940 Professional IC Vario 940 Professional IC Vario TWO/SeS Manual 8.940.
Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com 940 Professional IC Vario 940 Professional IC Vario TWO/SeS 2.940.2400 Manual 8.940.8027EN 11.
Teachware Metrohm AG CH-9100 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://documents.metrohm.com.
■■■■■■■■■■■■■■■■■■■■■■ Table of contents Table of contents 1 Introduction 1 1.1 Instrument description ......................................................... 1 1.2 Intended use ......................................................................... 3 1.3 Safety instructions ................................................................ 4 1.3.1 General notes on safety ........................................................... 4 1.3.2 Electrical safety .........................................
■■■■■■■■■■■■■■■■■■■■■■ Table of contents 3.13.2 Connecting the suppressor .................................................... 33 3.14 Metrohm CO2 Suppressor (MCS) ....................................... 38 3.14.1 General information on MCS ................................................. 38 3.14.2 Connecting the MCS ............................................................. 39 3.14.3 Installing adsorption cartridges .............................................. 40 3.15 Installing the detector ...
■■■■■■■■■■■■■■■■■■■■■■ Table of contents 5.13.2 Regenerating the H2O adsorption cartridge ............................ 88 5.14 Servicing the detector ........................................................ 89 5.15 Rinsing the sample path .................................................... 89 5.16 Separation column ............................................................. 90 5.16.1 Separating efficiency .............................................................. 90 5.16.
■■■■■■■■■■■■■■■■■■■■■■ 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 VI ■■■■■■■■ Front ................................................................................................. 7 Rear ..................................................................................................
■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction 1 Introduction 1.1 Instrument description The 940 Professional IC Vario is a professional ion chromatograph. It is distinguished by: ■ ■ ■ ■ ■ ■ ■ ■ Its intelligence: All of the functions are monitored, optimized and documented in an FDA-compatible manner. Intelligent components, such as iColumns, save important data onto a chip. Its compact design: It has a small footprint. Its modularity: It provides flexibility for use in various applications.
■■■■■■■■■■■■■■■■■■■■■■ 1.1 Instrument description Column thermostat The column thermostat regulates the temperature for the separation columns and the eluent, thereby providing stable measuring conditions. The interior of the column thermostat can be heated and cooled. There are two column holders with chip readers in the column thermostat. Eluent degasser The eluent degasser removes gas bubbles and dissolved gases from the eluent.
■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction Detector Metrohm offers a series of different detectors for various analysis tasks. A suitable detector type must be ordered as a separate accessory. Sample degasser The sample degasser removes gas bubbles and dissolved gases from the sample. Separation column The intelligent separation column separates different components according to their interactions with the column.
■■■■■■■■■■■■■■■■■■■■■■ 1.3 Safety instructions 1.3 Safety instructions 1.3.1 General notes on safety WARNING This instrument may only be operated in accordance with the specifications in this documentation. This instrument has left the factory in a flawless state in terms of technical safety. To maintain this state and ensure non-hazardous operation of the instrument, the following instructions must be observed carefully. 1.3.
■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction Protection against electrostatic charges WARNING Electronic components are sensitive to electrostatic charges and can be destroyed by discharges. Do not fail to pull the mains cable out of the mains connection socket before you set up or disconnect electrical plug connections at the rear of the instrument. 1.3.3 Tubing and capillary connections CAUTION Leaks in tubing and capillary connections are a safety risk. Tighten all connections well by hand.
■■■■■■■■■■■■■■■■■■■■■■ 1.4 Symbols and conventions More details about the disposal of your old equipment can be obtained from your local authorities, from waste disposal companies or from your local dealer. 1.4 Symbols and conventions The following symbols and formatting may appear in this documentation: Cross-reference to figure legend The first number refers to the figure number, the second to the instrument part in the figure. Instruction step Carry out these steps in the sequence shown.
■■■■■■■■■■■■■■■■■■■■■■ 2 Overview of the instrument 2 Overview of the instrument 2.1 Front Figure 1 Front 1 Bottle holder Offers space for the eluent bottle and additional accessories. 2 Detector chamber Offers space for two embedded detectors and additional accessories. 3 Column holder For a third separation column outside the column thermostat. 4 Metrohm CO2 Suppressor (MCS) 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 2.1 Front 5 Suppressor 6 Column thermostat With two column holders for two separation columns. 7 Inline filter In the anion channel. 8 Sample degasser In the anion channel. Removes air bubbles from the sample. 9 Injection valve In the anion channel. 10 Pulsation absorber In the anion channel. 11 Inline filter In the cation channel. 12 Sample degasser In the cation channel. Removes air bubbles from the sample. 13 Injection valve In the cation channel.
■■■■■■■■■■■■■■■■■■■■■■ 2.2 2 Overview of the instrument Rear Figure 2 Rear 1 Bottle holder Offers space for the eluent bottle and additional accessories. 2 Back panel Removable. Enables access to the detector chamber. 3 Drainage tubing connection For connecting the drainage tubing, which guides escaped liquids away from the detector chamber. 4 Transport locking screws For securing the vacuum pump(s) when transporting the instrument. Up to two vacuum pumps can be installed in an instrument.
■■■■■■■■■■■■■■■■■■■■■■ 2.3 Feed-throughs for capillaries and cables 5 Vacuum connection For connecting an Extension Module that has a degasser but not its own vacuum pump. This connection has to be firmly sealed with a stopper when not in use. 6 Exhaust opening Labeled Exhaust. For extracting the air from the vacuum chamber. 7 PC connection socket For connecting the instrument to the computer with the USB cable (6.2151.020). 8 USB connection sockets Labeled USB 1 and USB 2.
