Metrohm 874 User Manual
874 Oven Sample Processor
Manual
8.874.8002EN
Metrohm AG
CH-9101 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
info@metrohm.com
www.metrohm.com
874 Oven Sample Processor
Manual
8.874.8002EN 06/2011 dm
Teachware
Metrohm AG
CH-9101 Herisau
teachware@metrohm.com
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been
checked with great care, errors cannot be entirely excluded. Should you
notice any mistakes please send us your comments using the address
given above.
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Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Instrument versions ................................................................. 1
1.1.2 Instrument components .......................................................... 2
1.1.3 Intended use ........................................................................... 2
1.2 About the documentation ................................................... 3
1.2.1 Notation and Pictograms ......................................................... 3
1.3 Safety instructions ................................................................ 4
1.3.1 General notes on safety ........................................................... 4
1.3.2 Electrical safety ........................................................................ 4
1.3.3 Tubing and capillary connections ............................................. 5
1.3.4 Personnel safety ...................................................................... 5
1.3.5 Flammable solvents and chemicals ........................................... 7
1.3.6 Recycling and disposal ............................................................. 7
Table of contents
2 Overview of the instrument 8
3 Installation 12
3.1 Setting up the instrument .................................................. 12
3.1.1 Packaging .............................................................................. 12
3.1.2 Checks .................................................................................. 12
3.1.3 Location ................................................................................ 12
3.2 Connecting a mains cable .................................................. 12
3.3 Mounting the sample insert .............................................. 13
3.4 Mounting the needles ........................................................ 14
3.5 Mounting the heating tube ............................................... 17
3.6 Mounting the drying flasks ............................................... 18
3.7 Mounting the dust filter .................................................... 20
3.8 Mounting the air/nitrogen connector ............................... 20
3.9 Mounting the safety shield ................................................ 22
3.10 Mounting the KF titration cell ........................................... 23
3.11 Inserting the heating tube into the KF titration cell ....... 24
874 Oven Sample Processor
3.12 Attaching the sample rack ................................................. 27
3.13 Adjusting the guide rod ..................................................... 28
3.14 Connecting a computer ..................................................... 28
3.15 Connecting MSB devices ................................................... 30
3.15.1 Connecting dosing devices .................................................... 31
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III
Table of contents
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3.15.2 Connecting a stirrer or titration stand .................................... 32
3.15.3 Connecting a remote box ...................................................... 33
3.16 Connecting USB devices ..................................................... 34
3.16.1 Connecting a barcode reader ................................................. 34
4 Processing a sample series 36
5 Handling and maintenance 37
5.1 General ................................................................................ 37
5.2 Care ...................................................................................... 37
5.3 Quality Management and validation with Metrohm ....... 37
6 Troubleshooting 39
6.1 Problems and their solutions ............................................. 39
7 Appendix 40
7.1 Remote interface ................................................................ 40
7.1.1 Pin assignment of the remote interface .................................. 40
7.2 Stirring rate ......................................................................... 42
8 Technical specifications 43
8.1 Lift and turntable ............................................................... 43
8.2 Oven ..................................................................................... 43
8.3 Gas flow .............................................................................. 43
8.4 Outlet heater ....................................................................... 44
8.5 Interfaces and connectors ................................................. 44
8.6 Mains connection ............................................................... 44
8.7 Safety specifications ........................................................... 44
8.8 Electromagnetic compatibility (EMC) ................................ 45
8.9 Ambient temperature ......................................................... 45
8.10 Reference conditions .......................................................... 46
8.11 Dimensions .......................................................................... 46
9 Conformity and warranty 47
9.1 Declaration of Conformity ................................................. 47
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IV
9.2 Quality Management Principles ........................................ 48
9.3 Warranty (guarantee) ......................................................... 49
10 Accessories 51
10.1 Scope of delivery 2.874.0010 ............................................ 51
