Metrohm 896 User Manual

IC Professional Detector
896 Professional Detector – Conductivity & Amperometry
Manual
8.896.8006EN
Metrohm AG CH-9100 Herisau Switzerland Phone +41 71 353 85 85 Fax +41 71 353 89 01 info@metrohm.com www.metrohm.com
IC Professional Detector
896 Professional Detector – Conduc-
tivity & Amperometry
2.896.0030
8.896.8006EN
Manual
10.2012 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 Setting up the instrument .................................................... 9
3.1.1 Packaging ................................................................................ 9
3.1.2 Checks .................................................................................... 9
3.1.3 Location .................................................................................. 9
3.1.4 Proposed setup ........................................................................ 9
3.2 Mounting base tray and bottle holder (optional) ............ 10
3.2.1 Removing / mounting the base tray ....................................... 10
3.2.2 Removing / mounting the bottle holder ................................. 12
3.3 Conductivity detector ......................................................... 15
3.3.1 Connect the detector capillaries ............................................. 15
3.4 Amperometric detector ...................................................... 18
3.5 Connecting the instrument ................................................ 18
3.5.1 Connecting the instrument to the PC ..................................... 18
3.5.2 Connecting the instrument to power supply .......................... 18
4 Start-up 20
4.1 Instrument test with dummy cell ...................................... 20
4.2 Testing the leak sensor ...................................................... 22
4.3 Testing the preheating capillary ....................................... 22
4.4 Testing the detector output capillary ............................... 23
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Table of contents
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4.5 Testing the measuring cell ................................................. 25
4.6 Deaerating the measuring cell .......................................... 27
4.7 Connecting the electrode connection cables ................... 28
4.8 Attaching the front lid ....................................................... 30
5 Operation and maintenance 31
5.1 General notes ...................................................................... 31
5.1.1 Care ...................................................................................... 31
5.1.2 Maintenance by Metrohm Service .......................................... 31
5.1.3 Operation .............................................................................. 31
5.1.4 Shutting down ...................................................................... 32
5.2 Conductivity detector ......................................................... 32
5.2.1 Maintenance ......................................................................... 32
5.2.2 Remedying blockage ............................................................. 32
5.3 Amperometric detector ...................................................... 33
5.3.1 Maintenance ......................................................................... 33
5.3.2 Preheating capillary maintenance ........................................... 33
5.4 Quality Management and validation with Metrohm ....... 34
6 Troubleshooting 35
6.1 Problems with the hardware ............................................. 35
6.2 Problems with the baseline ............................................... 35
6.3 General remarks regarding sensitivity fluctuations ......... 38
6.4 Problems with sensitivity ................................................... 38
6.5 Problems with the pressure ............................................... 39
6.6 Problems with the measuring signal ................................ 39
6.7 Problems with the chromatogram .................................... 40
6.8 Other problems ................................................................... 41
6.9 Systematic error diagnostics ............................................. 42
7 Technical specifications 44
7.1 Reference conditions .......................................................... 44
7.2 Conductivity detector ......................................................... 44
7.3 Amperometric detector ...................................................... 45
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7.4 Power connection ............................................................... 46
7.5 Leak sensor ......................................................................... 46
7.6 Ambient conditions ............................................................ 46
7.7 Housing ............................................................................... 47
7.8 Interfaces ............................................................................. 47
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8 Warranty (Guarantee) 49
9 Accessories 51
Index 59
Table of contents
7.9 Safety specifications ........................................................... 47
7.10 Electromagnetic compatibility (EMC) ................................ 48
9.1 Scope of delivery ................................................................ 51
9.2 Optional accessories ........................................................... 54
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Table of figures

Table of figures
Figure 1 Front – Front lid attached .................................................................. 6
Figure 2 Front – Front lid removed .................................................................. 7
Figure 3 Rear .................................................................................................. 8
Figure 4 Connection detector – separation column ....................................... 16
Figure 5 Connection detector – suppressor ................................................... 17
Figure 6 Connection detector – MCS ............................................................ 17
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1 Introduction

1.1 Instrument description

The 896 Professional Detector – Conductivity & Amperometry is an intelligent Stand-Alone Detector equipped with a high-performance conductivity detector and an amperometric detector.
As a stand-alone detector, it can for example be combined with instru­ments of the 850 Professional IC 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.
Multiple detector installations can be implemented with the 896 Professio­nal Detector – Conductivity & Amperometry, even with the instruments of the Compact IC family (881 and 882) and with the 883 Basic IC plus, which possess only one detector connector which would normally be occupied by a conductivity detector. Applications can thus be carried out that require not only conductivity detection but also amperometric detec­tion.