■■■■■■■■■■■■■■■■■■■■■■ 2 Overview of the instrument Openings on the door Figure 3 1 Feed-throughs on the door Luer connector For connecting a capillary from inside and for inserting a syringe (6.2816.020) from outside. For manual sample injection. 2 Opening for capillaries For up to 3 capillaries. An opening for up to 3 capillaries is located on the door of the instrument.
■■■■■■■■■■■■■■■■■■■■■■ 2.3 Feed-throughs for capillaries and cables Openings on the back panel Figure 4 1 Openings for capillaries and cables Openings for capillaries 2 Openings for cables The removable back panel is outfitted with openings through which capillaries and cables can be lead out of the detector chamber. Ducts for capillaries There are ducts for capillaries between the instrument and base tray as well as between the instrument and the bottle holder.
■■■■■■■■■■■■■■■■■■■■■■ Figure 5 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 3.1 Setting up the instrument 3 Installation 3.1 Setting up the instrument 3.1.1 Packaging The instrument is supplied in highly protective special packaging together with the separately packed accessories. Keep this packaging, as only this ensures safe transportation of the instrument. 3.1.2 Checks Immediately after receipt, check whether the shipment has arrived complete and without damage by comparing it with the delivery note. 3.1.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Also see: PEEK pressure screws video on the Internet http://ichelp.metrohm.com/maintenance.php?chapter=1_2. Connection capillaries PEEK capillaries and PTFE capillaries are used in the IC system. PEEK capillaries (polyetheretherketone) PEEK capillaries are temperature-resistant up to 100 °C, stable under pressure up to 400 bar (depending on the inner diameter), flexible, chemically inert and have an extremely smooth surface.
■■■■■■■■■■■■■■■■■■■■■■ 3.2 Capillary connections in the IC system ■ ■ The capillary ends do not have exactly flat edges. The two capillary ends do not completely meet. One prerequisite for dead-volume-free capillary connection is that both capillary ends are cut exactly flat. Therefore we recommend cutting PEEK capillaries only with a capillary cutter (6.2621.080). Also see: Cutting capillaries video on the Internet http://ichelp.metrohm.com/maintenance.php?chapter=1_1.
■■■■■■■■■■■■■■■■■■■■■■ 3.3 3 Installation Removing the handle The instrument is equipped with a handle in order to make it easier to transport. The handle can be removed once the instrument is in place in the lab. Accessories You do not need any accessories for the following work steps. Removing the handle 1 Removing the handle ■ ■ Unscrew the four knurled screws. Remove the handle. 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 3.4 Removing transport locking screws 3.4 Removing transport locking screws To avoid damage to the drives for the high-pressure pump and the vacuum pump during transport, the pumps are secured with transport locking screws. These are located at the rear of the instrument and labeled with Transport security screws. Remove these transport locking screws before the initial start-up. Accessories For this step you need: ■ Hex key 4 mm (6.2621.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Store the transport locking screws in a safe place. Reinsert the transport locking screws each time you transport the instrument a significant distance. CAUTION The pumps may be damaged if you transport the instrument without inserting the transport locking screws. 3.5 Connecting the drainage tubing and leak sensor The leak sensor detects leaking liquid that collects in the instrument's base tray.
■■■■■■■■■■■■■■■■■■■■■■ 3.5 Connecting the drainage tubing and leak sensor Connecting the drainage tubing 1 Cut a piece of silicone tubing into three pieces using scissors: 2 × approx. 40 cm and 1 × 20 cm 2 Attach one end of the 40 cm long piece to the drainage tubing connection on the bottle holder. 3 Attach one end of the 20 cm long piece to the drainage tubing connection on the detector chamber. 4 Attach each of the loose ends of both pieces of silicone tubing to one end of the Y connector.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Route the loose end into a waste container. 3.5.2 Connecting the leak sensor Plugging in the leak sensor connection cable The leak sensor connection cable is coiled up in the base tray. 1 Pull the leak sensor connection cable out of the base tray as far as needed. 2 Plug the plug for the leak sensor connection cable into the leak sensor connection socket (labeled Leak Sensor). 3.
■■■■■■■■■■■■■■■■■■■■■■ 3.7 Connecting the eluent bottle 3.7 Connecting the eluent bottle The eluent is aspirated out of the eluent bottle via the eluent aspiration tubing . The eluent aspiration tubing is installed on the input for the eluent degasser. The tubing has to be be fed out of the instrument through a suitable opening (see "Openings on the back panel", page 12) before the loose end can be connected to the eluent bottle.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation 2 Mounting the tubing adapter and the aspiration filter Install the parts of the tubing adapter for aspiration filter (6.2744.210) accessory set: ■ ■ ■ Start by pushing the tubing weighting onto the loose end of the eluent aspiration tubing. Then push the clamping screw onto the loose end of the eluent aspiration tubing. Lastly, push the filter holder onto the loose end of the eluent aspiration tubing and screw it onto the tubing nipple.
■■■■■■■■■■■■■■■■■■■■■■ 3.7 Connecting the eluent bottle 4 Mounting the adsorber tube NOTE Depending on the eluent used, the adsorber tube (6.1609.000) must be filled differently: ■ ■ ■ ■ 24 ■■■■■■■■ For alkaline eluents or eluents with a low buffer capacity: first a little cotton, then CO2 adsorber material. For all other eluents: only cotton. Remove the plastic cover from the large opening of the adsorber tube. Fill the adsorber tube and close it again using the plastic cover.
