850 Professional IC AnCat – MSM-HC – MCS – 2.850.3040 Manual 8.850.
Metrohm AG CH-9101 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com 850 Professional IC AnCat – MSM-HC – MCS – 2.850.3040 Manual 8.850.8028EN 05.
Teachware Metrohm AG CH-9101 Herisau teachware@metrohm.com This documentation is protected by copyright. All rights reserved. Although all the information given in this documentation has been checked with great care, errors cannot be entirely excluded. Should you notice any mistakes please send us your comments using the address given above. Documentation in additional languages can be found on http://products.metrohm.com under Literature/Technical documentation.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents Table of contents 1 Introduction 1 1.1 Instrument description ......................................................... 1 1.2 Intended use ......................................................................... 3 1.3 About the documentation ................................................... 3 1.3.1 Symbols and conventions ........................................................ 3 1.4 Safety instructions .....................................................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents 3.11 Inline filter ........................................................................... 42 3.12 Pulsation damper ............................................................... 43 3.13 Sample degasser ................................................................. 45 3.14 Injection valve ..................................................................... 46 3.14.1 Connecting the injection valve ............................................... 46 3.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents 5.5 High pressure pump ........................................................... 77 5.5.1 Protection .............................................................................. 77 5.5.2 Maintenance ......................................................................... 78 5.6 Inline filter ........................................................................... 88 5.6.1 Maintenance .........................................................................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents 7.7 High pressure pump ......................................................... 111 7.8 Sample degasser ............................................................... 112 7.9 Injection valve ................................................................... 112 7.10 Column thermostat .......................................................... 113 7.11 High Capacity Metrohm Suppressor Module (MSM-HC) .......................................................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Table of figures Figure 1 Figure 2 Figure 3 Figure 4 Figure 5 Figure 6 Figure 7 Figure 8 Figure 9 Figure 10 Figure 11 Figure 12 Figure 13 Figure 14 Figure 15 Figure 16 Figure 17 Figure 18 Figure 19 Figure 20 Figure 21 Figure 22 Figure 23 Figure 24 Figure 25 Figure 26 Figure 27 Figure 28 Figure 29 Figure 30 Figure 31 Figure 32 Figure 33 Figure 34 Figure 35 Figure 36 Figure 37 Figure 38 Figure 39 Figure 40 Figure 41 Figure 42 Figure 43 Figure 44 Front 850 Professiona
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Figure 45 Figure 46 Figure 47 Figure 48 VIII ￭￭￭￭￭￭￭￭ Components of the inlet valve and outlet valve ................................ 86 Changing the filter .......................................................................... 88 MSM-HC – Components ................................................................. 95 Pump tubing connection – Changing the filter ...............................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction 1 Introduction 1.1 Instrument description The instrument 850 Professional IC – AnCat – MSM-HC – MCS (2.850.3040) is one of the model versions of the Professional IC line of instruments manufactured by the Metrohm Company. The Professional IC line of instruments is distinguished by: ￭ ￭ ￭ ￭ ￭ ￭ ￭ the intelligence of its components, which are able to monitor and optimize all functions and to provide documentation according to FDA requirements. its compactness.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1.1 Instrument description used for the purpose of protecting other sensitive components against contaminations in the solutions used. The fine 2 µm material of the readily and easily replaceable filter platelets removes particles such as bacteria and algae from the solutions.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction interactions with the column. The Metrohm analytical columns are equipped with a chip on which their technical specifications and their history (first use / setting up, operating hours, injections, ... ) are saved. 1.2 Intended use The 850 Professional IC is used for the ion chromatographic determination of cations and anions. The two channels can be operated in parallel or completely independently of one another.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1.4 Safety instructions Instruction step Carry out these steps in the sequence shown. Warning This symbol draws attention to a possible life hazard or risk of injury. Warning This symbol draws attention to a possible hazard due to electrical current. Warning This symbol draws attention to a possible hazard due to heat or hot instrument parts. Warning This symbol draws attention to a possible biological hazard.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction Warning Only personnel qualified by Metrohm are authorized to carry out service work on electronic components. Warning Never open the housing of the instrument. The instrument could be damaged by this. There is also a risk of serious injury if live components are touched. There are no parts inside the housing which can be serviced or replaced by the user. Mains voltage Warning An incorrect mains voltage can damage the instrument.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1.4 Safety instructions 1.4.3 Tubing and capillary connections Caution Leaks in tubing and capillary connections are a safety risk. Tighten all connections well by hand. Avoid applying excessive force to tubing connections. Damaged tubing ends lead to leakage. Appropriate tools can be used to loosen connections. Check the connections regularly for leakage. If the instrument is used mainly in unattended operation, then weekly inspections are mandatory. 1.4.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument 2 Overview of the instrument 2.1 Front 1 9 10 11 8 12 2 7 5 3 6 4 2 7 5 3 6 4 Figure 1 1 Front 850 Professional IC – AnCat – MSM-HC – MCS Detector chamber Space for the conductivity detector (see Chapter 3.19, page 63). 850 Professional IC – AnCat – MSM-HC – MCS 2 Eluent degasser See Chapter 3.9, Page 36.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.1 Front 3 High pressure pump See Chapter 3.10, Page 37. 4 Purge valve For deaerating the high pressure pump (see Chapter 3.10.1, page 37). 5 Injection valve See Chapter 3.14, Page 46. 6 Pulsation damper See Chapter 3.12, Page 43. 7 Sample degasser See Chapter 3.13, Page 45. Use optional. 8 Column thermostat See Chapter 3.15, Page 49. 9 Column holder For two separation columns (see Chapter 3.22, page 69) in the column thermostat and one outside the column thermostat.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 2 Overview of the instrument Rear 22 1 21 20 2 19 3 18 4 5 17 6 16 7 8 15 14 9 Figure 2 1 10 11 12 13 Rear 850 Professional IC AnCat – MSM-HC – MCS Knurled screws For fastening the rear panel (2-22) and handle (5-2). 2 Vacuum connection For connecting further degassing chambers in extension modules. Labeled with Vacuum.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.2 Rear 3 Mains switch For switching the instrument on and off. 4 Mains connection socket For connecting the mains cable. 6 MSB connectors 2 MSB connectors (labeled with MSB 1 and MSB 2) for connecting MSB devices I = ON 0 = OFF 5 USB connectors 2 USB connectors (labeled with USB 1 and USB 2). Caution: The 850 must be switched off when connecting a device. MSB = Metrohm Serial Bus.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument Caution When connecting an instrument to the MSB connector (2-6) you must switch off the 850 Professional IC .
