Metrohm 945 Professional Detector Vario – Conductivity & Amperometry User Manual

945 Professional Detector Vario
945 Professional Detector Vario – Conductivity & Amperometry
Manual
8.945.8003EN / 2014-06-23
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
8.945.8003EN / 2014-06-23
Manual
zst
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.
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Table of contents

1 Introduction 1
1.1 Instrument description ......................................................... 1
1.2 Intended use ......................................................................... 2
1.3 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 ........................................... 4
1.3.5 Recycling and disposal ............................................................. 4
1.4 About the documentation ................................................... 4
1.4.1 Content and scope .................................................................. 4
1.4.2 Symbols and conventions ........................................................ 5
2 Overview of the instrument 6
Table of contents
2.1 Front ...................................................................................... 6
2.2 Rear ........................................................................................ 8
3 Installation 9
3.1 Base tray and bottle holder ................................................. 9
3.1.1 Basic information on base tray and bottle holder ..................... 9
3.1.2 Mounting base tray and bottle holder (optional) ...................... 9
3.2 Connecting the instrument to a computer ....................... 14
3.3 Connecting the instrument to the power supply ............. 14
3.4 Conductivity detector ......................................................... 15
3.4.1 Connecting the detector capillaries ........................................ 15
3.5 Amperometric detector ...................................................... 18
4 Start-up 19
4.1 Instrument test with dummy cell ...................................... 19
4.2 Testing the leak sensor ...................................................... 21
4.3 Testing the preheating capillary ....................................... 22
4.4 Testing the detector outlet capillary ................................ 23
4.5 Testing the measuring cell ................................................. 24
4.6 Deaerating the measuring cell .......................................... 26
4.7 Connecting the electrode cables ....................................... 27
4.8 Attaching the front cover .................................................. 29
945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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Table of contents
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5 Operation and maintenance 30
5.1 General notes ...................................................................... 30
5.1.1 Care ...................................................................................... 30
5.1.2 Maintenance by Metrohm Service .......................................... 30
5.1.3 Operation .............................................................................. 30
5.1.4 Shutting down ...................................................................... 31
5.2 Conductivity detector ......................................................... 31
5.2.1 Maintenance ......................................................................... 31
5.2.2 Remedying blockage ............................................................. 31
5.3 Amperometric detector ...................................................... 32
5.3.1 Maintenance ......................................................................... 32
5.3.2 Preheating capillary maintenance ........................................... 32
5.4 Quality management and qualification with Metrohm .. 33
6 Troubleshooting 34
6.1 Problems with the hardware ............................................. 34
6.2 Problems with the baseline ............................................... 34
6.3 General remarks regarding sensitivity fluctuations ......... 37
6.4 Problems with sensitivity ................................................... 37
6.5 Problems with the pressure ............................................... 38
6.6 Problems with the measuring signal ................................ 38
6.7 Problems with the chromatogram .................................... 39
6.8 Other problems ................................................................... 40
6.9 Systematic error diagnostics ............................................. 41
7 Technical specifications 43
7.1 Reference conditions .......................................................... 43
7.2 Power connection ............................................................... 43
7.3 Conductivity detector ......................................................... 43
7.4 Amperometric detector ...................................................... 44
7.5 Leak sensor ......................................................................... 45
7.6 Ambient conditions ............................................................ 45
7.7 Housing ............................................................................... 46
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7.8 Interfaces ............................................................................. 46
7.9 Safety specifications ........................................................... 46
7.10 Electromagnetic compatibility (EMC) ................................ 47
8 Warranty (guarantee) 48
945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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9 Accessories 50
Index 52
Table of contents
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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 .............................................................. 18
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945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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1 Introduction

1.1 Instrument description

The 945 Professional Detector Vario – Conductivity & Amperome­try is an intelligent stand-alone detector equipped with a high-perfor-
mance conductivity detector and an amperometric detector.
As a stand-alone detector, it can be combined with instruments such as those of the 940 Professional IC Vario family for which all available detec­tor connectors have already been assigned to conductivity detectors (AnCat systems or other multi-channel systems) and be used for the deter­mination of electroactive substances in the mobile phase.
The 945 Professional Detector Vario – Conductivity & Amperometry ena­bles multiple detector installations also with the instruments of the 930 Compact IC Flex family and with the 883 Basic IC plus, which are equipped with only one detector connector, which is normally occupied by a conductivity detector. This makes it possible to run applications that require both conductivity detection and amperometric detection.