■■■■■■■■■■■■■■■■■■■■■■ 3.8 3 Installation Connecting the eluent degasser The high-pressure pump cannot generate uniform flow if the eluent contains small gas bubbles or dissolved gas. As a result, the baseline cannot be stabilized correctly. In order to achieve good measurement results, the eluent has to be degassed before it goes into the high-pressure pump. The eluent degasser is completely connected. No installation work is required. 3.
■■■■■■■■■■■■■■■■■■■■■■ 3.10 Installing an inline filter Figure 9 1 High-pressure pump with purge valve 2 Pump head Purge valve The high-pressure pump is completely connected. No installation work is required. 3.10 Installing an inline filter Inline filters reliably protect the separation column from potential contamination from the eluent. The small filter plates with 2 µm pore size can be replaced quickly and easily. They remove particles from the solutions, such as bacteria and algae.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Figure 10 1 Inline filter 2 Input capillary Connected to the purge valve. Output capillary Connected to the pulsation absorber. The inline filter is completely connected. No installation work is required. 3.11 Installing the pulsation absorber The pulsation absorber is installed between the high-pressure pump and the injection valve.
■■■■■■■■■■■■■■■■■■■■■■ 3.12 Injection valve 3.12 Injection valve The injection valve connects the eluent path to the sample path. By a quick and precise switching of the valve a defined quantity of sample solution is injected and flushed to the separation column with the eluent. The quantity of injected sample solution is determined either by the volume of the sample loop or by an 800 Dosino, if Metrohm's intelligent partial loop injection techniques (MiPT) are being used.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Figure 12 1 Pressure screw Fastened to Port 6. 3 Pressure screw Fastened to Port 3. Exchanging the sample loop 2 Sample loop Exchanging the sample loop 1 Removing the existing sample loop ■ ■ Unscrew the pressure screws (6.2744.010) at Port 3 and Port 6. Remove the sample loop. 2 Installing a new sample loop ■ ■ Fasten one end of the sample loop to Port 3 using a PEEK pressure screw (6.2744.010). Use the second PEEK pressure screw (6.2744.
■■■■■■■■■■■■■■■■■■■■■■ 3.13 Suppressor 3.13 Suppressor The suppressor drive of the 940 Professional IC Vario can hold various rotors. The large rotors such as the SPM Rotor A (6.2835.000) and the MSM-HC Rotor A (6.2842.000) can be inserted directly. Small rotors like the MSM Rotor A (6.2832.000) and the MSM-LC Rotor A (6.2844.000) must first be fitted into the adapter (6.2842.020) which can then be inserted into the suppressor housing. A connecting piece (6.2835.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation CAUTION The rotor may be destroyed during start-up if not inserted correctly. Therefore, follow the following instructions exactly. Inserting large rotors 1 Removing the union nut Loosen the union nut and remove it. 2 Inserting the rotor ■ ■ Clean the sealing surface of the rotor with ethanol using a lintfree cloth.
■■■■■■■■■■■■■■■■■■■■■■ 3.13 Suppressor NOTE The rotor's sealing surface is approximately 4 mm inside the suppressor drive if the rotor is inserted correctly. If this is not the case, then the rotor has to be moved into the correct position from below using a sharp object (e.g. a screwdriver). 3 Inserting the connecting piece ■ ■ Clean the sealing surface of the connecting piece with ethanol using a lint-free cloth.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation ■ Insert the rotor into the adapter so that the tubing connections on the rear of the rotor fit into the corresponding recesses inside the adapter and one of the three holes of the rotor is visible in the slot of the adapter. 2 Inserting the adapter Insert the adapter into the suppressor drive just like a large rotor (see "Inserting large rotors", page 31). 3.13.
■■■■■■■■■■■■■■■■■■■■■■ 3.13 Suppressor Recommended installation Alternative installation Installing bottles with auxiliary solutions Accessories To connect the bottles of the auxiliary solutions, you will need the following accessories: ■ 34 ■■■■■■■■ XML structure missing: ul 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 3.13.2.1 3 Installation Installing the eluent path The eluent path is connected with the capillaries in and out. 1 Connect the capillary labeled with in with the output of the separation column using a short pressure screw (6.2744.070). 2 Use a long pressure screw (6.2744.090) to connect the capillary labeled with out to the input of the MCS (see Chapter 3.14.2, page 39). 3.13.2.
■■■■■■■■■■■■■■■■■■■■■■ 3.13 Suppressor 1 Fasten the capillary labeled regenerant to the outlet of the inline filter (6.2821.120) using a pressure screw (6.2744.070). 2 Use a pressure screw (6.2744.070) to fasten one end of the PEEK capillary (6.1803.030) to the inlet of the inline filter. 3 Use a pressure screw (6.2744.070) and an adapter (6.2744.080) to fasten the other end of the PEEK capillary to Port 1 of the Dosino. 4 Connect the FEP tubing (6.1805.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Connecting the rinsing solution inlet with STREAM 1 Connect the detector output capillary and the capillary labeled rinsing solution to each other using a coupling (6.2744.040) and two pressure screws (6.2744.070). Connecting the rinsing solution inlet to the Dosino The rinsing solution capillary can be connected to the Dosino to which the regenerant capillary is already connected.
■■■■■■■■■■■■■■■■■■■■■■ 3.14 Metrohm CO2 Suppressor (MCS) 4 Connect the FEP tubing (6.1805.120) from the bottle with the rinsing solution with the adapter Dosino Port 4/M6 to the Port 4 of the Dosino. If you would like to use a separate Dosino for the rinsing solution, you will need the following additional accessories: ■ ■ ■ ■ Dosino (2.800.0010) Dosing unit 50 mL (6.3032.250) Accessory kit: Flex/Vario: ChS (6.5000.030) IC equipment: Dosino Regeneration (6.5330.