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Index 70
Table of contents
10.2 Scope of delivery 2.874.0020 ............................................ 59
10.3 Optional accessories ........................................................... 66
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Table of figures
Table of figures
Figure 1 Front 874 Oven Sample Processor ..................................................... 8
Figure 2 Rear 874 Oven Sample Processor .................................................... 10
Figure 3 6.2041.720 sample rack .................................................................. 11
Figure 4 Connecting the mains cable ............................................................ 12
Figure 5 Mounting the sample insert ............................................................. 13
Figure 6 Mounting the needles ..................................................................... 15
Figure 7 Mounting the tubing ....................................................................... 16
Figure 8 Mounting the heating tube ............................................................. 17
Figure 9 Preparing the drying flasks ............................................................... 18
Figure 10 Mounting the tubings ..................................................................... 19
Figure 11 Mounting the dust filter .................................................................. 20
Figure 12 External gas connector .................................................................... 21
Figure 13 Mounting the safety shield .............................................................. 22
Figure 14 Coulometric KF titration cell ............................................................ 25
Figure 15 Volumetric KF titration cell .............................................................. 26
Figure 16 Attaching the rack ........................................................................... 27
Figure 17 Adjusting the guide rod ................................................................... 28
Figure 18 Connecting the computer ............................................................... 29
Figure 19 Connecting a dosing device ............................................................. 32
Figure 20 Connecting MSB stirrer .................................................................... 32
Figure 21 Rod Stirrer and titration stand .......................................................... 33
Figure 22 Connecting a remote box ................................................................ 33
Figure 23 USB connectors ............................................................................... 34
Figure 24 Connectors of the remote box ......................................................... 40
Figure 25 Pin assignment of the remote socket and plug ................................ 40
Figure 26 Rotational speed depending on stirring rate .................................... 42
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874 Oven Sample Processor
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1 Introduction
1.1 Instrument description
The 874 Oven Sample Processor is used whenever the heating up of a
sample and/or the thermal expulsion of moisture in solid substances or liquids is required. In combination with a coulometric or volumetric KF titrator, the 874 Oven Sample Processor is the ideal analysis system for water
determination in samples that contain disruptive components or from
which moisture can be removed only with difficulty.
One of its decisive advantages is the reduction of sample preparation to a
minimum. Thanks to the use of hermetically sealed sample vessels ("headspace vials"), the filling of the samples can be accomplished directly onsite. The PTFE-coated septa guarantee a constant, non-falsified water content, even after prolonged holding times.
1 Introduction
The sample heated in the oven module releases its moisture in the form of
water vapor, which is conveyed into a measuring cell with the aid of a gas
flow. An air pump is installed for the purpose of generating the gas flow.
An inlet valve is available for nitrogen or other inert gases. The determination of the moisture can be accomplished in the measuring cell either coulometrically or volumetrically according to Karl Fischer.
The operation and control of the 874 Oven Sample Processor is accomplished by means of the tiamo™ PC software. This enables convenient
programming of method runs, ranging from the simple to the complex.
The integration of the 874 Oven Sample Processor together with other
instruments (e. g. with a coulometer) using one user interface, makes not
only simple operation possible, but also the evaluation and storage of the
measurement data from all of the linked instruments in one single database.
1.1.1 Instrument versions
The 874 Oven Sample Processor is available in two versions with different
accessories.
￭ Version 2.874.0010 with accessories for the usage of standard vials
(volume 6 mL)
￭ Version 2.874.0020 without accessories for the usage of standard
vials. Appropriate accessories can be ordered for specific vessel sizes.
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1.1 Instrument description
1.1.2 Instrument components
The 874 Oven Sample Processor has the following components:
￭ Oven
Oven module made of aluminum with software-operated temperature
control for heating the sample vessel.
￭ Fan
Propeller fan for cooling the oven module.
￭ Inlet valve
Valve for switching over the source of the gas flow.
￭ Air pump
Pump for generating the gas flow.
￭ Outlet heater
Heating tube for preventing the condensation of moisture.
￭ Lift with rods
Guidance device with needle adapter and tubing for the gas flow.
￭ Turntable
For the standard sample rack with a capacity of 36 sample vials (6 mL)
or the special sample rack with a capacity of 25 sample vials (⌀ = 16 ...
32 mm).
