Related Manuals for Metrohm 945 Professional Detector Vario – Conductivity & Amperometry
Summary of Contents for Metrohm 945 Professional Detector Vario – Conductivity & Amperometry
- Page 1 945 Professional Detector Vario 945 Professional Detector Vario – Conductivity & Amperometry Manual 8.945.8003EN / 2014-06-23...
- Page 3 Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com 945 Professional Detector Vario 945 Professional Detector Vario – Conductivity & Amperometry 2.945.0030 Manual 8.945.8003EN / 2014-06-23...
- Page 4 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.
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Page 5: Table Of Contents
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents Table of contents 1 Introduction Instrument description ............1 Intended use ................. 2 Safety instructions ..............2 1.3.1 General notes on safety ............2 1.3.2 Electrical safety ................ 2 1.3.3 Tubing and capillary connections ..........3 1.3.4 Flammable solvents and chemicals ........... - Page 6 5.3.1 Maintenance ................. 32 5.3.2 Preheating capillary maintenance ........... 32 Quality management and qualification with Metrohm . . 33 6 Troubleshooting Problems with the hardware ..........34 Problems with the baseline ..........34 General remarks regarding sensitivity fluctuations ..37 Problems with sensitivity ...........
- Page 7 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents 9 Accessories Index ￭￭￭￭￭￭￭￭ 945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
- Page 8 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures Table of figures Figure 1 Front – Front cover attached ............. 6 Figure 2 Front – Front cover removed ............. 7 Figure 3 Rear ....................8 Figure 4 Connection detector–separation column ......... 17 Figure 5 Connection detector–suppressor ............. 17 Figure 6 Connection detector–MCS ..............
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Page 9: Instrument Description
The 942 Extension Module Vario, 891 Professional Analog Out and 800 Dosinos, Remote Boxes, etc. can all be operated through the 945 Profes- sional Detector Vario – Conductivity & Amperometry. This opens up the flexibility of Metrohm IC systems considerably. The instrument is comprised of the following modules: Conductivity detector... -
Page 10: Intended Use
The electrical safety when working with the instrument is ensured as part of the international standard IEC 61010. WARNING Only personnel qualified by Metrohm are authorized to carry out service work on electronic components. ￭￭￭￭￭￭￭￭ 945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030) -
Page 11: Tubing And Capillary Connections
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction 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. -
Page 12: Flammable Solvents And Chemicals
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1.4 About the documentation 1.3.4 Flammable solvents and chemicals WARNING All relevant safety measures are to be observed when working with flammable solvents and chemicals. Set up the instrument in a well-ventilated location (e.g. fume cup- ￭ board). Keep all sources of flame far from the workplace. ￭... -
Page 13: Symbols And Conventions
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction Additional information on the configuration and operation with MagIC Net can be found in the "MagIC Net Tutorial" or in the MagIC Net online help. 1.4.2 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 sec- ond to the instrument part in the figure. -
Page 14: Overview Of The Instrument
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2.1 Front 2 Overview of the instrument Front Figure 1 Front – Front cover attached Power LED Amperometric detector Amperometric detector standby indicator. Permanently installed. Conductivity detector Power LED Permanently installed. Instrument standby indicator. Front cover Knurled screw For the amperometric detector. For removing the front cover. - Page 15 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument Figure 2 Front – Front cover removed AE connection socket Power LED For connecting the auxiliary electrode. Amperometric detector standby indicator. Cell holder WE connection socket With chip for the automatic detection of the For connecting the working electrode.
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Page 16: Rear
10 MSB connection sockets For connecting the power supply cable Two MSB connection sockets (labeled MSB 1 (6.2122.0x0). and MSB 2) for connecting MSB devices. (MSB = Metrohm Serial Bus) ￭￭￭￭￭￭￭￭ 945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030) -
Page 17: Base Tray And Bottle Holder
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation 3 Installation Base tray and bottle holder 3.1.1 Basic information on base tray and bottle holder The base tray (6.2061.110) and bottle holder (6.2061.100) protect IC instruments from dust, dirt and leaking fluids. The supply bottles for eluent and auxiliary solutions can be positioned neatly on the bottle holder. - Page 18 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.1 Base tray and bottle holder Removing the base tray Before you can remove the base tray, the following preconditions must be met: The instrument is switched off. ￭ The bottle holder is cleared. ￭ All of the cable connections on the rear have been disconnected. ￭...