■■■■■■■■■■■■■■■■■■■■■■ 3.14.2 3 Installation Connecting the MCS The MCS is connected between the suppressor and the detector. Connecting the MCS Figure 14 Connecting the MCS 1 Air aspiration capillary For drawing in air with low CO2 content (via the CO2 adsorption cartridge). 3 Luer coupling (6.2744.120) Mounted on the air aspiration capillary with a pressure screw (6.2744.070). 2 Pressure screw, short (6.2744.070) Installed on the air aspiration capillary.
■■■■■■■■■■■■■■■■■■■■■■ 3.14 Metrohm CO2 Suppressor (MCS) CAUTION If the MCS is not used, the input and output must be sealed with the threaded stoppers (6.2744.220). 3.14.3 Installing adsorption cartridges The suctioned air has to have the lowest CO2 content possible in order for the CO2 to be removed from the eluent as efficiently as possible. In order to achieve this, the air is aspirated through a CO2 adsorption cartridge (6.2837.000).
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation 1 Preparing the adsorption cartridge holder ■ Push the 4 clips into the slots on the adsorption cartridge holder. 2 Connecting adsorption cartridges ■ ■ ■ ■ Attach the PVC tubing to the tip of the H2O adsorption cartridge. Insert the adapter into the other end of the PVC tubing. Insert the adapter into the star-shaped cap of the CO2 adsorption cartridge. Attach the capillary connected to the MCS's Air in connection to the tip of the CO2 adsorption cartridge.
■■■■■■■■■■■■■■■■■■■■■■ 3.15 Installing the detector 3.15 Installing the detector The 940 Professional IC Vario provides enough space for two detectors and additional accessories in the detector chamber. The detectors are available as accessories and are supplied with separate manuals. Placing the detector in the instrument Follow the instructions in the chapter Inserting the detector in the manual for the detector.
■■■■■■■■■■■■■■■■■■■■■■ 3.16 3 Installation Connecting the sample degasser (optional) Gas bubbles in the sample lead to poor reproducibility, as the quantity of sample in the sample loop is not always the same. Therefore, we recommend degassing samples that contain gas before injection. NOTE The sample degasser does not have to be connected. We recommend only using the sample degasser if the application requires it. The rinsing time increases by at least 2 minutes when the sample degasser is connected.
■■■■■■■■■■■■■■■■■■■■■■ 3.16 Connecting the sample degasser (optional) Connecting the sample degasser CAUTION If the sample degasser is not used, the input and output must be sealed with threaded stoppers (6.2744.220). 1 Removing the threaded stoppers Remove and keep the threaded stoppers (6.2744.220) from the input and output of the sample degasser. 2 Connecting the output capillary ■ ■ Push a long pressure screw over the loose end of the capillary connected to port 1 of the injection valve.
■■■■■■■■■■■■■■■■■■■■■■ 3.17 3 Installation Connecting the instrument to a computer NOTE The instrument must be switched off when being connected to a computer. Accessories For this step you need the following accessories: ■ USB connecting cable (6.2151.020) Connecting the USB cable 1 Insert the USB cable into the computer connection socket on the rear of the instrument labeled PC. 2 Insert the other end into a USB port on the computer. 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 3.18 Connecting the instrument to the power supply 3.18 Connecting the instrument to the power supply WARNING The power supply unit must not get wet. Protect it from liquids. The power supply 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).
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation After being switched on, the LED on the front of the instrument flashes. The instrument conducts a system test and establishes a connection to the software. Once the system test is complete and the connection to the software has been established, the LED lights up continuously. 3.19 Initial start-up Even before the guard column and separation column are installed, the entire system has to be completely rinsed with eluent for the first time.
■■■■■■■■■■■■■■■■■■■■■■ 3.19 Initial start-up MagIC Net detects the instrument and all of its modules. 3 Starting equilibration ■ Start the equilibration in MagIC Net: Workplace ▶ Run ▶ Equilibration ▶ Start HW. 4 Deaerating the high-pressure pump ■ ■ ■ ■ ■ ■ ■ ■ ■ Push the end of the purging needle (6.2816.040) over the end of the deaerating capillary on the purge valve. Insert the syringe (6.2816.020) in the Luer connector of the purging needle. Open the purge valve using the rotary knob (approx.
■■■■■■■■■■■■■■■■■■■■■■ 3.20 3 Installation Connecting and rinsing the guard column Guard columns protect the separation column and substantially increase its service life. Guard columns available from Metrohm are either actual guard columns or what are known as guard column cartridges that can be used together with a cartridge holder. The process for installing a guard column cartridge in the associated holder is described in the leaflet for the guard column.
■■■■■■■■■■■■■■■■■■■■■■ 3.20 Connecting and rinsing the guard column ■ Guard column (suitable for the separation column) Connecting the guard column 1 Removing the coupling Remove the coupling installed between the column input capillary and the column output capillary for the initial start-up. 2 Preparing the guard column ■ Remove the stopper and the sealing cap from the guard column.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation ■ ■ ■ 3.21 Start manual control in MagIC Net and select the high-pressure pump: Manual ▶ Manual control ▶ Pump – Flow: in accordance with column leaflet – On Rinse the guard column with eluent for approx. 5 minutes. Use manual control in MagIC Net to stop the high-pressure pump again: Off. Connecting the separation column The intelligent separation column (iColumn) is the heart of the ion chromatographic analysis.