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.1 About this chapter 3 Installation 3.1 About this chapter The Installation chapter contains ￭ ￭ ￭ ￭ 3.2 this overview a brief set of instructions for the initial installation of the 850 Professional IC – AnCat – MSM-HC – MCS (see Chapter 3.2, page 12). At each step you will find cross-references to more detailed installation instructions for individual components, should you require such aids. an installation diagram (see Chapter 3.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation ￭ ￭ ￭ Place the detectors in the instrument and connect them (see Chapter 3.6.2, page 24). Connect the leak sensor (see Chapter 3.6.4, page 26). Connect drainage tubings (see Chapter 3.6.5, page 27). 3 Connecting the eluent path ￭ ￭ ￭ ￭ Equip an eluent aspiration tubing for each of the two high pressure pumps and connect with the eluent bottle (see Chapter 3.8.1, page 32). Instead of the columns, connect a 6.2744.040 coupling with a 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.2 Initial installation ￭ ￭ Connect a part of the 6.1803.040 PTFE capillary with a 6.2744.090 long pressure screw to the input of the sample degasser. Guide the other end out of the instrument through a capillary feed-through and connect it to the Sample Processor. Guide the sample outlet capillary connected to the sample output of the injection valve out of the instrument through a capillary feed-through and onward to the waste container and then fasten it there.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 8 Initial start-up (see Chapter 4.1, page 71) ￭ ￭ ￭ ￭ ￭ Switch on the PC and start MagIC Net. Switch on the instrument. Deaerate the high pressure pump (see Chapter 3.10.2, page 40). Set contact pressure of the peristaltic pump (see "Set flow rate", page 59). Rinse instrument without column. 9 Installing guard and separation column ￭ ￭ ￭ ￭ ￭ ￭ Remove the 6.2744.040 coupling between the column inlet capillary and the eluent inlet capillary of the MSM-HC.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.3 Installation diagram 3.3 Installation diagram The following installation diagram shows the capillary connections for a system with a cation channel and an anion channel and sequential suppression (MSM-HC and MCS): Anion channel With the upper high pressure pump, the MSM-HC, the MCS and the left-hand conductivity detector. Cation channel With the lower high pressure pump and the right-hand conductivity detector.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 5 11 10 4 9 26 28 19 18 29 22 3 8 30 7 20 27 1 27 27 23 25 24 17 21 15 28 1 16 6 14 12 13 28 Figure 3 1 2 Installation diagram 850 Professional IC – AnCat – MSM-HC – MCS Eluent aspiration tubing 6.1834.080 Two aspiration tubings for two different eluents (see Chapter 3.8.1, page 32). 850 Professional IC – AnCat – MSM-HC – MCS 2 Column inlet capillary For the cation channel.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.3 Installation diagram 3 Detector inlet capillary 4 Conductivity detector For the cation channel. 5 Detector outlet capillary 6 Column inlet capillary For the anion channel. Connected to the injection valve and threaded into the capillary recesses of the column thermostat. 7 Connection capillary Capillary of the MSM-HC labeled with Eluent. 8 Connection capillary Capillary of the MSM-HC labeled with Detector.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 25 Rinsing solution outlet capillary Capillary of the MSM-HC labeled with Waste. 26 Air aspirating capillary For aspirating CO2-low air from the cartridges of the MCS. 27 PEEK pressure screws, short 6.2744.070 28 PEEK pressure screws, long 6.2744.090 29 Tubing olive 6.2744.030 30 Pump tubing connection with safety device 6.2744.180 3.4 Setting up the instrument 3.4.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.5 Capillary connections in the IC system 4 1 Figure 4 2 3 Connection of capillaries with pressure screws 1 PEEK pressure screw 6.2744.014 Use on the injection valve. 2 Connection capillary 3 PEEK pressure screw, short 6.2744.070 For use on the high pressure pump, the purge valve, the inline filter, the pulsation damper, the guard column and the separation column. 4 PEEK pressure screw, long 6.2744.090 Usage on other components. Is not used on all instruments.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Caution For the capillary connections between the injection valve (see Chapter 3.14, page 46) and detector (see Chapter 3.19, page 63), PEEK capillaries with an internal diameter of 0.25 mm must be used. These are already connected to a newly delivered instrument. PTFE capillaries (polytetrafluoroethylene) PTFE capillaries are transparent and enable visual tracing of the liquids to be pumped. They are chemically inert, flexible and temperature-resistant up to 80°C.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.6 Rear of the instrument 1 1 2 3 5 4 Figure 5 Rollers and handle 1 Knurled screws For fastening the handle (5-2) and the rear panel of the detector chamber. 2 Handle 3 Knurled screws For fastening the roller holder (5-5). 4 Rollers 5 Roller holder Removing handle 1 Loosen knurled screws (5-1) and remove handle (5-2). Removing rollers Proceed as follows to remove the rollers: 1 Remove knurled screws (5-3). 2 Remove roller holder (5-5).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Mounting handle as MPak holder Note When extended, the handle (6-2) can also be used for hanging up MPaks (eluent bags). 1 Move handle (6-2) upwards and screw in the knurled screws (6-1) again. 2 1 1 Figure 6 1 Handle as MPak holder Knurled screws For fastening the handle (6-2) and the rear panel of the detector chamber. 850 Professional IC – AnCat – MSM-HC – MCS 2 Handle Extended. As holder for MPaks (eluent bag).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.6 Rear of the instrument 3.6.2 Positioning and connecting the detector 4 4 1 1 1 2 3 3 4 4 1 1 1 5 Figure 7 Detector 1 5 Detector 2 Removable rear panel 1 Knurled screws For fastening the removable rear panel. 2 Rear panel Removable 3 Cable feed-throughs For feeding through detector cables. 4 Capillary feed-throughs 5 Detector connection sockets Labeled with Detector 1 and Detector 2 for connecting Metrohm detectors.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Note Up to two detectors can be positioned and connected. Caution The instrument must be turned off when connecting a detector. 1 Removing rear panel ￭ ￭ ￭ Unscrew knurled screws (7-1) on the rear panel. Remove handle if still fastened to the instrument. Remove rear panel (7-2). 2 Positioning the detector ￭ Put the detector through this opening and position it on the support surface intended for this purpose. Slide it right up to the front.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.6 Rear of the instrument ￭ Connect the detector cable to the detector connection socket Detector 1 (7-5). 5 Conntecting detector output Note The detector output capillary must be free of blockages (the measuring cell is tested to 5 MPa = 50 bar backpressure). Guide the detector output capillary into a sufficiently large waste container and fasten it there. 3.6.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 1 2 Figure 8 Connection for the leak sensor on the rear of the instrument 1 Leak sensor connector socket Is labeled with "Leak Sensor". 3 Leak sensor connection cable Is firmly mounted on the rear of the instrument. 3.6.5 3 2 Leak sensor connector plug Drainage tubing Fluid that escapes in the covering plate or in the detector chamber flows through the drainage tubing into the base tray and past the leak sensor into the waste container.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.6 Rear of the instrument 1 2 3 4 5 6 7 8 9 Figure 9 Drainage tubing 1 Drainage tubing connection For draining escaped fluid from the covering plate. 2 Drainage tubing Section of the 6.1816.020 silicon tubing. For draining escaped fluid from the covering plate. 