1 Introduction

The 896 Professional Detector – Conductivity & Amperometry is a stand­alone detector that combines the advantages of the IC Conductivity Detector and the IC Amperometric Detector with the combination oppor­tunities of the 850 Professional IC instruments. It is directly controlled by the MagIC Net™ software.
872 Extension Modules, 891 Analog Out and 800 Dosinos, Remote Boxes, etc. can all be operated through the 896 Professional Detector – 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 indicates 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 896 Professional Detector – Conductivity & Amperometry, elec­troactive substances can be determined in the mobile phase of an IC sys­tem. Amperometric methods are used for the determination, which com-
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1.2 Intended use

bine an outstanding sensitivity with a high degree of selectivity. The instal­led 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 896 Professional Detector – 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 896 Professional Detector – Conductivity & Amper­ometry therefore requires the user to have basic knowledge and experi­ence in the handling of 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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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 896 Professional Detector – Conductiv­ity & Amperometry, its assembly and connection to the IC instrument,
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.
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Additional information for configuration and operation with MagIC Net™ can be found in the "Tutorial for MagIC Net™" 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 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 a possible damage of instruments or instrument parts.
Note
This symbol marks additional information and tips.
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2.1 Front

2
3
1
4 5
6
7
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2 Overview of the instrument

2.1 Front
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Figure 1 Front – Front lid attached
Power LED
1
Amperometric detector standby indicator.
Conductivity detector
3
Permanently installed.
Front lid
5
For the amperometric detector.
Coupling
7
Connector for the eluent output capillary of the conductivity detector. Labeled with
Cond. Eluent out.
Amperometric detector
2
Permanently installed.
Power LED
4
Standby indicator instrument.
Knurled screw
6
For removing the front lid.
Detector input capillary
8
Of the conductivity detector. Permanently mounted.
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2
3
4
5
6
7
8 109
2 Overview of the instrument
Figure 2 Front – Front lid removed
Auxiliary electrode socket
1
For connecting the auxiliary electrode. Labeled with AE.
Cell holder
3
With chip for the automatic detection of the measuring cell.
Reference electrode socket
5
For connecting the reference electrode. Labeled with RE.
Tray
7
Thread
9
For the knurled screw used for fastening the front lid.
Power LED
2
Amperometric detector standby indicator.
Working electrode socket
4
For connecting the working electrode. Labeled with WE.
Coupling
6
For connecting one connection capillary to the measuring cell. Labeled with Eluent to
cell.
Drain nozzle
8
For draining liquid from the tray. Plugged with a stopper.
Coupling
10
For connecting the detector input capillary. Labeled with Eluent in.
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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
Outlet for 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 an 872 Extension Module or an 891 Professional Analog Out. Labeled with Extension Module.
Leak sensor connection socket
7
For connecting the Leak sensor connector plug, labeled with
Leak Sensor.
Mains cable connection socket
9
For connecting the mains cable (6.2122.0x0).
Cable feed-through
2
Outlet for detector cable.
USB connection sockets
4
Two USB connection sockets, labeled with
USB 1 and USB 2.
Detector connection sockets
6
For the connection of the installed detector, labeled with Detector 1 and Detector 2. The detector connection sockets which are not used must be covered with a lid.
Mains switch
8
For switching the instrument on and off.
MSB connection sockets
10
Two MSB connection sockets for connecting instruments with MSB connection, labeled with MSB 1 and MSB 2.
(MSB = Metrohm Serial Bus)
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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 Location

The instrument has been developed for operation indoors and may not be used in explosive environments.

3 Installation

Place the instrument in a location of the laboratory which is suitable for operation and free of vibrations and which provides protection against corrosive atmosphere and contamination by chemicals.
The instrument should be protected against excessive temperature fluctu­ations and direct sunlight.
The distance between the rear of the instrument and the wall must be large enough to secure air circulation on the cooling plate.