■■■■■■■■■■■■■■■■■■■■■■ 3.21 Connecting the separation column NOTE The separation column may not be connected until after the instrument has already been put into operation once (see Chapter 3.19, page 47). The guard column and separation column have to be replaced by a coupling (6.2744.040) until then. 52 ■■■■■■■■ 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation Connecting the separation column 1 Removing the stoppers CAUTION When inserting the column, ensure that it is inserted correctly based on the marked flow direction. ■ Remove the stoppers from the separation column. 2 Installing the input of the separation column There are 3 possibilities: ■ ■ ■ Attaching the bottom end of the separation column directly to the guard column.
■■■■■■■■■■■■■■■■■■■■■■ 3.22 Conditioning 5 Installing the output of the separation column ■ Fasten the column output capillary to the upper end of the separation column using a PEEK pressure screw (6.2744.070). 6 Inserting the separation column ■ Insert the separation column with chip into the column holder until you hear it snap in place. The separation column is now detected by MagIC Net. 3.
■■■■■■■■■■■■■■■■■■■■■■ 3 Installation ■ Ensure that the eluent aspiration tubing is immersed in the eluent and there is enough eluent in the eluent bottle. 3 Starting equilibration ■ ■ Start the equilibration in MagIC Net: Workplace ▶ Run ▶ Equilibration ▶ Start HW. Visually inspect whether all capillaries and their connections from the high-pressure pump to the detector are leak-tight.
■■■■■■■■■■■■■■■■■■■■■■ 4 Operation The 940 Professional IC Vario – TWO/SeS is operated solely using the MagIC Net software. You can find information on operating the software in the tutorial for MagIC Net or in the online help. 56 ■■■■■■■■ 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance 5 Operation and maintenance 5.1 IC system 5.1.1 Operation CAUTION In order to avoid disruptive temperature influences, the entire system including the eluent bottle must be protected from direct sunlight. 5.1.2 Care The instrument requires appropriate care. Excess contamination of the instrument may result in functional disruptions and a reduction in the lifetime of the sturdy mechanical and electronic components.
■■■■■■■■■■■■■■■■■■■■■■ 5.1 IC system 5.1.4 Shutting down and starting back up If the instrument is not used for a long period, the whole IC system (without separation column) must be rinsed to be free of salts using methanol/ ultrapure water (1:4). This prevents eluent salts from crystallizing and then causing damage. Rinsing the IC system to be free of salts 1 In the software, stop the hardware and wait until the pressure in the high-pressure pump has dissipated.
■■■■■■■■■■■■■■■■■■■■■■ 5.2 5 Operation and maintenance Capillary connections All connections between injection valve, separation column and detector must be as short as possible, have a low dead volume and be completely leak-tight. The PEEK capillary downstream of the detector must be free of blockages. Only use PEEK capillaries with an inner diameter of 0.25 mm in the highpressure section between the high-pressure pump and the detector. 5.
■■■■■■■■■■■■■■■■■■■■■■ 5.4 Column thermostat – Replacing the capillaries 1 3 1 2 2 1 1 1 Figure 15 Column thermostat 1 Recesses For feeding capillaries into and out of the instrument. 3 Column holder With column recognition. For fastening the column. 60 ■■■■■■■■ 2 Preheating grooves For regulating the temperature of the eluent. 940 Professional IC Vario TWO/SeS (2.940.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance Replacing the preheating capillaries In order to make threading the column input capillary into the column thermostat's preheating grooves easier, we recommend loosening the screws for the holder plate a little, but not removing them all the way. 1 Guide the column input capillary into the column thermostat via a suitable recess (15-1). 2 Push the column input capillary into the outermost of the two preheating grooves (15-2) from the bottom.
■■■■■■■■■■■■■■■■■■■■■■ 5.6 Servicing the eluent degasser The composition of the eluent plays a critical role in chromatographic analysis: 5.5.2 Concentration An increase in the concentration generally leads to shorter retention times and faster separation, but also to a higher background conductivity signal. pH pH changes lead to shifts in dissociation equilibria and thus to changes in retention times.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance Connecting the connecting tubing 1 ■ ■ 5.7 Insert the clamping screws on the connector and screw them in by hand. Tighten the clamping screws with the wrench. Notes on operating the high-pressure pump CAUTION The pump head is filled ex works with methanol/ultrapure water. Ensure that the eluent used is miscible with this solvent.
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump 5.8 Servicing the high-pressure pump Figure 16 High-pressure pump – parts 1 Pressure screw, short (6.2744.070) Fastened to the outlet valve holder. 2 Outlet valve holder 3 Fastening screw 4 Pump head 5 Inlet valve holder 6 Pressure screw, short (6.2744.070) Fastened to the inlet valve holder. 7 Eluent aspiration tubing connector Consists of a coupling with a pressure screw. 8 Pressure screw, short (6.2744.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance CAUTION Maintenance work on the high-pressure pump may not be carried out unless the instrument is switched off. Recommended procedure We recommend the following for the maintenance of the pump head: 1. 2. 3. 4. Service the inlet valve and the outlet valve. Remove the pump head. Service both pistons. Reinstall the pump head. You can find brief video sequences on the following maintenance steps on the Internet at http://www.metrohm.
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump Cleaning the outlet valve 1 Removing the outlet valve ■ ■ ■ Unscrew the connection capillary to the auxiliary piston from the outlet valve holder (16-2) (1). Start by loosening the outlet valve holder with the adjustable wrench and then unscrew it by hand (2) and remove it. Remove the outlet valve from the outlet valve holder (3).