3 Drainage tubing connection For draining escaped fluid from the detector chamber. 4 Drainage tubing Section of the 6.1816.020 silicon tubing. For draining escaped fluid from the detector chamber.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 7 Drainage tubing Section of the 6.1816.020 silicon tubing. Guides escaped fluid into a waste container. 9 Drainage tubing connection For supplying escaped fluid through the connected drainage tubing to the leak sensor. 8 Drainage tubing connection For draining escaped fluid from the base tray through the connected drainage tubing.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.7 Capillary and cable feed-throughs 4 1 2 3 1 2 Figure 10 Capillary feed-throughs on the doors 1 Luer connectors For connecting a 6.2816.020 syringe. For manual sample feeding. 2 Capillary feed-through 3 PEEK pressure screws, short 6.2744.070 4 Door Do not feed capillaries through the Luer connectors (10-1). The capillaries are fastened with PEEK pressure screws (10-3) from inside to the Luer connector.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 3 Installation 6 7 8 8 Rear 6 5 Front 2 1 7 4 3 9 Figure 11 10 11 12 12 11 10 9 Capillary feed-throughs base tray/covering plate 1 Side panel (right) Right panel. 2 Rear of the instrument 3 Side panel (left) Left panel. 4 Front of the instrument 5 Capillary feed-through Upper. From front to right. 6 Capillary feed-through Upper. From front to back. 7 Capillary feed-through Upper. From front to back. 8 Capillary feed-through Upper.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.8 Eluent 3.8 Eluent 3.8.1 Connecting eluent bottle The eluent is aspirated out of the eluent bottle via the eluent aspiration tubing (12-1). The eluent aspiration tubing is connected to the eluent degasser (see Chapter 3.9, page 36). The tubing must be threaded through a suitable capillary feed-through (see Chapter 3.7, page 29) of the instrument before the other end can be equipped.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 1 3 2 Figure 12 4 Installing eluent bottle attachment 1 Eluent aspiration tubing 6.1834.080 2 Tubing nipple From accessory set 6.1602.160. 3 O-ring From accessory set 6.1602.160. 4 Bottle attachment From accessory set 6.1602.160. 3 Mounting aspiration filter ￭ Insert filter holder (13-1) into the aspiration filter (13-2) and screw tight. 1 Figure 13 1 Filter holder From accessory set 6.2744.210.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.8 Eluent 4 Installing tubing weighting and aspiration filter 1 3 2 Figure 14 4 5 Installing tubing weighting and aspiration filter 1 Eluent aspiration tubing 6.1834.080 2 Eluent bottle attachment 6.1602.160 3 Tubing weighting From accessory set 6.2744.210. 4 Clamping screw From accessory set 6.2744.210. 5 Aspiration filter 6.2821.090 With filter holder from accessory set 6.2744.210.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Fasten the bottle attachment (14-2) on the eluent bottle (16-10). The aspiration filter (16-6) must rest on the base of the eluent bottle. ￭ 6 Mounting the adsorber tube Note In the case of alkaline eluents and eluents with lower buffer capacity, the eluent bottle must be equipped with a CO2 adsorber (16-4). First, place a piece of wadding (16-3), then the CO2 adsorber (16-4) in the large opening of the adsorber tube (16-2) and close with the plastic cover.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.9 Eluent degasser 5 Eluent 6 Aspiration filter 6.2821.090 7 Filter holder From accessory set 6.2744.210. 8 Clamping screw From accessory set 6.2744.210. 9 Tubing weighting From accessory set 6.2744.210. 10 Eluent bottle 6.1608.070 11 Bottle attachment 6.1602.160 12 SGJ clip 6.2023.020 13 Tubing nipple 14 Thread stopper 3.9 Eluent degasser Gas bubbles in the eluent lead to an unstable baseline, as high pressure pumps can transport liquids, but not gases.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Tubing flare With tubing nipple. 4 Clamping screw 5 Eluent aspiration tubing 6.1834.080 For aspirating the eluent. The clamping screw (17-4) is firmly mounted. 6 Connection capillary 6.1834.090 Connection from the eluent degasser to the high pressure pump (see Chapter 3.10, page 37). The clamping screw (17-4) is firmly mounted. 1 Caution The clamping screws (17-4) must be tightened carefully. Use the 6.2621.050 wrench for this. ￭ ￭ 2 ￭ ￭ ￭ 3.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.10 High pressure pump 2 13 1 2 3 4 12 5 2 6 2 11 2 7 10 2 8 9 Figure 18 2 Capillary connections high pressure pump/purge valve 1 Connection capillary PEEK capillary, connects main piston and auxiliary piston. 2 PEEK pressure screw, short 6.2744.070 3 Outlet valve holder 4 Pump head 6.2824.110 5 Fastening screws For fastening the pump head. 6 Inlet valve holder 7 Pump head input capillary PEEK capillary at the input of the pump head.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Note The eluent aspiration tubing is already installed in the newly delivered instrument. The following installation instructions need not be carried out at the time of initial installation. Connecting inlet to the high pressure pump 5 1 2 Figure 19 1 3 High pressure pump – Connect inlet Pressure screw For connecting the coupling (19-2) to the pump head input capillary (18-7). 2 Coupling 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.10 High pressure pump 3.10.2 Deaerating the high pressure pump The high pressure pump will only operate perfectly if the pump head contains no more air bubbles. Therefore it must be deaerated during initial start-up and after every change of eluent. Caution The high pressure pump must not be deaerated before the initial startup (see Chapter 4.1, page 71).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Deaerating the high pressure pump The instrument must be connected to the PC and switched on to deaerate the high pressure pump. 5 4 5 6 3 7 2 5 1 Figure 20 Deaerating the high pressure pump 1 Syringe 10 mL 6.2816.020 For aspirating the eluent. 2 Luer connector On purging needle. 3 Purging needle 6.2816.040 4 Deaerating capillary 5 PEEK pressure screws, short 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.11 Inline filter 4 Setting the flow rate ￭ ￭ ￭ Start MagIC Net (if not yet started). Ensure that the eluent aspiration tubing is immersed sufficiently in the eluent. Let the high pressure pump run. 5 Aspirating eluent ￭ Aspirate with the syringe (20-1) until bubble-free eluent flows into the syringe. 6 Completing deaerating ￭ ￭ ￭ ￭ 3.11 Turn off high pressure pump. Close rotary knob (20-7). Remove syringe (20-1) from the Luer connector (20-2).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Installing the inline filter Caution Observe the flow direction marked on the filter housing for the connection of the inline filter. 1 Figure 21 2 3 2 4 Connecting inline filter 1 Connection capillary Connects the purge valve with the inline filter 2 PEEK pressure screws, short 6.2744.070 3 Inline filter 6.2821.120 Protects against particles. 4 Connection capillary Connects the inline filter with the pulsation damper.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.12 Pulsation damper The pulsation damper protects the separation column from damage caused by pressure fluctuations when switching the injection valve, and reduces interfering pulsations during highly sensitive measurements. In order to ensure these functionalities, it must be connected between the high pressure pump (see Chapter 3.10, page 37) and injection valve (see Chapter 3.14, page 46). The pulsation damper can be operated in both directions.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.13 3 Installation Sample degasser The sample degasser removes gas bubbles and disolved gases from the sample. For degassing, the sample flows into a vacuum chamber through a special fluoropolymer capillary. Gas bubbles in the sample lead to poor reproducibility, as the quantity of sample in the sample loop would not always be the same. Samples (containing gas) should therefore be degassed before injection.