- Page 19 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation The instrument is lying on its side, and the bottom surface is visible. ￭ To mount the base tray, you need a 3 mm hex key (6.2621.100). 1 Place the base tray in such a way that the openings in the base tray match exactly the screw threads in the bottom of the instrument.
- Page 20 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.1 Base tray and bottle holder 1 Remove the two covering stoppers. 2 Loosen the two cylinder screws with the 3 mm hex key and remove them. 3 Remove the bottle holder. Stack other instruments in the required order. Mount the bottle holder (6.2061.100) onto the topmost instrument on the stack.
- Page 21 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Mounting the bottle holder Before you can mount the bottle holder, the following preconditions must be met: The instrument is switched off. ￭ To mount the bottle holder, you need a 3 mm hex key (6.2621.100). 1 Place the bottle holder onto the topmost instrument in such a way that the openings in the bottle holder exactly match the screw threads on the top surface of the instrument.
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Page 22: Connecting The Instrument To A Computer
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.2 Connecting the instrument to a computer A longer section of silicone tubing (6.1816.020) may have to be cut to size and mounted (see also the manual for the IC instrument). 5 If one of the instruments in the stack is equipped with a leak sensor connection socket, connect the leak sensor (see manual of the IC instrument). -
Page 23: Conductivity Detector
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation For Germany, …: Power supply cable with IEC 60320 line socket, type ￭ C13, with CEE 7 plug, type VII (6.2122.040), 1.5 m For the USA, …: Power supply cable with IEC 60320 line socket, type ￭ C13, with NEMA 5-15 plug, type 498 (6.2122.070), 1.5 m Connecting the power supply cable 1 Inserting the power supply cable... - Page 24 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.4 Conductivity detector NOTE The detector outlet capillary must be free of blockages in order to generate sufficient backpressure (the measuring cell is tested to 5 MPa = 50 bar backpressure). Connecting the detector inlet capillary The detector inlet capillary is connected differently depending on the equipment of the IC instruments: For instruments without suppression, directly to the separation column ￭...
- Page 25 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation Figure 4 Connection detector–separation column Detector inlet capillary PEEK pressure screw, short (6.2744.070) Separation column Connecting the detector inlet capillary to the suppressor 1 Connecting the detector inlet Connect the detector inlet capillary (5-1) and the capillary of the ￭...
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Page 26: Amperometric Detector
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3.5 Amperometric detector Figure 6 Connection detector–MCS Detector inlet capillary PEEK pressure screw, long (6.2744.090) MCS outlet Amperometric detector The following tasks are part of the installation of the amperometric detec- tor: Inserting the working electrode and the reference electrode into the ￭... -
Page 27: Instrument Test With Dummy Cell
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up 4 Start-up The 945 Professional Detector Vario – Conductivity & Amperometry is put into operation together with the IC system. Additional information can be found in the Start-up chapter in the manual for the IC instrument. The following tests and installation tasks must be performed during the first start-up of the IC instrument with the 945 Professional Detector Vario –... - Page 28 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.1 Instrument test with dummy cell 2 Connecting the electrode connection cables to the detector (unless they are already connected) Plug the straight plug of the working electrode connection cable ￭ (red sleeve) into the WE socket of the detector. Plug the straight plug of the reference electrode connection cable ￭...
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Page 29: Testing The Leak Sensor
1 Hold a cloth moistened with eluent or tap water on the two contacts of the leak sensor . The leak sensor of the detector responds. If the leak sensor does not respond, please request Metrohm Service. ￭￭￭￭￭￭￭￭ 945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030) -
Page 30: Testing The Preheating Capillary
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.3 Testing the preheating capillary Testing the preheating capillary The amperometric detector is equipped with a preheating capillary in its interior to ensure that the eluent flows through the measuring cell at a constant temperature. The preheating capillary need not, however, always be connected. -
Page 31: Testing The Detector Outlet Capillary
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up A constant pressure should establish itself after a while. Testing the detector outlet capillary The detector outlet capillary must be of a certain length in order to be able to generate sufficient backpressure. The required length is dependent on the flow that has been set. -
Page 32: Testing The Measuring Cell
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.5 Testing the measuring cell 4 Loosening the detector outlet capillary Loosen the detector outlet capillary from the Eluent to cell connec- tor. Wipe up emerging liquid with a cloth. 5 Observe the pump pressure Observe the pump pressure display in the program part Manual of MagIC Net. - Page 33 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up Connecting the measuring cell outlet: ￭ Use a pressure screw (6.2744.014) to fasten the tested detector outlet capillary to the Out connector on the measuring cell (see "Testing the detector outlet capillary", page 23). 2 Inserting the measuring cell Insert the chip of the measuring cell into the cell holder so that you can hear it locking in.