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance NOTE The maximum treatment time in an ultrasonic bath is 20 s. Ultrasonic baths that last longer than this can damage the ruby ball inside the valve. The outlet valve has to be replaced if it remains clogged after the ultrasonic bath. 3 Reinserting the outlet valve into the pump head ■ ■ ■ Insert the outlet valve into the outlet valve holder (the seal must be visible) (1).
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump Spare parts If the inlet valve cannot be cleaned, you will need a new inlet valve (6.2824.170) for this step. Cleaning the inlet valve 1 Removing the inlet valve ■ ■ Start by loosening the inlet valve holder with the adjustable wrench (1) and then unscrew it by hand (2) and remove it. Remove the inlet valve from the inlet valve holder (3).
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance NOTE The maximum treatment time in an ultrasonic bath is 20 s. Ultrasonic baths that last longer than this can damage the ruby ball inside the valve. The inlet valve has to be replaced if it remains clogged after the ultrasonic bath. 3 Reinserting the inlet valve into the pump head ■ ■ Insert the inlet valve into the inlet valve holder (the seal must be visible) (1).
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump Has the pressure dissipated? Is the instrument switched off? ■ ■ 1 Release the coupling from the pressure screw and seal it with a stopper. 2 Unscrew and remove the pressure screw on the pump head's output (16-8). 3 Unscrew and remove the four fastening screws (16-3) using the hex key. 4 Remove the pump head (16-4). Replacing the piston seal Carry out the following work on both pistons in turn.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance Figure 17 High-pressure pump – cross-section 1 Outlet valve holder 2 Outlet valve (6.2824.160) 3 Backup ring 4 Piston seal (6.2741.020) 5 Pump head 6 Inlet valve (6.2824.170) 7 Inlet valve holder 8 Zirconium piston (6.2824.070) 9 Piston cartridge Accessories For this step you need the following accessories: You can find these parts in the accessory kit: Vario/Flex Basic (6.5000.000). ■ ■ Adjustable wrench (6.2621.
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump 1 2 Figure 18 1 2 Tip Spare part Tool for piston seal (6.2617.010) Sleeve For this step you need a new piston seal (6.2741.020). Replacing the piston seal Figure 19 1 Piston cartridge Removing the piston cartridge from the pump head 2 Backup ring 1 Removing the piston cartridge Loosen the piston cartridge (17-9) using the adjustable wrench and then unscrew it from the pump head by hand. Place it off to the side.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance 3 Removing the old piston seal CAUTION Screwing the (6.2617.010) special tool for the piston seal into the piston seal destroys this completely! CAUTION Avoid touching the sealing surface in the pump head with the tool! Only screw the tip (18-1) of the tool for piston seal far enough into the piston seal that the seal can be pulled out.
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump Optional: Cleaning/replacing the zirconium oxide piston If the baseline still remains unstable after replacing the valves and piston seal, the zirconium oxide piston in the high-pressure pump may be dirty or scratched. In that case, the zirconium oxide piston must have to be cleaned or replaced.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance Figure 21 Components of the piston cartridge 1 Piston cartridge screw 2 Retaining washer 3 Zirconium oxide piston (6.2824.070) 4 Spring retainer 5 Spring (6.2824.060) 6 Inner plastic sleeve Protects from metallic abrasion.
■■■■■■■■■■■■■■■■■■■■■■ 5.8 Servicing the high-pressure pump You can find these parts in the accessory kit: Vario/Flex Basic (6.5000.000). 4 mm hex key (6.2621.030) ■ Mounting the pump head NOTE To prevent the pump head from being mounted the wrong way, it has fastening bolts with different bore hole depths, i.e. one fastening bolt is longer than all others. The bore hole with the greatest depth must therefore be assigned to the longest bolt.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance Connecting the input for the high-pressure pump 1 ■ ■ 5.9 Remove the stopper from the coupling. Tighten the coupling to the pressure screw located on the pump head input capillary (1). Reconnect the pump head output capillary to the pump head output (2). Servicing the inline filter NOTE You can find a video sequence for this task in the Multimedia Guide IC Maintenance or on the Internet at http://www.metrohm.com/com/ Support/Video/ICGeneral.
■■■■■■■■■■■■■■■■■■■■■■ 5.9 Servicing the inline filter Removing the filter Figure 22 Inline filter – removing the filter 1 Filter housing Inline filter housing. Part of the accessories (6.2821.120). 3 Filter (6.2821.130) Packaging contains 10 pieces. 2 Filter screw Screw for the inline filter. Part of the accessories (6.2821.120). 1 Shutting off the flow Switch off the high-pressure pump in the software. 2 Removing the inline filter Unscrew the both pressure screws from the inline filter.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance Inserting a new filter 1 Inserting a new filter ■ Place the new filter flat in the filter housing (22-1) using tweezers. 2 Mounting the filter screw ■ Screw the filter screw (22-2) back into the filter housing (22-1) and tighten by hand. Then use two adjustable wrenches (6.2621.000) to tighten it slightly. 3 Remounting the inline filter ■ Screw pressure screws back onto the inline filter.
■■■■■■■■■■■■■■■■■■■■■■ 5.10 Servicing the pulsation absorber 5.10 Servicing the pulsation absorber CAUTION The pulsation absorber is maintenance-free and must not be opened. 5.11 Injection valve Maintenance on the injection valve is best performed by specialist personnel from Metrohm during annual service. 5.12 Suppressor 5.12.1 Notes for operating the suppressor NOTE The suppressor units must never be regenerated in the same flow direction the eluent is pumped.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance CAUTION The suppressor has to be regenerated (see Chapter 5.12.3.2, page 82), cleaned (see Chapter 5.12.3.3, page 83) or replaced (see Chapter 5.12.3.4, page 85) if the capacity of the suppressor is reduced or if the backpressure is high. 5.12.2 Taking care of the suppressor housing CAUTION The transparent suppressor housing can become fogged. The suppressor housing is made of PMMA (poly(methyl methacrylate)).