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.14 Injection valve 4 Guide the other end of the connection capillary out of the instrument through a capillary feed-through. Caution If the sample degasser is not used, the input and output must be sealed with the 6.2744.220 thread stoppers. 3.14 Injection valve The injection valve connects the eluent and sample path.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Connection capillary Connected to connector 4. Carries eluent to the injection valve. 4 Connection capillary (column inlet capillary) Connected to connector 5. Carries eluent to the separation column. 5 Connection capillary Connected to connector 1. Carries sample to the injection valve. 6 Connection capillary Connected to connector 2. Carries sample to the waste container. 7 PEEK pressure screw 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.14 Injection valve 3 4 2 3 4 1 3 2 6 1 3 A 6 B 5 4 1 Figure 25 5 4 2 5 1 2 Injection valve – Positions A Position FILL B Position INJECT 1 Eluent input Capillary coming from the high pressure pump. 2 Eluent output Capillary to the column. 3 Sample input Sample aspirating capillary. 4 Sample output Capillary to waste container. 5 Sample loop 3.14.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.15 3 Installation Column thermostat The column thermostat controls the temperature of the column and eluent channel and thus ensures stable measuring conditions. It provides space for 2 separation columns.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.15 Column thermostat 1 3 1 2 2 1 1 1 Figure 26 1 Column thermostat Capillary feed-throughs For guiding the capillaries in and out. 2 Capillary recesses For controlling the temperature of the eluent. Preheating capillary already pre-installed. 3 Column holder For fastening the columns. With column recognition. The column thermostat contains two column holders (26-3) equipped with chip recognition.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Note The column input capillary is already threaded into the capillary recesses of the column thermostat at the time the instrument is first delivered. The following installation instructions need not be carried out at the time of initial installation. Threading capillaries 1 Introduce column input capillary into the column thermostat via a suitable capillary feed-through (26-1).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.16 High Capacity Metrohm Suppressor Module (MSM-HC) 3.16 High Capacity Metrohm Suppressor Module (MSM-HC) 3.16.1 General information on the MSM-HC The MSM-HC is used for chemical suppression during anion analysis if eluents with a high ionic concentration are used or if the concentration is being significantly increased in the course of a gradient application.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 4 8 1 1 2 2 3 5 7 6 Figure 27 MSM-HC – Connectors 1 Union nut 2 MSM-HC connecting piece 6.2835.010 3 Eluent inlet capillary Labeled with Eluent. 4 Eluent outlet capillary Labeled with Detector. 5 Rinsing solution inlet capillary Labeled with H2O. 6 Rinsing solution outlet capillary Labeled with Waste. 7 Regeneration solution outlet capillary Labeled with Waste. 8 Regeneration solution inlet capillary Labeled with H2SO4.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.16 High Capacity Metrohm Suppressor Module (MSM-HC) Connecting the capillaries of the MSM-HC 1 Connecting the eluent inlet capillary ￭ Fasten the end of the inlet capillary labeled with Eluent with a 6.2744.070 short PEEK pressure screw to the output of the column. 2 Connecting the eluent outlet capillary ￭ Fasten the end of the outlet capillary labeled with Detector with a long PEEK pressure screw (6.2744.090) to the input of the MCS.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3.17 Peristaltic pump 3.17.1 Principle of the peristaltic pump The Peristaltic pump is used for pumping sample and auxiliary solutions. It can rotate in both directions. The peristaltic pump pumps liquids according to the principle of displacement. The pump tubing is clamped between the rollers (28-3) and the tubing cartridge (28-5).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.17 Peristaltic pump 3.17.2 1 Installing the peristaltic pump 2 3 4 5 6 7 8 1 6.2744.180 6.2744.160 9 Figure 29 10 6 3 7 8 Installing the pump tubing 1 PEEK pressure screws, short (6.2744.070) 2 Tubing olive (6.2744.034) 3 Stopper The colors of the stopper indicate the inner diameter of the pump tubing. 4 Tubing cartridge (6.2755.000) 5 Contact pressure lever 6 Union nut 7 Adapter 8 Tubing olive Either with filter holder (6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Connecting the pressure side Note Depending on the use of the peristaltic pump, on the pressure side you can either connect: ￭ ￭ Case A: a 6.2744.180 pump tubing connection with filter (see Figure 30, page 57) or Case B: a 6.2744.160 pump tubing connection without filter (see Figure 31, page 58). For pumping the auxiliary solutions to the MSM or to the SPM, a 6.2744.180 pump tubing connection with filter must be used. Case A: 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.17 Peristaltic pump 1 Figure 31 1 Union nut 3 Tubing olive 2 3 Install pump tubing connection without filter 2 ￭ ￭ ￭ ￭ Adapter Slide union nut (31-1) onto the pump tubing. Select a suitable adapter (31-2) and slide it onto the pump tubing. The type of adapter depends on the pump tubing (see Table 1, page 58). Place the tubing olive (31-3) onto the pump tubing. Screw the union nut (31-1) onto the tubing olive (31-3).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Pump tubing Adapter 6.1826.340 (black/black) 6.1826.360 (white/white) 6.1826.380 (gray/gray) 6.1826.390 (yellow/yellow) Set flow rate The contact pressure of the tubing cartridge must be adjusted in order to regulate the flow rate. Proceed as follows: Set the contact pressure 1 ￭ ￭ ￭ ￭ Fully loosen the contact pressure lever (29-5), i.e. press it all the way down. Switch on the peristaltic pump.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.18 Metrohm CO2 suppressor (MCS) 3.18 Metrohm CO2 suppressor (MCS) 3.18.1 General information on the MCS The MCS removes the CO2 from the eluent flow. This reduces the background conductivity, improves the detection sensitivity and minimizes the injection and carbonate peaks. The MCS is used for removing CO2 from the eluent flow before detection. CO2 can reach the eluent flow through the sample itself or arise through the suppression reaction in the MSM.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Aspirating capillary For aspirating air low in CO2 (as a result of CO2 adsorption cartridge (33-4)). 4 PEEK pressure screw, long 6.2744.090 5 Capillary connection 6 Pressure screw, short 6.2744.070 Mounted on the air aspirating capillary. 7 Luer coupling 6.2744.120 Mounted on the air aspirating capillary with pressure screw 6.2744.070. Connecting the MCS 1 Connecting the MSM Connect the eluent output capillary (labeled with Detector) using a 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.18 Metrohm CO2 suppressor (MCS) 8 3 3 7 6 5 9 1 Figure 33 2 3 4 3 Adsorption cartridge holder 1 PEEK pressure screw, short 6.2744.070 2 Luer coupling 6.2744.120 3 Clips For fastening the adsorption cartridges. 4 CO2 adsorption cartridge 6.2837.000 For removing the CO2 from the aspirated air. 3-layer filled, blue-brown-gray. 5 Adapter 6.1808.190 For connecting the H2O adsorption cartridge and CO2 adsorption cartridge.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 2 Removing the caps ￭ ￭ Remove the two locking caps at the tip of the two cartridges. In the case of the H2O adsorption cartridge, replace the round sealing cap on the larger end with the star-shaped sealing cap. 3 Connecting the CO2 adsorption cartridge ￭ ￭ Insert the CO2 adsorption cartridge into the coupling (33-2) on the end of the MCS aspirating capillary .