1 Introduction

The 945 Professional Detector Vario – Conductivity & Amperometry is a stand-alone detector that combines the advantages of the IC Conductivity Detector and the IC Amperometric Detector with the combination possi­bilities provided by 940 Professional IC Vario instruments. It is directly con­trolled by the MagIC Net software.
The 942 Extension Module Vario, 891 Professional Analog Out and 800 Dosinos, Remote Boxes, etc. can all be operated through the 945 Profes­sional Detector Vario – Conductivity & Amperometry. This opens up the flexibility of Metrohm IC systems considerably.
The instrument is comprised of the following modules:
Conductivity detector
The conductivity detector continuously measures the conductivity of the liquid passing through and outputs the measured values in digital form (DSP – Digital Signal Processing). The conductivity detector exhibits out­standing thermal stability and thus guarantees reproducible measuring conditions.
Amperometric detector
With the 945 Professional Detector Vario – Conductivity & Amperometry, electroactive substances can be determined in the mobile phase of an IC system. Determination makes use of amperometric methods, which com­bine outstanding sensitivity with a high degree of selectivity. The installed
945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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1.2 Intended use

potentiostat generates the voltages for the direct current amperometry (DC), for the pulse amperometry (PAD) and the flexible integrated pulse amperometry (flexIPAD) as well as for the recording of cyclovoltammo­grams. The installed preheating capillary ensures a constant eluent tem­perature on the cell.
1.2 Intended use
The 945 Professional Detector Vario – Conductivity & Amperometry is used as an independent detector in an IC system. With its two different detector types, it is used on the one hand for the precise measurement of conductivity during ion chromatography determination of anions and cati­ons and on the other hand for the determination of electroactive substan­ces in the mobile phase of an IC or general liquid chromatography system.
The present instrument is used for working with chemicals and flammable samples. Usage of the 945 Professional Detector Vario – Conductivity & Amperometry therefore requires the user to have basic knowledge and experience in handling toxic and caustic substances. Knowledge with respect to the application of the fire prevention measures prescribed for laboratories is also mandatory.
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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.

1.3.2 Electrical safety

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.
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945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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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.
Mains voltage
WARNING
An incorrect mains voltage can damage the instrument.
Only operate this instrument with a mains voltage specified for it (see rear panel of the instrument).
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. 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.
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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. Clean up spilled liquids and solids immediately. Follow the safety instructions of the chemical manufacturer.

1.3.5 Recycling and disposal

This product is covered by European Directive 2002/96/EC, WEEE – Waste from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative effects on the environment and public health.
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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 About the documentation
CAUTION
Please read through this documentation carefully before putting the instrument into operation. The documentation contains information and warnings which the user must follow in order to ensure safe opera­tion of the instrument.

1.4.1 Content and scope

This document describes the 945 Professional Detector Vario – Con­ductivity & Amperometry, its assembly and connection to the IC instru-
ment, as well as the installation, operation and maintenance of the indi­vidual components. Technical specifications, troubleshooting and informa­tion concerning scope of delivery and optional accessories make up the rest of the manual.
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You will find additional information on the installation and maintenance of the IC instrument and the Sample Processor in the respective manuals.
945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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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:
Method Dialog text, parameter in the software
File New Menu or menu item
[Next] Button or key
1 Introduction
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.
WARNING
This symbol draws attention to a possible life-threat­ening 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.
CAUTION
This symbol draws attention to possible damage to instruments or instrument parts.
NOTE
This symbol highlights additional information and tips.
945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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2.1 Front