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1.1.3 Intended use
The 874 Oven Sample Processor is designed for usage as an auxiliary
device for sample preparation in analytical laboratories. Its main area of
application is the moisture determination according to Karl Fischer (coulometric or volumetric). The 874 Oven Sample Processor enables the application of thermal gas extraction technique.
The present instrument is suitable for processing chemicals and flammable
samples. The usage of the 874 Oven Sample Processor therefore requires
that the user has 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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874 Oven Sample Processor
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1.2 About the documentation
Caution
Please read through this documentation carefully before putting the
instrument into operation. The documentation contains information
and warnings which have to be followed by the user in order to ensure
safe operation of the instrument.
1.2.1 Notation and Pictograms
The following notations and pictograms (symbols) are used in these
Instructions for Use:
1 Introduction
Cross-reference to illustration
legend number
The first number stands for the
number of the illustration, the
second for the legend number.
Instruction step
Follow these steps.
Methode Dialog, Parameter in the soft-
ware
[Weiter] Button in the software or Key on
the keyboard.
Warning
This symbol draws attention to a
possilbe danger of life or injury.
Warning
This symbol draws attention to a
possilbe danger through electrical
current.
Warning
This symbol draws attention to a
possible danger through heat or
hot instrument parts.
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1.3 Safety instructions
1.3 Safety instructions
1.3.1 General notes on safety
Warning
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Warning
This symbol draws attention to a
possible biological hazard.
Caution
This symbol draws attention to
possible damage of instruments or
instrument parts.
Comment
This symbol marks additional
information and tips.
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.
Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.
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.
Warning
Warning
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4
There are no parts inside the housing which can be serviced or replaced
by the user.
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1 Introduction
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.
Always pull the mains cable out of the mains connection socket before
connecting or disconnecting electrical appliances on the rear panel 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.
1.3.4 Personnel safety
Warning
Wear protective goggles and working clothes suitable for laboratory
work while operating the 874 Oven Sample Processor. It is also advisable to wear gloves when caustic liquids are used or in situations where
glass vessels could break.
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1.3 Safety instructions
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Warning
Always install the safety shield supplied with the equipment before
using the instrument for the first time. Pre-installed safety shields are
not allowed to be removed.
The 874 Oven Sample Processor may not be operated without a safety
shield!
Warning
Personnel are not permitted to reach into the working area of the
instrument while operations are running!
A considerable risk of injury exists for the user.
Warning
In the event of a possible blockage of a drive, the mains plug must be
pulled out of the socket immediately. Do not attempt to free jammed
sample vessels or other parts while the device is switched on. Blockages
can only be cleared when the instrument is in a voltage-free status; this
action generally involves a considerable risk of injury.
Warning
The 874 Oven Sample Processor is not suitable for utilization in biochemical, biological or medical environments in its basic equipment version.
Appropriate protective measures must be implemented in the event
that potentially infectious samples or reagents are being processed.
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874 Oven Sample Processor
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1.3.5 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.
￭ Keep all sources of flame far from the workplace.
￭ Clean up spilled fluids and solids immediately.
￭ Follow the safety instructions of the chemical manufacturer.
1.3.6 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.
1 Introduction
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.
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2 Overview of the instrument
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
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Figure 1 Front 874 Oven Sample Processor
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874 Oven Sample Processor
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2 Overview of the instrument
Safety shield (6.2751.140)
1
Sample rack (6.2041.720)
3
For 36 sample vials (6 mL).
Guide bolts
5
For the sample rack.
Rod holder
7
With knurled screw.
Working head
9
Gas outlet
11
With M6 thread.
Heating tube connector
13
Support rod (6.2016.030)
15
For fixing the titration cell.
Oven module
17
With PTFE covering.
Conditioning position
2
For the conditioning vessel.
Turntable
4
Guide rod
6
For stripping off the sample vessel.
Guide head
8
Distributor
10
Air pump inlet
12
For the 6.2724.010
Lift
14
Beaker sensor
16
Oven housing
18
With ventilation slits.
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USB 2
1
2
3
4
5
6
7
8
9
Figure 2 Rear 874 Oven Sample Processor
USB connector (USB 1 and USB 2)
1
USB ports (type A) for connecting a printer,
USB hub, Titrandos, additional USB devices
etc.
