49 Acceptor Sample 31 30 29 28 50 50 33 Waste 34 Fig. 8: Diagram of tubing connections 17 PEEK sample loop (6.1825.210; 20 µL) 30 Pump tubing (6.1826.040) for conveying the sample 19 PEEK capillary (6.1831.060; 1 m) Connection Valve A – Waste 31 Pump tubing (6.1826.030) for conveying the acceptor solution 20 PEEK capillary (6.1831.040; 15 cm) Connection Valve A – Valve B 33 PTFE capillary (6.1803.
2.3 Attaching the accessories 2.3.6 Attaching the accessories to the waste bottle The waste bottle which receives the sample and acceptor solutions is connected to the IC system as follows (see Fig. 8): 1 Attach bottle attachment • Screw bottle attachment 48 (6.1602.150) on to waste bottle 49 (6.1608.070). 2 Connect tubing to the dialysis cell • Pull one end of the PTFE capillary 45 connected to the dialysis cell through a PVDF compression fitting 46 (6.2744.000), allowing 5 cm of tubing to project.
2 Installation 2.3.7 Conditioning the dialysis system Before effecting the first analysis, rinse the dialysis cell, the inserted dialysis membrane and all tubing connections with ultrapure water. Proceed as follows: 20 1 Settings on the 733 IC Separation Center • Press the key for injection valve A on the 733 IC Separation Center. This switches injection valve A to the "FILL" position. • Press the key for injection valve B on the 733 IC Separation Center.
3.1 Manual operation 3 Operation The 754 Dialysis Unit cannot be manually operated unless the installation has been carried out properly as described in section 2 (mains connection, attaching pump tubing and dialysis cell, connection to the IC system). 3.1 Manual operation Switch instrument on/off The 754 Dialysis Unit is switched on and off using mains switch 13 on the rear of the instrument (see Fig.
3 Operation 3.2 Operation via 732 IC Detector Switch instrument on/off The 754 Dialysis Unit is switched on and off using mains switch 13 on the rear of the instrument (see Fig. 2): I Instrument switched on 0 Instrument switched off POWER After the instrument has been switched on the power lamp 3 lights up to show that the instrument is ready for use.
3.3 The dialysis procedure 3.3 The dialysis procedure 3.3.1 Dialysis flow chart Every sample dialysed with the 754 Dialysis Unit comprises the following four steps: 1 Rinsing Valve A: Valve B: FILL INJECT Sample channel, acceptor channel and sample loop are rinsed (rinsing time: approx. 2 min). Fill Inject A B Column Eluent Acceptor Waste Sample 2 Dialysis with «Stopped Flow» Valve A: Valve B: FILL FILL The sample is dialysed with resting acceptor solution (dialysis time: approx. 10 min).
3 Operation 3.3.2 Programming with the 732 IC Detector Program without suppression To dialyse in an IC system without suppression a program has to be created for controlling the valves in the 733 IC Separation Center and the 754 Dialysis Unit connected with cable 6.2143.200. The following example program contains the necessary program steps. PROGRAM progr.type: number of cycles Rinsing time Dialysis time Transfer time Programming time cycle 1 0.0 valve A: valve B: remote: fill inject 1******* 2.
3.3 The dialysis procedure 3.3.3 Setting the rinsing time A rinsing time of 2 min is normally sufficient to ensure thorough rinsing of the sample and acceptor channels. This time can be increased if required. 3.3.4 Setting the transfer time The time allowed for transferring the enriched acceptor solution to the sample loop must be set to ensure that the part of the acceptor solution with the highest concentration of ions is transferred to the sample loop.
3 Operation 12.0 Fluoride Chloride Concentration [mg/L] 10.0 Nitrite Bromide Nitrate 8.0 Phosphate Sulphate 6.0 4.0 2.0 0.0 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Transfer time [min] 3.3.5 Setting the dialysis time After calculating the optimum transfer time, determine the optimum dialysis time. This value will depend on the total ion concentration.
3.3 The dialysis procedure 3.3.6 2 Measure the standard with dialysis • Set the dialysis time in the program to 5 min (see section 3.3.2). • Immerse sample suction tubing 26 in the standard used in point 1. • Start the program on the 732 IC Detector with the key. Wait until the LED in the key stops flashing, signalling the end of the evaluation. 3 Additional measurements • Increase the dialysis time in the program (see section 3.3.
3 Operation 28 3 Starting up the IC System • Switch on the 732 IC Detector, load method and set program status to active (see the 732/733 Manual). • Switch on 709 IC Pump and condition IC column (see the 709 Manual). • If applicable, switch on the 753 Suppressor Module and the remote control (see the 753 Manual). • Switch on data evaluation system (e.g. «IC Metrodata for Win95»).
4.1 Malfunctions and their rectification 4 Malfunctions – Maintenance 4.1 Malfunctions and their rectification If difficulties appear with the IC system during analysis, their cause are best investigated in the order separating column → pump → eluent → IC system. An overview of possible malfunctions, their causes and remedies can be found in the instruction manuals of the 732/733 IC System (section 5.3.2).
4 Malfunctions – Maintenance 4.2 Maintenance and servicing 4.2.1 Handling dialysis membranes Dialysis membranes are very sensitive to contact and drying out. Avoid touching them by hand and ensure that the membrane in the cell never dries out. The service life of a dialysis membrane is approx. 1 week under frequent use. Do not hesitate to replace the membrane if signs of decreased yield or blockages become apparent.