2
3
1
4 5
6
7
8

2 Overview of the instrument

2.1 Front
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Figure 1 Front – Front cover attached
Power LED
1
Amperometric detector standby indicator.
Conductivity detector
3
Permanently installed.
Front cover
5
For the amperometric detector.
Coupling
7
For connecting the detector outlet capillary of the conductivity detector. Labeled Cond. Eluent out.
Amperometric detector
2
Permanently installed.
Power LED
4
Instrument standby indicator.
Knurled screw
6
For removing the front cover.
Detector inlet capillary
8
Of the conductivity detector. Permanently mounted.
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945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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1
2
3
4
5
6
7
8 109
2 Overview of the instrument
Figure 2 Front – Front cover removed
AE connection socket
1
For connecting the auxiliary electrode.
Cell holder
3
With chip for the automatic detection of the measuring cell.
RE connection socket
5
For connecting the reference electrode.
Tray
7
Thread
9
For the knurled screw used for fastening the front cover.
Power LED
2
Amperometric detector standby indicator.
WE connection socket
4
For connecting the working electrode.
Coupling
6
For connecting a connection capillary to the measuring cell. Labeled Eluent to cell.
Drain nozzle
8
For draining liquid from the tray. Plugged with a stopper.
Coupling
10
For connecting the detector inlet capillary. Labeled Eluent in.
945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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2.2 Rear

1
2
3
4
5
6
7
8 9
10
2.2 Rear
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Figure 3 Rear
Cable feed-through
1
Output for the detector cable.
PC connection socket
3
For connecting the instrument to the com­puter with the USB cable (6.2151.020).
Extension Module connection socket
5
For connecting a 942 Extension Module Vario or an 891 Professional Analog Out. Labeled Extension Module.
Leak sensor connection socket
7
For connecting the leak sensor connection cable, labeled Leak Sensor.
Power socket
9
For connecting the power supply cable (6.2122.0x0).
Cable feed-through
2
Output for the detector cable.
USB connection sockets
4
Two USB connection sockets, labeled USB 1 and USB 2.
Detector connection sockets
6
For the connection of the installed detector, labeled Detector 1 and Detector 2. The detector connection sockets which are not used must be covered with a lid.
Power switch
8
For switching the instrument on and off.
MSB connection sockets
10
Two MSB connection sockets (labeled MSB 1 and MSB 2) for connecting MSB devices.
(MSB = Metrohm Serial Bus)
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3 Installation

3.1 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.
In a complex IC system, several different instruments may be used, such as an analyzer, an extension module and a detector. These instruments can be set up in one or more stacks. We recommend that a base tray and bot­tle holder be mounted for each stack of IC instruments.
The bottle holder and base tray must be removed or set up every time one of the following instruments is to be mounted on or under a 940 Profes­sional IC Vario:

3 Installation

One or more 942 Extension Module Vario. One 944 Professional UV/VIS Detector Vario. One 945 Professional Detector Vario. Or another instrument with the same-sized footprint.

3.1.2 Mounting base tray and bottle holder (optional)

The base tray and bottle holder come fully assembled on a new ion chro­matograph. If you wished to install an extension module on the ion chro­matograph, you would have to remove the bottle holder and put it back on top of the topmost instrument. If you wished to install an extension module below the ion chromatograph, you would have to remove the base tray and set it under the lowest instrument.
3.1.2.1
Removing/mounting the base tray
The base tray must be removed if you want to install another instrument under the IC instrument.
CAUTION
Do not allow capillaries or leak sensor cables to be pinched!
Pinches in the leak sensor cable or the capillaries fed through the guide ducts between the base tray and the instrument may lead to malfunc­tions.
Unplug the leak sensor cable. Remove all of the capillaries from the capillary ducts.
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3.1 Base tray and bottle holder
1
2
3
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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. The capillaries are removed from the guide ducts between the instru-
ment and the base tray.
There are no loose parts in the instrument.
To remove the base tray, you need a 3 mm hex key (6.2621.100).
Tilt the instrument sideways and lay it down flat.
1
Loosen the four cylinder screws with the 3 mm hex key and remove
2
them and their washers.
Remove the base tray.
3
The base tray must always be mounted under the lowermost instrument of the stack.
Mounting the base tray
Before you can mount 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. There are no loose parts in the instrument.
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945 Professional Detector Vario – Conductivity & Amperometry (2.945.0030)
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