MSB connector (MSB 1 to MSB 3)
3
Metrohm Serial Bus. For connecting external
dosing devices, stirrers or remote boxes.
Mini DIN, 9-pin.
Type plate
5
Contains specifications concerning mains
voltage, instrument type and serial number.
Air/nitrogen connector
7
With M6 interior thread. Inlet for external
gassing.
Drying flask holder
9
Controller connector (Controller)
2
For connecting a computer with installed PC
software.
Mains connection socket
4
Warning symbol
6
Biological hazard.(see Chapter 1.3.4, page
5)
Gas inlet and outlet
8
For connecting drying flasks, with M6 inner
thread.
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874 Oven Sample Processor
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1
2
3
2 Overview of the instrument
Conditioning position
1
For the conditioning vessel.
Handle
3
With fixing screw.
Figure 3 6.2041.720 sample rack
Guide pins
2
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11
3.1 Setting up the instrument
P: 115W U: 100 - 240 V f: 50 - 60 Hz
Nr.
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.
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Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctuations and direct sunlight.
3.2 Connecting a mains cable
Warning
This instrument must not be operated except with the mains voltage
specified for it (see rear panel of the instrument).
Protect the connection sockets against moisture.
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Figure 4 Connecting the mains cable
874 Oven Sample Processor
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1
2
3
6.2063.020
6.2627.010
3.3 Mounting the sample insert
The dimensions of the supplied sample insert are optimized for the usage
of 6.2419.007 sample vials (6 mL) from Metrohm . This ensures the
best possible transfer of heat between oven and sample.
3 Installation
Figure 5 Mounting the sample insert
Note
The sample insert may not be inserted or removed unless it has been
cooled down.
Proceed as follows:
Insert the 6.2627.010 oven insert with the spring in place into the
1
oven from above and slide it all the way to the bottom.
Place the 6.2063.020 sample insert into the oven from above.
2
Tighten the sample insert with the supplied hexagon screws. The
3
required hexagon key is part of the accessories.
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3.4 Mounting the needles
Note
If vessels with other dimensions are to be used, then individually modified sample inserts can be ordered. The precise vessel dimensions
(including tolerances) will be required when ordering. Non-standard
sample vessels may not exhibit dimensions outside of the following limit
values:
￭ Diameter 10.0…32.0 mm
￭ Immersion depth 20.0…45.0 mm
3.4 Mounting the needles
Two different types of needle holders are available for mounting needles.
The length of the needle holder defines how deeply the injection needle
penetrates the sample vessel. The 6.2049.040 needle holder, which is
58 mm in length, ensures that the needle penetrates the liquid or powdery sample. The carrier gas can flow through the sample and effect an
efficient expulsion of the moisture it contains.
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If there is a danger that the heated sample could clog the needle, then
use the 6.2049.050 needle holder with 73 mm length. In this case the
injection needle penetrates the sample vessel only slightly deeper than the
outlet needle and has no contact with the sample itself.
Needle holders with the dimensions required for situations calling for special sample vessels can be supplied by Metrohm upon request.
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874 Oven Sample Processor
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6.2816.080
6.2049.040/6.2049.050
6.2816.070
1
2
3
3 Installation
Mounting the injection and outlet needle
Figure 6 Mounting the needles
Mount the needles as follows
Screw the needle holder (6.2049.040 or 6.2049.050) into the distri-
1
butor on the guide head.
Screw the 6.2816.080 outlet needle onto the Luer connector of
2
the needle holder.
Carefully guide the 6.2816.070 injection needle into the opening
3
of the distributor from above and allow it to drop down.
Note
Take care to ensure that the white PTFE seal is positioned securely
on the needle.
Screw the 6.1805.470 FEP tubing by hand onto the opening of
4
the distributor. Screw the other end of the tube into the opening of
the gas outlet on the upper side of the tower.
874 Oven Sample Processor
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3.4 Mounting the needles
6.1805.470
4
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Figure 7 Mounting the tubing
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874 Oven Sample Processor
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