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.19 Conductivity detector 1 3 2 Figure 34 1 IC detector 1.850.9010 3 Detector input capillary Permanently installed.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 1 3 2 Figure 35 1 Detector cable With mounted plug. 3 Type plate With serial number. Conductivity detector rear 2 Detector output capillary Permanently installed. Note In order to prevent unnecessary peak widening after separation, the connection between the outlet of the separation column and the inlet in the detector should be kept as short as possible.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.20 Connecting the instrument 3 Figure 36 1 Detector input capillary 3 MCS output 2 1 Connection detector – MCS 2 Pressure screw, long 6.2744.090 3.20 Connecting the instrument 3.20.1 Connecting the instrument to the PC Note The instrument must be turned off when connecting the PC. 1 Connecting the USB cable Connect the PC connection socket (2-18) of the instrument to a USB connector of the computer via the 6.2151.020 USB cable. 3.20.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation The mains cable is three-core and provided with a plug with grounding. If another plug has to be mounted, the yellow/green conductor (IEC standard) must be connected to the protective ground (protection class I). 1 Connecting the mains cable ￭ ￭ Plug the mains cable into the mains connection socket (2-4). Connect the mains cable to the mains supply. 2 Switching the instrument on and off Switch the instrument on and off with the mains switch (2-3).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.21 Guard column Note The guard column may only be installed after the initial start-up (see Chapter 4.1, page 71) of the instrument. Until then, use the 6.2744.040 coupling instead of the guard and separation column. Connecting and rinsing the guard column 1 Connecting the guard column Caution When inserting the guard column, always ensure that it is inserted correctly corresponding to the flow direction (if indicated).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.22 3 Installation Separation column The intelligent separation column (iColumn) is the heart of the ion chromatographic analysis. It separates the different components corresponding to their interactions with the column. Metrohm analytical columns are equipped with a chip on which their technical specifications and their history (first use / setting up, operating hours, injections, ... ) are saved.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.22 Separation column Connecting and rinsing the separation column 1 Connecting the separation column Caution When using the columns, always ensure that these are correctly inserted corresponding to the flow direction indicated. ￭ ￭ Remove stoppers from the separation column. Connect the lower end of the separation column with a 6.2744.070 short PEEK pressure screw to the outlet capillary of the guard column (if used), or to the column input capillary .
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up 4 Start-up The chapter Start-up is divided into 2 sections: 4.1 Initial start-up The initial start-up is carried out during the initial installation. Conditioning Conditioning is carried out as a final installation step and each time after the system is started. Initial start-up The initial start-up is carried out during the initial installation. The entire system is flushed before guard column and separation column are installed.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.2 Conditioning 4 Setting the contact pressure of the peristaltic pump Note This work step needs to be performed only if a peristaltic pump is being used. ￭ If peristaltic pumps are used, set the contact pressure (see "Set flow rate", page 59). 5 Rinsing the instrument without columns ￭ Rinse the instrument (without columns) with eluent for 5 minutes. The instrument is now prepared for the installation of the columns (see Chapter 3.21, page 67). 4.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up 2 Preparing the instrument ￭ ￭ Ensure that the column is correctly mounted in accordance with the flow direction indicated on the label (arrow must point in the direction of flow). Ensure that the eluent aspiration tubing is immersed in the eluent and that there is enough eluent in the eluent bottle. 3 Checking leak-tightness ￭ ￭ In MagIC Net, start the equilibration.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.1 General information 5 Operation and maintenance 5.1 General information 5.1.1 Care Warning The instrument housing must not be opened by untrained personnel. The instrument requires appropriate care. Excess contamination of the instrument may result in functional disruptions and a reduction in the service life of the sturdy mechanics and electronics.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.1.3 5 Operation and maintenance Operation Caution In order to avoid disturbing temperature influences, the entire system including the eluent bottle must be protected against direct sunlight. 5.1.4 Shutting down If the instrument is shut down for a longer period, the entire IC system (without separation column) must be rinsed salt-free with methanol/ultra pure water (1:4), in order to prevent eluent salts from forming crystals which may cause subsequent damage.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.3 Door 5.3 Door Caution The door is made of PMMA (polymethylmetacrylate). It must never be cleaned with abrasive media or solvents. Caution Never use the door as a handle. 5.4 Eluent 5.4.1 Production The chemicals used for the production of eluents should have a degree of purity of at least "p.a.". Only ultra pure water (resistance > 18.2 MΩ*cm) may be used for dilution (this generally applies for reagents which are used in ion chromatography).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.4.2 5.4.2.1 5 Operation and maintenance Operation Supply bottle The supply bottle with the eluent must be connected as indicated in Chapter 3.8.1, Page 32. This is above all important for eluents with volatile solvents (e.g. acetone). Moreover, condensation must also be prevented in the eluent bottle. Drop formation can change the concentration ratio in the eluent. 5.4.2.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.5 High pressure pump Caution In order to spare the pump seals, the pump should not be operated dry. Therefore ensure that the eluent supply is correctly connected and that there is enough eluent in the eluent bottle each time before turning on the pump. 5.5.2 Maintenance Caution Maintenance work on the high pressure pump may not be carried out unless the instrument is switched off.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance Cleaning/replacing the zirconium oxide piston Clean one piston after the other as follows: 1 Removing the piston cartridge from the pump head Loosen the piston cartridge with a wrench and unscrew from the pump head by hand. 1 2 Figure 37 1 Removing piston 2 Pump head Piston 2 Dismantle the piston Caution On the inside of the piston cartridge there is a taut spring than can jump out of the piston cartridge if suddenly loosing tension.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.5 High pressure pump ￭ 1 Figure 38 2 3 Remove the backup ring from the pump head and lay to the other parts. 4 5 6 8 7 Components of the piston cartridge 1 Piston cartridge screw 2 Retaining washer 3 Zirconium oxide piston with piston shaft Order number: 6.2824.070. 4 Spring retainer 5 Spring Order number: 6.2824.060. 6 Inner plastic sleeve Protects from metallic abrasion.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance parts: a tip for removing the old piston seal and a sleeve for inserting the new piston seal. 1 2 Figure 39 1 Tool for piston seal 6.2617.010 2 Pin Pin for removing the old piston seal. Sleeve Sleeve for inserting the new piston seal. Caution Screwing the 6.2617.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.5 High pressure pump 1 2 Figure 40 1 Removing the piston seal 2 Piston seal Tool for piston seal Pin of the tool. 2 Inserting the new piston seal into the tool Insert the new piston seal tightly by hand into the recess of the sleeve of the tool for the piston seal (39-2). The sealing springs must be visible from the outside. 1 2 Figure 41 1 Tool for piston seal 6.2617.010 Sleeve for inserting the new piston seal.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance 1 2 Figure 42 Inserting the piston seal into the pump head 4 Replacing the piston cartridge Screw the assembled piston cartridge back into the pump head and tighten, first by hand, then additionally by approx. 15° with a wrench. Cleaning the inlet valve and outlet valve 1 Removing valves ￭ ￭ Unscrew the connection capillary for the auxiliary piston (18-1) from the outlet valve holder.