■■■■■■■■■■■■■■■■■■■■■■ 5.12 Suppressor 5.12.3.2 Regenerating the suppression rotor If the suppressor units are loaded with certain heavy metals (such as iron) or organic contamination for long periods, then the standard regeneration solution may no longer be able to completely remove them. This constantly reduces the capacity of the suppressor units, which results in reduced phosphate sensitivity in mild cases and a large increase in the baseline in severe cases.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance ■ ■ In the software, use the Step command to switch to the next suppressor unit and regenerate it as described above. As soon as all three suppressor units have been regenerated, disconnect the capillary labeled regenerant from the coupling. 3 Rinsing the suppressor After regeneration, each of the three suppressor units must be rinsed with degassed ultrapure water for about 15 minutes.
■■■■■■■■■■■■■■■■■■■■■■ 5.12 Suppressor 2 Dismantling the suppressor ■ ■ ■ Unscrew union nut (23-1) from the housing (23-4). Pull the connecting piece (23-2) out of the housing together with the the rotor (23-3). If rotor A gets stuck in the housing, you can knock it loose as follows: Put a pointed object into the slot in the housing and use it to knock rotor A loose. Detach the connecting piece from the rotor.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance ■ ■ Insert the rotor (23-3) into the housing (23-4) in such a way that the tubing connections on the rear of rotor fit into the corresponding recesses inside the housing and one of the three holes of the rotor is visible from below in the slot of the housing (23-5). The rotor's sealing surface is approximately 4 mm inside the housing if the rotor is inserted correctly.
■■■■■■■■■■■■■■■■■■■■■■ 5.12 Suppressor Replacing parts of the suppressor 1 Disconnecting the suppressor from the IC system ■ ■ Switch off the instrument. Disconnect all capillaries of the suppressor from the IC system. 2 Dismantling the suppressor ■ ■ ■ Unscrew union nut (23-1) from the housing (23-4). Pull the connecting piece (23-2) out of the housing together with the the rotor (23-3).
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance ■ The rotor's sealing surface is approximately 4 mm inside the housing if the rotor is inserted correctly. If this is not the case, the rotor must be moved into the right position from below using a sharp object. 5 Cleaning the new connecting piece ■ Clean the surface of the new connecting piece (23-2) with ethanol using a lint-free cloth.
■■■■■■■■■■■■■■■■■■■■■■ 5.13 Servicing the Metrohm CO2 Suppressor (MCS) 5.13 Servicing the Metrohm CO2 Suppressor (MCS) 5.13.1 Replacing the CO2 adsorption cartridge Maintenance interval The CO2 adsorption cartridge (6.2837.000) loses capacity over time. In addition, it can become slightly clogged due to too much liquid. It has to be replaced regularly about every 6 months. Capacity loss The adsorption capacity of the CO2 adsorption cartridge is limited and decreases over time.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance 2 Regenerating the adsorber material Allow the depleted adsorber material to dry overnight in an oven at 140 °C. The dried adsorber material once again has the original color and can be reused. Two H2O adsorption cartridges are provided so that the H2O adsorption cartridge can continue to work without interruption. 5.14 Servicing the detector Follow the maintenance instructions in the the detector's manual. 5.
■■■■■■■■■■■■■■■■■■■■■■ 5.16 Separation column The time upon stopping the watch corresponds to the "transfer time". If the sample is injected automatically, the rinsing time has to be at least three times the transfer time. Checking the rinsing time You can determine if the applied rinsing time is sufficient by measuring the sample carry-over directly. Proceed as follows to do this: 1 Preparing two samples ■ ■ Sample A: A typical sample for the application. Sample B: Ultrapure water.
■■■■■■■■■■■■■■■■■■■■■■ 5 Operation and maintenance representative) or on the Internet at http://www.metrohm.com in the Ion Chromatography product area. You can find information on special IC applications in the corresponding "Application Bulletins" or "Application Notes", which are available on the Internet at http:// www.metrohm.com in the Applications area or free of charge upon request from your responsible Metrohm representative. 5.16.
5.17 Quality Management and qualification with Metrohm 5.17 ■■■■■■■■■■■■■■■■■■■■■■ Quality Management and qualification 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 "Metrohm Quality Management" available from your local Metrohm representative.
■■■■■■■■■■■■■■■■■■■■■■ 6 Troubleshooting 6 Troubleshooting Problem Cause Remedy Marked drop in pressure. Leak in the system. Check all capillary connections and seal leaks, if necessary (see Chapter 3.2, page 14). The baseline has a large amount of noise. The eluent is not sufficiently degassed. Ensure that the connectors for the eluent degasser are firmly connected (see Chapter 5.6, page 62). The eluent path has a leak. Check the eluent path and fix the leak.
■■■■■■■■■■■■■■■■■■■■■■ 6.1 Problem Cause Remedy Note: 6.2821.180 pump tubing connection with filter must be used. Guard column – Blocked. Replace the guard column (see Chapter 3.20, page 49). Separation column – Blocked. ■ ■ Regenerate the separation column (see Chapter 5.16.4, page 91). Replace the separation column (see "Connecting the separation column", page 53). Note: Samples should always be microfiltered . The retention times in the chromatogram have changed unexpectedly.