3.1.4 Proposed setup

One option is to install the 896 Professional Detector – Conductivity & Amperometry directly above an 850 IC instrument. To accomplish this, the bottle holder of the IC instrument must be removed and then be placed back on the 896 Professional Detector – Conductivity & Amperometry (see Chapter 3.2, page 10).
The other option is to position the 896 Professional Detector – Conductiv­ity & Amperometry directly underneath the 850 IC instrument. To accom­plish this, the base tray of the IC instrument must be removed and then be placed back on underneath the 896 Professional Detector – Conductivity & Amperometry (see Chapter 3.2, page 10).
As an alternative, the 896 Professional Detector – Conductivity & Amper­ometry can be set up together with other instruments using the same sup­port surface in one separate stack next to the IC instrument. We recom­mend that one bottle holder (6.2061.100) and one base tray (6.2061.110) be mounted for each stack of IC instruments.
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3.2 Mounting base tray and bottle holder (optional)

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If a 896 Professional Detector – Conductivity & Amperometry is to be set up underneath an 881 Compact IC pro or an 882 Compact IC plus, then the System Connector (6.2061.120) must be used instead of the base tray of the IC instrument; this adjusts the larger surface area of the 896 Profes­sional Detector – Conductivity & Amperometry to the smaller surface area of the 881 or 882, respectively.
The 896 Professional Detector – Conductivity & Amperometry cannot be set up above an 881 Compact IC pro or an 882 Compact IC plus.
3.2 Mounting base tray and bottle holder (optional)
The 6.2061.110 base tray and 6.2061.100 bottle holder protect IC instru­ments from dust, dirt and leaking fluids. If more than one instrument of the Professional IC family is used, these can be set up in one or more stacks. We recommend that a base tray and a bottle holder be mounted for each stack of IC instruments.
Bottle holder and base tray must be removed or mounted every time one of the following instruments is to be mounted on or under an 850 Profes­sional IC instrument:
One or more 872 Extension Module. An 887 Professional UV/VIS Detector. An 896 Professional Detector. or another instrument of the same support surface.

3.2.1 Removing / mounting the base tray

The base tray must be removed, in case you want to place another instru­ment under the IC instrument. Proceed as follows:
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 connections at the rear of the instrument are disconnected. There are no loose parts in the instrument.
To remove the base tray, you need a 3 mm hexagon key (6.2621.100).
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2
3
Tilt the instrument sideways and lay it down flat.
1
Loosen the cylinder screws with the 3 mm hexagon key and remove
2
them and their washers.
Remove the base tray.
3
3 Installation
The base tray must always be mounted under the lowermost instrument of the stack. Proceed as follows:
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 connections at the rear of the instrument are disconnected. There are no loose parts in the instrument. The instrument is lying on it side, and the bottom surface is visible.
To mount the base tray, you need a 3 mm hexagon key (6.2621.100).
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3.2 Mounting base tray and bottle holder (optional)
1
3
2
Place the base tray in such a way that the openings in the base tray
1
match exactly the screw threads in the bottom of the instrument.
Slide the four washers onto the four cylinder screws, insert the
2
screws and tighten them with the 3 mm hexagon key.
Set the instrument up on the base tray.
3
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Stack other instruments in the required order. Mount the bottle holder (6.2061.100) onto the topmost instrument on the stack (see "Mounting the bottle holder", page 13).

3.2.2 Removing / mounting the bottle holder

The bottle holder must be removed in case you want to mount another instrument on top of the IC instrument. Proceed as follows:
Removing the bottle holder
Before you can remove the bottle holder, the following preconditions must be met:
The instrument is switched off. The bottle holder is cleared. Drainage tubing is disconnected from the drainage tubing connection
of the bottle holder.
To remove the bottle holder, you need a 3 mm hexagon key (6.2621.100).
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2 3
Remove the two covering stoppers.
1
Loosen the two cylinder screws with the 3 mm hexagon key and
2
remove them.
Remove the bottle holder.
3
3 Installation
Stack other instruments in the required order. Mount the bottle holder (6.2061.100) onto the topmost instrument on the stack (see "Mounting the bottle holder", page 13).
Proceed as follows:
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 hexagon key (6.2621.100).
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