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.5 High pressure pump 1 2 3 4 Figure 43 Removing valves 1 Outlet valve holder 2 Outlet valve Order number: 6.2824.160 3 Inlet valve Order number: 6.2824.170 4 Inlet valve holder 2 Cleaning undissected valve Clean contaminated or blocked valves initially without dismantling them completely. ￭ ￭ Rinse the valve in eluent flow and counterflow direction using a spray bottle filled with ultra pure water, RBS solution or acetone.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance ￭ ￭ Place the valve with the seal faced downwards above the recess in the holder. Push the valve components out of the valve housing using the needle of the tool. 1 2 3 4 Figure 44 Dismantling valve 1 Needle For pushing the valve components out of the valve housing. 2 Valve 3 Holder 4 Recess For collecting the valve components. The components of the valve are collected in the recess of the holder.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.5 High pressure pump 1 Figure 45 2 3 4 5 5 6 6 7 9 8 8 9 7 10 10 Components of the inlet valve and outlet valve 1 Inlet valve 6.2824.170 2 Outlet valve 6.2824.160 3 Inlet valve housing 4 Outlet valve housing 5 Sealing ring (black) 6 Sleeve 7 Sapphire sleeve The shiny side must point to ruby ball. 8 Ruby ball 9 Ceramic holder for ruby ball 10 Seal The larger opening must point outwards.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance ￭ ￭ ￭ Place the valve housing over the stacked components and hold it tightly. By tilting the tool, the valve components slide into the valve housing. Press the seal by hand well on the valve housing. 6 Checking the flow direction Rinse the valve in the direction of the arrow on the valve housing and check wether liquid is escaping on the other end.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.6 Inline filter Mounting the pump head Note To prevent the pump head from being positioned the wrong way, it is provided with different bore hole depths for the fastening bolts, i. e. a fastening bolt is longer than all others. The bore hole with the greatest depth must therefore be assigned to the longest bolt. If this is not the case, the pump will not function perfectly. 1 Mount the pump head on the pump again using the four fastening screws (18-5).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance Changing the filter The flow must be stopped before changing the filter. 1 Removing the inline filter ￭ Unscrew the pressure screws (46-1) from the inline filter. 2 Unscrewing the filter screw ￭ Screw the filter screw (46-4) out of the filter housing (46-2) with the aid of two 6.2621.000 adjustable wrenches. 3 Inserting the filter ￭ ￭ Remove the old filter (46-3) with tweezers.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.7 Inline sample preparation 5.7 Inline sample preparation To protect the separation column (see Chapter 3.22, Page 69) against foreign particles which can affect the separating efficiency, we recommend that all samples undergo a microfiltration (filter 0.45 µm). The ultrafiltration cell can be used for filtration (see documentation on the IC Equipment for Ultrafiltration). Samples containing significant amounts of gas should be degassed. The sample degasser (see Chapter 3.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance 2 Aspirating the sample and measuring time Aspirate a sample typical for the later application and use a stop watch to measure the time required by the sample to travel from the sample vessel to the end of the sample loop. The time measured corresponds to the "transfer time". The rinsing time should be at least 3 times the transfer time.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.9 Sample degasser 5.9 Sample degasser 5.9.1 Operation If you are working with sample degassing, the longer "transfer time" (see Ascertaining the transfer time, page 90) means that it is also necessary to rinse for longer (with the subsequent sample). The rinsing time should be at least 3 times the "transfer time" so as to minimize the carry-over effects. The "transfer time" itself depends on the pump capacity, total capillary volume and volume of gas removed (i.e.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance The MSM-HC consists of 3 suppressor units, which are used for suppression, regenerated with sulfuric acid or rinsed with ultra pure water in rotation. In order to record every new chromatogram under comparable conditions, you should normally work with a freshly regenerated suppressor. Caution The MSM-HC must never be switched over in a dry state, as there is a risk of jamming.
5.11 High Capacity Metrohm Suppressor Module (MSM-HC) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Regenerating the MSM-HC Caution The pump tubings made of PVC must not be used for rinsing with solutions containing organic solvents. In this case, other pump tubings must be used for rinsing. Note The high pressure pump can be used for regeneration. For this, remove the guard column and separation column and connect the capillary directly to the MSM-HC (regenerate in opposite direction).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 5 Operation and maintenance 2 3 4 5 Figure 47 MSM-HC – Components 1 Union nut 2 MSM-HC connecting piece 6.2835.010 3 MSM-HC rotor A 6.2842.000 4 MSM-HC housing 5 Slot in the MSM-HC housing Cleaning the MSM-HC Clean the MSM-HC as follows: 1 Disconnecting the MSM-HC from the IC system ￭ ￭ Switch off the instrument. Disconnect the MSM-HC from the separation column, peristaltic pump and detector.
5.11 High Capacity Metrohm Suppressor Module (MSM-HC) ￭ ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Check whether solution emerges at the MSM-HC connecting piece (47-2). If one of the supply or discharge lines remained blocked, the MSM-HC connecting piece (47-2) must be replaced (order number 6.2835.010). 4 Cleaning the MSM-HC rotor A ￭ Clean the sealing surface of the MSM-HC rotor A (47-3) with ethanol using a lint-free cloth.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.11.3.3 5 Operation and maintenance Replacing parts of the MSM-HC It may be necessary to replace parts of the MSM-HC in the following cases: ￭ ￭ Loss of suppression capacity which cannot be eliminated (reduced phosphate sensitivity and/or significant rise in the baseline). Blockage of the MSM-HC which cannot be eliminated (solutions can no longer be pumped through the suppressor).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.12 Peristaltic pump ￭ ￭ Insert the new MSM-HC rotor A (47-3) in the MSM-HC housing (47-4) in such a way that the tubing connections on the rear of MSM-HC rotor A fit into the corresponding recesses inside the MSM-HC housing and one of the three holes of MSM-HC rotor A is visible from below in the slot (47-5) of the MSM-HC housing. If the MSM-HC rotor A (47-3) is correctly inserted, its sealing surface will be approx. 4 mm within the MSM-HC housing (47-4).
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance Caution The 6.1826.xxx pump tubings consist of PVC or PP and therefore must not be used for rinsing with solutions containing acetone. In this case, use other pump tubings or use another pump for rinsing. 5.12.2 Maintenance 5.12.2.1 Pump tubing The pump tubing used in the peristaltic pump is a consumable whose service life is restricted.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.12 Peristaltic pump Order number Name Material Inner diameter Use 6.1826.330 Pump tubing LFL (orange/white), 3stopper PVC (Tygon) 0.64 mm No special applications. 6.1826.340 Pump tubing LFL (black/black), 3-stopper PVC (Tygon) 0.76 mm For the sample solution in inline dialysis. 6.1826.360 Pump tubing LFL (white/white), 3-stopper PVC (Tygon) 1.02 mm For sample transfer. 6.1826.380 Pump tubing LFL (gray/gray), 3-stopper PVC (Tygon) 1.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance 3 Mounting filter screw ￭ Screw the filter screw (48-3) back into the tubing olive (48-1) and tighten by hand. Then additionally tighten with two 6.2621.000 adjustable wrenches. 5.13 Metrohm CO2 suppressor (MCS) 5.13.1 Replacing the CO2 adsorption cartridge The CO2 adsorption cartridge 6.2837.000 (33-4) must be replaced regularly. This is because of blockages and losses in capacity. Blockage Moisture can block the CO2 adsorption cartridge.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.14 Conductivity detector 5.14 Conductivity detector 5.14.1 Maintenance Caution The conductivity detector must not be opened! Warning When rinsing the detector, the pressure must not exceed 5 MPa. In order to ensure this, the maximum pressure of the high pressure pump must be set to 5 MPa in MagIC Net. If the conductivity detector is blocked, you should first of all check whether the blockage results from the capillary ends being pressed together too firmly.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.15.2 5 Operation and maintenance Protection To protect the separation column against foreign particles, which can affect the separating efficiency, we recommend that both the eluent and the samples undergo a microfiltration (filter 0.45 µm) before being aspirated via the 6.2821.090 aspiration filter. The use of guard columns (see Chapter 3.21, page 67) serves for protecting the actual separation columns and increases their service life considerably.