■■■■■■■■■■■■■■■■■■■■■■ 6 Troubleshooting Problem Cause Remedy Individual peaks are greater than expected. Sample – Sample carryover from the previous measurement. Check the rinsing time (see "Checking the rinsing time", page 90). Suppressor – Insufficient flow of regeneration solution or rinsing solution. There is a leak in the system. Check all connections. Suppressor – Backpressure too high. Clean the suppressor (see Chapter 5.12.3.3, page 83) or replace parts (see Chapter 5.12.3.4, page 85).
■■■■■■■■■■■■■■■■■■■■■■ 6.1 Problem Cause Remedy Extreme spread of the peaks in the chromatogram. Splitting (dual peaks) Capillary connections – dead volume in the system. Check the capillary connections (see Chapter 3.2, page 14) (use PEEK capillaries with an inner diameter of 0.25 mm between the injection valve and detector). Guard column – Diminished efficiency. ■ Replace the guard column (see Chapter 3.20, page 49). Separation column – Dead volume at the column head.
■■■■■■■■■■■■■■■■■■■■■■ 7 Technical specifications 7 Technical specifications 7.1 Reference conditions The technical specifications listed in this chapter refer to the following reference conditions: Ambient temperature +25 °C (± 3 °C) Instrument status Operating > 40 minutes (in equilibrium) 7.
■■■■■■■■■■■■■■■■■■■■■■ 7.4 Housing 7.4 Housing Dimensions Width 365 mm Height 642 mm Depth 380 mm Operating elements Indicators LED standby indicator On/off switch On the rear of the instrument 7.5 Leak sensor Electronic, no calibration necessary Type 7.6 Column thermostat Type Thermostat using Peltier technology for two intelligent separation columns Adjustable temperature range 0 - +80 °C, in 0.
■■■■■■■■■■■■■■■■■■■■■■ 7.7 7 Technical specifications Eluent degasser Material Fluoropolymer Resistance to solvents No restriction (except PFC) Time to establish vacuum < 60 s 7.8 High-pressure pump Type ■ ■ ■ ■ ■ ■ Serial dual-piston pump Intelligent pump head recognition Chemically inert Metal-free pump heads Materials in contact with the eluent: PEEK, ZrO2, PTFE/PE Self-optimizing flow and pressure Flow rate Adjustable flow range 0.001 - 20.
■■■■■■■■■■■■■■■■■■■■■■ 7.9 Injection valve Gradient capability Isocratic or gradient (extendable to quaternary) Profile Step, linear, convex and concave Resolution < 1 nL/min 7.9 Injection valve Actuator switching time typ. 100 ms Maximum operating pressure 35 MPa (350 bar) Material PEEK 7.10 Suppressor Resistance to solvents No restriction Switching time typ. 100 ms 7.
■■■■■■■■■■■■■■■■■■■■■■ 7.12 7 Technical specifications Detector You can find the technical specifications for the detector in the detector's manual. 7.13 Sample degasser Material Fluoropolymer Resistance to solvents No restriction (except PFC) Time to establish vacuum < 60 s 7.14 Power connection Required voltage 100 - 240 V ± 10% (autosensing) Required frequency 50 - 60 Hz ± 3 Hz (autosensing) Power consumption ■ Power supply unit ■ ■ ■ 7.
■■■■■■■■■■■■■■■■■■■■■■ 7.16 Safety specification 7.
■■■■■■■■■■■■■■■■■■■■■■ 8 Warranty (guarantee) 8 Warranty (guarantee) Metrohm guarantees that the deliveries and services it provides are free of defects in materials, design or manufacturing. The general warranty period is 36 months (exclusions below) from the date of delivery, or 18 months in the event of continuous operation. The warranty remains valid on the condition that the servicing is provided by a service organization authorized by Metrohm at defined intervals and with a defined scope.
■■■■■■■■■■■■■■■■■■■■■■ The same warranty periods that are specified for a corresponding new part apply to parts that are replaced or repaired within the above-mentioned warranty periods. However, replacement or repair of a part does not extend the warranty period of the entire system. Deficiencies 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 Up-to-date information on the scope of delivery and optional accessories for your instrument can be found on the Internet. NOTE When you receive your new instrument, we recommend downloading the accessories list from the Internet, printing it out and keeping it together with the manual for reference purposes.
■■■■■■■■■■■■■■■■■■■■■■ The Partslists webpage will be displayed. 7 Select the desired output language. 8 With the article number entered, click on the command Generate PDF. The PDF file with the accessories data will be created in the language selected. Direct access for all instruments If you are unable to find your instrument using the search as described above, this may be due to the instrument not being sold anymore.
■■■■■■■■■■■■■■■■■■■■■■ Index Index A Adsorption cartridges Connection ........................ 40 Ambient conditions .................. 97 Aspiration filter (6.2821.090) .... 61 Aspiration tubing for eluent ...... 22 B Baseline Conditioning ...................... 55 Unstable ............................. 64 C Capillaries Installation ......................... 14 Carry-over ................................ 89 Cartridges Connection ........................ 40 Clean Inlet valve ...........................
■■■■■■■■■■■■■■■■■■■■■■ Index Leak sensor Installation ......................... 21 Interface ........................... 101 Technical specifications ....... 98 Leak-tightness .......................... 48 Leaky piston seals ..................... 64 Loop See also "Sample loop" ....... 28 M Mains voltage ............................. 4 Maintenance High-pressure pump ........... 64 Injection valve .................... 80 Suppressor ......................... 80 Maintenance Agreement ..........