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Page 34: Deaerating The Measuring Cell
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.6 Deaerating the measuring cell Watch the detector outlet capillary: Liquid must emerge from the ￭ end of the detector outlet capillary. If no liquid emerges from the end of the detector outlet capillary: – Detach the capillary from the Out connection on the mea- suring cell and check whether the end has been pinched by the pressure screw. -
Page 35: Connecting The Electrode Cables
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up Lift out the reference electrode. ￭ Wait until the reference electrode chamber has filled with eluent. ￭ Reinsert the reference electrode. Wipe up any emerging eluent ￭ with a cloth. Screw the nut on the reference electrode connector back on ￭... - Page 36 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4.7 Connecting the electrode cables Connecting the electrode cables to the detector Prerequisites: The measuring cell is switched off. ￭ 1 Plug the straight plug of the working electrode cable (red sleeve) into the WE socket of the detector. 2 Plug the straight plug of the reference electrode cable (black sleeve) into the RE socket of the detector.
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Page 37: Attaching The
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Start-up Attaching the front cover In order to obtain good measuring results, we recommend that the front cover be put back in place. When you are attaching the front cover, observe the following: Do not pinch any capillaries! ￭... -
Page 38: Operation And Maintenance
Metrohm. A shorter maintenance interval is recommended if you frequently work with caustic and corrosive chemicals. Metrohm Service provides professional technical consultation at all times for the maintenance and servicing of all Metrohm instruments. 5.1.3... -
Page 39: Shutting Down
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation and maintenance 5.1.4 Shutting down If the instrument is shut down for a longer period of time, the entire IC system must be rinsed as follows to rid it of salts in order to prevent elu- ent salts from forming crystals which may cause subsequent damage. Rinse all capillaries and the Dosino (if present) with methanol/ultrapure ￭... -
Page 40: Amperometric Detector
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5.3 Amperometric detector 3 In MagIC Net, set the maximum pressure of the high-pressure pump to 5 MPa. 4 Rinse the detector thoroughly with eluent. Amperometric detector 5.3.1 Maintenance WARNING When rinsing the detector without column, the pressure must not exceed 5 MPa. -
Page 41: Quality Management And Qualification With Metrohm
(see "Rinsing the preheating capillary", page 32). If the blockage can also not be dissolved by rinsing in the opposite direc- tion, then the preheating capillary must be replaced by a Metrohm Service employee. Quality management and qualification with... -
Page 42: Troubleshooting
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.1 Problems with the hardware 6 Troubleshooting Problems with the hardware Problem Cause Remedy Leak sensor Leaking capillary connec- Find any leaking capillary connections and seal responds. tion. them. Measuring cell leaking. Screw apart the measuring cell and then reas- semble it. - Page 43 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting Problem Cause Remedy Measuring cell – Working Clean the working electrode (see the leaflet for electrode contaminated. the working electrode). Measuring cell – Measur- Check the capillary connections on the mea- ing cell leaking. suring cell. IC system – Eluent contam- Prepare a new eluent.
- Page 44 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.2 Problems with the baseline Problem Cause Remedy Replace the GC working electrode if it has ￭ been used with oxidative potentials at the upper limit and polishing no longer helps. Air bubble in the measur- Deaerate the measuring cell (see Chapter 4.6, ing cell.