5.16 Quality Management and validation with Metrohm 5.16 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Quality Management and validation with Metrohm Quality Management Metrohm offers you comprehensive support in implementing quality management measures for instruments and software. Further information on this can be found in the brochure «Quality Management with Metrohm» available from your local Metrohm agent. Validation Please contact your local Metrohm agent for support in validating instruments and software.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting 6 Troubleshooting 6.1 Problems and their solutions Problem Cause Remedy Marked drop in pressure Leak in the system. Check and seal connections (see Chapter 3.5, page 19). Marked rise in pressure 6.2821.120 inline filter blocked. Replace 6.2821.130 filter (see Chapter 5.6, page 88). MSM-HC – blocked. ￭ Regenerate the MSM-HC (see Chapter 5.11.3.1, page 93). Note: 6.2821.180 pump tubing connection with filter must be used . Conductivity detector blocked.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.1 Problems and their solutions Problem Peak areas lower than expected Peristaltic pump – insufficient or no delivery rate Very noisy baseline 106 ￭￭￭￭￭￭￭￭ Cause Remedy Eluent – Evaporation of the organic solvent in the eluent. Check the eluent bottle attachment (see Figure 14, page 34). Sample – Leak in the sample path. Check the sample path. Sample – Blockage in the sample path. Check the sample path. Sample – Sample loop not (completely) filled.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Problem 6 Troubleshooting Cause Remedy MCS – vacuum pump defective. Contact the Metrohm Service. MSM-HC – not connected. Connecting the MSM-HC (see Chapter 3.16, page 52). MCS – not connected. Connect the MCS. Incorrect eluent. Change eluent (see Chapter 5.4.2.3, page 77). MSM-HC – regeneration or rinsing solution flow problems. Check the flow of the regeneration and rinsing solution (see Chapter 3.16.2, page 52). Column chip contaminated.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.1 Problems and their solutions Problem Cause Remedy ￭ Replace separation column (see "Connecting and rinsing the separation column", page 70). Conductivity detector is not recognized in the software No connection. ￭ Extreme spread of the peaks in the chromatogram. Splitting (dual peaks) Connections – dead volume in the system. Check the connections (see Chapter 3.5, page 19) (use PEEK capillaries with an internal diameter of 0.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Problem Vacuum is not being built 6 Troubleshooting Cause Remedy Eluent – Gas bubbles in the eluent. Check connections of the eluent degasser (see Chapter 3.9, page 36). High pressure pump – defective. Request Metrohm Service. Eluent Degasser – Connector Vacuum on the rear of the instrument not (tightly) sealed. ￭ 850 Professional IC – AnCat – MSM-HC – MCS ￭ Seal the connector Vacuum tightly with a 6.144.6040 threaded stopper.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.1 Reference conditions 7 Technical specifications 7.1 Reference conditions The technical data listed in this Chapter refers to the following reference conditions: Ambient temperature +25 °C (± 3 °C) Instrument status > 40 minutes in operation (equilibrated) 7.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.5 7 Technical specifications Housing Dimensions Width 365 mm Height 642 mm Depth 380 mm Material of base tray, housing and bottle holder Polyurethane hard foam (PUR) with flame retardation for fire class V0, CFC-free, painted Operating elements Indicators LED for power display On/Off switch On the rear panel of the instrument 7.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.8 Sample degasser Pressure range Pump 0…50.0 MPa (0…500 bar) Pump head 0…35.0 MPa (0…350 bar) (applies for the standard PEEK pump head) Residual pulsation <1% Safety shutdown Function Automatic shutdown upon reaching the pressure limit values Maximum pressure limit ￭ Minimum pressure limit ￭ ￭ ￭ ￭ ￭ Gradient capacity Adjustable from 0.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.10 7 Technical specifications Column thermostat Type Peltier technique thermostat for two intelligent separation columns Adjustable temperature range 0…+ 80 °C, in increments of 0.1 °C Heating Ambient temperature +50 °C Cooling Ambient temperature –20 °C Temperature reproducibility ± 0.2 °C Stability < 0.05 °C Heating up time < 30 minutes from 20 to 50 °C Cooling time < 40 minutes from 50 to 20 °C 7.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.13 Metrohm CO2 suppressor (MCS) 7.13 Metrohm CO2 suppressor (MCS) Material fluoropolymer Resistance to solvents No restriction (apart from PFC) Vacuum Working range Microprocessor-controlled / stabilized Build-up time after start < 30 s Capillary volume 400 µL Recommended flow range 0.1…1.0 mL 7.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Technical specifications Cell temperature 20…50 °C in increments of 5 °C Temperature stability < 0.001 °C Temperature compensation 0…5 %/K adjustable, default 2.3 %/K Heating up time < 30 minutes (40 °C) 7.15 Mains connection Required voltage 100…240 V ± 10 % (auto-sensing) Required frequency 50…60 Hz ± 3 (auto-sensing) Power consumption ￭ Power supply unit ￭ ￭ ￭ 7.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.17 Safety specification 7.17 Safety specification Design / Test ￭ ￭ ￭ ￭ 7.18 Electromagnetic compatibility (EMC) Emission ￭ ￭ ￭ ￭ ￭ Immunity ￭ ￭ ￭ ￭ ￭ ￭ ￭ ￭ ￭ ￭ 7.19 EN/IEC/UL 61010-1 CSA-C22.2 No.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Conformity and warranty 8 Conformity and warranty 8.1 Declaration of Conformity 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 850 Professional IC The 850 Professional IC is an intelligent instrument for ion chromatography analysis.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8.2 Quality Management Principles EN 61010-1 Safety requirements for electrical equipment for measurement, control and laboratory use This instrument meets the requirements of the ETL Listed Mark for the North American market. It conforms to the electrical safety standards UL 61010-1 and CSA-C22.2 No. 61010-1. This product is listed in Intertek’s Directory of Listed Products. Manufacturer Metrohm Ltd., CH-9101 Herisau/Switzerland Metrohm Ltd.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 8 Conformity and warranty Software development Software development occurs in terms of the software life cycle. Tests are performed to detect programming errors and to assess the program’s functionality in a laboratory environment. Components All components used in the Metrohm instruments have to satisfy the quality standards that are defined and implemented for our products. Suppliers of components are audited by Metrohm as the need arises.