4.2 Maintenance and servicing 4.2.4 Shutdown If the dialysis cell is to be switched off a long period of time the acceptor and sample channels should be rinsed with ultrapure water for approx. 10 min. Then remove the inlet and outlet leads from the dialysis cell and block each of the openings 41, 41 42, 42 43 and 44 (see Fig. 7) with a 6.2744.060 dummy stopper. 4.2.
4 Malfunctions – Maintenance 4.2.6 Replacing the dialysis membrane The dialysis membrane may have to be replaced in the following cases (see section 4.1 as well): • Reduced yield from dialysis • Membrane has dried out, or is damaged by deposits or bacterial growth • Irremediable blockage of the sample channel (sample can no longer be conveyed through the dialysis cell) To replace the membrane, proceed as follows (see Fig.
4.2 Maintenance and servicing 754 Dialysis Unit 5 Close dialysis cell • Place top part 38 on bottom part 35 so that both parts lie flush. • Screw the 5 screws 39 in all the way in and tighten using the 6.2621.070 Allen key. 6 Attach dialysis cell • Place the assembled dialysis cell 34 in cell holder 6 of the 754 Dialysis Unit. 7 Connect dialysis cell • Screw PEEK capillary 24 to inlet opening 42 of the bottom part 35 of the cell.
4 Malfunctions – Maintenance 34 754 Dialysis Unit
5.1 Technical data 5 Appendix 5.1 Technical data Dialysis cell Material Plexiglass (polymethyl methacrylate) Solvent compatibility Water, ethanol (no organic sovents!) Cell volume 240 µL (from inlet to outlet opening) Diameter of membrane 47 mm Pump Pump type 2-channel peristaltic pump with rotational speed of 20/min (50 Hz) 24/min (60 Hz) Pump capacity (with water, without counterpressure) with 6.1826.030 pump tubing: typically 0.5…0.6 mL/min with 6.1826.040 pump tubing: typically 0.9…1.
5 Appendix Safety specifications Construction / Testing According to IEC 1010 / EN 61010 / UL 3101-1, protection class I, degree of protection IP40 Safety directions The Instructions for Use include information and warnings to which the user must pay attention in order to assure safe operation of the instrument.
5.2 Standard equipment 5.2 Standard equipment Subject to changes! All dimensions are given in mm. The 2.754.0010 Dialysis Unit includes the following parts: Quant. Order No. Description 1 6.1602.150 Bottle attachment GL45 for 6.1608.070 clear glass bottle GL45 1 6.1608.070 GL45 Clear glass bottle 2 L Waste bottle, with GL45 thread 262 136 1 5 5 1 6.1803.030 6.1803.040 6.1803.050 6.1825.210 PTFE Capillary tubing Length = 5 m 0.5 1.59 PTFE Capillary tubing Length = 1 m 0.5 1.
5 Appendix Quant. Order No. Description 2 6.1831.040 PEEK Capillary tubing Length = 15 cm 0.5 1.59 PEEK Capillary tubing Length = 40 cm 0.5 1.59 PEEK Capillary tubing Length = 1 m 0.5 1.59 3 1 1 1 6.1831.050 6.1831.060 6.2122.0X0 6.2621.070 Mains cable to customer's specifications: Cable socket Cable connector Type IEC 320/C 13 Type IEC 320/C 13 Type CEE (22), V Type SEV 12 (CH…)............................... 6.2122.020 Type CEE (7), VII (D…)........................... 6.2122.
5.3 Optional accessories Quant. Order No. Description 1 6.2756.000 Feedthrough For the 733 IC Separation Center, for feeding through capillary tubings 12 10 1 1 5.3 754 Dialysis Unit 6.2831.010 8.754.1003 Pincette For handling dialysis membranes 120 9 Instructions for use (English) for 754 Dialysis Unit Optional accessories Order No. Description 6.2143.200 Connecting cable Connecting cable 732 IC Detector – 754 Dialysis Unit. 6.2143.
5 Appendix 5.4 Warranty and conformity 5.4.1 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.
5.4 Warranty and conformity 5.4.2 EU Declaration of conformity EU Declaration of Conformity The METROHM AG company, Herisau, Switzerland hereby certifies that the instrument: 754 Dialysis Unit meets the requirements of EC Directives 89/336/EWG and 73/23/EWG.
5 Appendix 5.4.3 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: 754 Dialysis Unit Name of manufacturer: Metrohm Ltd.
5.5 Index 5.5 Index A D Acceptor solution .................................. 13,17,19,26 Air bubbles ...................................................... 20,29 Allen key (6.2621.070)................................ 15,32,38 Ambient temperature............................................ 36 Appendix .............................................................. 35 Application Bulletins ............................................... 5 Application Notes ...................................................
5 Appendix G General precautionary rules................................... 6 H Handling dialysis membranes.............................. 30 Handling of solvents .............................................. 6 Hazard.................................................................... 5 Holding clamp 7 Figure ............................................................... 2 Install tubing cartridges .................................. 13 Housing..............................................................
5.5 Index PEEK compression fitting 28 Figure ........................................................ 14,18 Installation.................................................. 13,14 Ordering designation...................................... 38 PEEK compression fitting 47 Figure ............................................................. 18 Installation....................................................... 19 Ordering designation...................................... 38 PEEK sample loop 17 Figure .............
5 Appendix Storage................................................................. 36 Support documentation ......................................... 5 Suppressor Module 753 ...................................... 11 Switch instrument on/off............................... 9,21,22 Switch off remote control ..................................... 21 Switch on remote control ..................................... 22 Switch pump on/off at an event ........................... 22 Switch pump on/off in a program ....