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Page 45: General Remarks Regarding Sensitivity Fluctuations
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting General remarks regarding sensitivity fluctuations Sensitivity fluctuations of up to 20% per week are normal for an unchanged system in constant operation. The sensitivity can increase to approximately twice as much for a short time when new working electrodes are inserted or when the conditions change. -
Page 46: Problems With The Pressure
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.5 Problems with the pressure Problems with the pressure Problem Cause Remedy Marked drop in IC system – Leak in the sys- Check the capillary connections and seal them. pressure. tem. The pressure in the IC system – Inline filter Replace the filter pad (see Chapter Operation system markedly blocked. -
Page 47: Problems With The Chromatogram
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting Problem Cause Remedy No measuring sig- IC system – No power sup- Check the power connection and the supply nal. ply. voltage. Peaks cut off at the Measuring range too Set a less sensitive measuring range. ￭ top. -
Page 48: Other Problems
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6.8 Other problems Problem Cause Remedy Extreme spread of IC system – Dead volume Replace the separation column. the peaks in the at the ends of the separa- chromatogram. tion column. Splitting (dual IC system – Dead volume Check the capillary connections. peaks) in the IC system. -
Page 49: Systematic Error Diagnostics
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 6 Troubleshooting Systematic error diagnostics If the causes of a malfunction cannot be found among the problem descriptions in the above chapters, then proceed systematically as follows: Systematic error diagnostics 1 Restarting the instrument and the software Switch off the instrument. ￭... - Page 50 If the problem has not yet been localized, continue with Step 8. 8 Requesting Metrohm Service If none of these measures help, please request Metrohm Service. NOTE Please note that, when the electrodes are replaced, the system requires a longer run-in time before the earlier values can be reproduced.
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Page 51: Technical Specifications
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Technical specifications 7 Technical specifications Reference conditions The technical specifications listed in this chapter refer to the following ref- erence conditions: Ambient tempera- +25 °C (± 3 °C) ture Instrument status Operating > 40 minutes (in equilibrium) Power connection Required voltage 100 - 240 V ±... -
Page 52: Amperometric Detector
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.4 Amperometric detector Cell constant Individual calibration data saved in the detector ￭ Adjustable in the range: 13.0 - 21.0 /cm ￭ Electrodes Ring-shaped electrodes made from stainless steel Materials in Chemically inert PCTFE contact with eluent Maximum oper- 5.0 MPa (50 bar) ating pressure Cell tempera-... -
Page 53: Leak Sensor
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Technical specifications Filter DC mode Hardware filter, can be selected by the user All modes Software filter, can be set by the user Temperature con- trol Temperature better than 0.05 °C with ambient temperature +8 °C…80 °C stability at the heater Operation Direct... -
Page 54: Housing
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7.7 Housing Housing Dimensions Width 365 mm Height 131 mm Depth 380 mm Material of hous- Polyurethane hard foam (PUR) with flame retardation for fire class UL94V0, CFC-free, coated Controls Indicators LED for standby operation On/off switch On the rear of the instrument Interfaces Input 1 USB upstream, type B (for connection to the PC) -
Page 55: Electromagnetic Compatibility (Emc)
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 7 Technical specifications Safety instructions This document contains safety instructions which have to be followed by the user in order to ensure safe operation of the instrument. 7.10 Electromagnetic compatibility (EMC) Requirements Standards ful- EN/IEC 61326-1 ￭ filled Emission Standards ful- EN/IEC 61000-6-3 ￭... -
Page 56: 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... - Page 57 This does not apply for software products sold under the Metrohm NIRSystems brand. If Metrohm AG is unable to meet this obligation due to circumstances beyond the control of Metrohm AG, then the ordering party shall be offered alternative solutions at preferential conditions.
- Page 58 The search results will be displayed. 4 In the search results, select the Devices tab (if it is not already selected) and then click on the Metrohm article number of the required instrument (e.g. 2.852.0050). The page with information pertaining to the searched article is dis- played.
- Page 59 Downloading the accessories list 1 Type http://partslists.metrohm.com into your Internet browser. The Partslists webpage will be displayed. 2 Select the desired output language. 3 Enter the article number and click on the Generate PDF command.
- Page 60 ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Index Index Power supply unit ..... 43 Ambient conditions ....45 Frequency ........ 43 Amperometric detector Installation ......18 Quality management ....33 Guarantee ........ 48 Maintenance ...... 32 Start-up ......18 Reference conditions ....43 Technical specifications ..44 Humidity ........