8.3 Warranty (guarantee) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Faults arising from circumstances that are not the responsibility of Metrohm, such as improper storage or improper use, etc. are expressly excluded from the warranty.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9 Accessories 9 Accessories Caution Subject to change without notice! 9.1 Scope of delivery 2.850.3040 850 Professional IC – AnCat – MSM-HC – MCS Order no. Description 1 1.850.3040 850 Professional IC AnCat MSM-HC – MCS 1 6.2122.0x0 Mains cable with C13 line socket IEC-60320-C13 Qty. Cable plug according to customer requirements. Switzerland: Type SEV 12 6.2122.020 Germany, …: Type CEE(7), VII 6.2122.040 USA, …: Type NEMA/ASA 6.2122.070 2 6.1602.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9.1 Scope of delivery Qty. 2 Order no. Description 6.1608.020 Glass bottle / 1000 mL / GL 45 Bottle for auxiliary solutions Width (mm): Height (mm): Volume (mL): 2 6.1608.070 Eluent bottle / 2 L / GL 45 Material: Height (mm): Volume (mL): 2 6.1609.000 Clear glass 262 2000 Adsorbing tube, large and bent For filling with adsorber material. Material: Height (mm): Inner diameter (mm): SGJ size: 1 6.1803.020 Glass 129 32 B-14/15 PTFE capillary 0.97 mm i.d.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Qty. 1 9 Accessories Order no. Description 6.1803.040 PTFE capillary 0.5 mm i.d. / 1 m Capillary for sample handling in IC. Material: PTFE Outer diameter (inches): 1/16 Inner diameter (mm): 0.5 Length (m): 1 1 6.1807.010 Y-connector for tubing 6-9 mm i.d. Connector for waste tubing 1 6.1815.010 Spiral band 0.5 m For holding together different cables or tubing. Length (m): 0.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9.1 Scope of delivery Qty. 2 Order no. Description 6.1816.020 Silicone tubing 6 mm i.d., 1 m For waste tubing. Material: Outer diameter (mm): Inner diameter (mm): Length (m): 2 6.1826.320 Silicone rubber 9 6 1 Pump tubing LFL (orange/yellow), 3 stoppers For suppressor solutions, acceptor solution in Inline Dialysis and for Inline Ultrafiltration 2 6.2023.020 Clip for SGJ 14/16 Material: 1 6.2057.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Qty. 1 9 Accessories Order no. Description 6.2151.020 Cable USB A - USB B 1.8 m USB connecting cable Length (m): 1 6.2251.000 1.8 Colored sleeves for capillaries Colored pieces of heat shrink tubing for capillary coding. Three pieces each of five different colors. 1 6.2322.010 PRIMUS multi anion standard solution: Promo 1 6.2322.020 PRIMUS multi cation standard solution: Promo 1 6.2617.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9.1 Scope of delivery Qty. 1 Order no. Description 6.2621.030 Hexagon key 4 mm Length (mm): 1 6.2621.050 73 1/4 in. wrench For 1/4 in. screws. For IC instruments Length (mm): 73 1 6.2621.080 Capillary cutter For plastic capillaries.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Qty. 1 9 Accessories Order no. Description 6.2621.100 Hexagon key 3 mm Hexagon key 3 mm for IC Sample Processors Length (mm): 73 1 6.2626.000 Drain nozzle (ProfIC) Drain nozzle for Professional IC instruments, for mounting on front panel 2 6.2739.000 Wrench For tightening connectors Length (mm): 1 6.2743.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9.1 Scope of delivery Qty. 1 Order no. Description 6.2744.014 Pressure screw 2x With UNF 10/32 connection. For the connection of PEEK capillaries Material: PEEK Length (mm): 26 2 6.2744.020 For IC instruments Material: Length (mm): 1 6.2744.034 Luer/UNF coupling PEEK 19 Coupling nozzle - UNF 10/32, 2 pieces Connection pressure screw and pump tubing. 2 pieces. For IC instruments with peristaltic pumps 3 6.2744.040 2 x UNF 10/32 coupling For connecting 1/16 in.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Qty. 3 9 Accessories Order no. Description 6.2744.070 Pressure screw short Short version. With UNF 10/32 connection. 5 pieces. For the connection of PEEK capillaries Material: PEEK Length (mm): 21 3 6.2744.090 Pressure screw long Long version. With UNF 10/32 connection. 2 pieces. For the connection of PEEK capillaries (MCS and Sample degasser) Material: PEEK 2 6.2744.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9.1 Scope of delivery Qty. 2 Order no. Description 6.2816.020 Syringe 10 mL with Luer connection For various applications in IC and VA Material: PP Length (mm): 102 Volume (mL): 10 1 6.2816.040 Purge tubing With PTFE tubing and Luer connection. For syringes. For aspirating eluents. 2 6.2821.090 Aspiration filter Pore size 20 µm, set of 5 pieces. For 6.1834.000 Aspiration tubing and 6.1821.040 and 6.1821.050 Filter tubes. Material: PE Outer diameter (mm): 9.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Qty. 1 9 Accessories Order no. Description 6.2837.000 CO2 adsorption cartridge Adsorption cartridge for CO2removal of the air aspirated by the MCS. 2 6.2837.010 H2O adsorption cartridge To CO2 Suppressor. Water adsorption cartridge for the aspirated air. 9.2 Optional accessories 2.850.3040 850 Professional IC – AnCat – MSM-HC – MCS Order no. Description 2.850.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 9.2 Optional accessories Order no. Description 6.2617.040 Tool for piston seal, macro For removing and assembling the piston seal for all macro pump heads 6.2741.040 PE/PTFE piston seal, macro For all macro pump heads 6.2824.130 Macro pump head PEEK Macro pump head for intelligente IC instruments, flow range 0.1...20 mL/min, maximum pressure 12.5 MPa. Material: PEEK (metal-free) 6.5333.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Order no. Description 6.6059.222 MagIC Net™ 2.2 Professional CD: 1 Licence 9 Accessories Professional PC program for controlling intelligent Professional IC systems, Compact IC instruments and their peripherals such as different autosamplers, 800 Dosinos dosing systems, 771 Compact Interface, etc. The software permits control, data acquisition, evaluation and monitoring as well as report generation for ion chromatographic analyses.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index Index Numbers/Symbols 6.2821.090 aspiration filter ...... 77 6.2821.130 filter ...................... 88 A Accessories Optional ........................... 131 Adsorption cartridges Connection ........................ 61 Ambient conditions ................ 110 Anion channel .......................... 16 Aspiration filter 6.2821.090 ...... 77 Aspiration tubing for eluent ...... 32 B Baseline Conditioning ...................... 73 Unstable .............................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Protection .................... 26, 77 Technical specifications ..... 111 Tubing connection .............. 37 Valves ................................. 86 Housing ................................. 111 Humidity ................................ 110 I IC column see also "Separation column" ........................................... 69 Immunity ................................ 116 Impurity MSM-HC Organic .............................. 93 Initial installation ......................
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index Separation column ............. 70 Rinsing time ............................. 91 Rise in pressure ......................... 77 Rollers ...................................... 21 S Safety instructions ...................... 4 Safety shutdown .................... 112 Safety specification ................. 116 Sample Carry-over .......................... 90 Sample loop ....................... 48 Transfer time ...................... 90 Sample degasser Installation ..................
