Metrohm 894 Professional CVS User manual

894 Professional CVS
Manual
8.894.8001EN / 2017-08-15

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
894 Professional CVS
Manual
8.894.8001EN / 2017-08-15 ebe

Technical Communication
Metrohm AG
CH-9100 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
This documentation has been prepared with great care. However, errors
can never be entirely ruled out. Please send comments regarding possible
errors to the address above.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
894 Professional CVS ￭￭￭￭￭￭￭￭ III
Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.2 Intended use ......................................................................... 2
1.3 About the documentation ................................................... 2
1.3.1 Further information and literature ............................................ 2
1.3.2 Symbols and conventions ........................................................ 3
1.4 Safety instructions ................................................................ 4
1.4.1 General notes on safety ........................................................... 4
1.4.2 Flammable solvents and chemicals ........................................... 4
1.4.3 Electrical safety ........................................................................ 4
1.4.4 Personnel safety ....................................................................... 5
1.4.5 Tubing and capillary connections ............................................. 6
1.4.6 Recycling and disposal ............................................................. 6
2 Overview of the instrument 7
2.1 Front ...................................................................................... 7
2.2 Rear ........................................................................................ 8
2.3 RDE measuring head .......................................................... 10
2.4 Measuring head connector plate and measuring head
insert .................................................................................... 11
2.5 Tubing connector (measuring head arm) ......................... 14
3 Installation 16
3.1 Setting up the instrument .................................................. 16
3.1.1 Packaging .............................................................................. 16
3.1.2 Checks .................................................................................. 16
3.1.3 Location ................................................................................ 16
3.2 Equipping the RDE measuring head ................................. 16
3.2.1 Connecting the gas inlet ........................................................ 19
3.2.2 Preparing electrodes and inserting them in the RDE measur-
ing head ................................................................................ 21
3.3 Establishing the tubing connections ................................. 28
3.3.1 Installing the four-way micro dosing tip ................................. 28
3.3.2 Installing capillaries ................................................................ 30
3.3.3 Installing FEP tubing .............................................................. 33
3.4 Connecting instruments electrically .................................. 40
3.4.1 Connecting the instrument to the power grid ........................ 40
3.4.2 Connecting the 894 Professional CVS .................................... 41
3.4.3 Connecting an 800 Dosino .................................................... 43

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ 894 Professional CVS
4 Start-up 47
5 System configuration 51
5.1 Manual operation ............................................................... 51
5.2 Semiautomated operation ................................................. 52
5.2.1 Connecting devices electrically ............................................... 52
5.2.2 Establishing the tubing connections ....................................... 52
5.3 Automated operation ......................................................... 56
5.3.1 Connecting devices electrically ............................................... 56
5.3.2 Establishing the tubing connections ....................................... 58
6 Operation and maintenance 65
6.1 Care ...................................................................................... 65
6.2 Maintenance by Metrohm Service .................................... 66
6.3 Replacing the measuring head .......................................... 66
6.4 Performing a Dummy cell test ........................................... 68
6.5 Replacing electrode cables ................................................ 70
6.6 Adjusting the sample needle in the Sample Processor ... 71
6.7 Calibrator ............................................................................. 72
6.8 Relocating the 894 Professional CVS ................................ 72
6.9 Quality management and qualification with Metrohm ... 74
7 Troubleshooting 75
7.1 894 Professional CVS ......................................................... 75
7.2 Peripheral devices ............................................................... 77
8 Appendix 79
8.1 Tubing lengths in the measuring head arm ..................... 79
8.2 "Status" LED – Various instrument statuses .................... 79
9 Technical specifications 80
9.1 Operating modes ................................................................ 80
9.2 Potentiostat ........................................................................ 80
9.3 Galvanostat ......................................................................... 81
9.4 Temperature measurement ................................................ 81
9.5 Measuring input ................................................................. 81
9.6 Accuracy .............................................................................. 81
9.7 Resolution ........................................................................... 82

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
894 Professional CVS ￭￭￭￭￭￭￭￭ V
9.8 Calibrator ............................................................................. 82
9.9 Stirrer ................................................................................... 82
9.10 Hardware ............................................................................. 83
9.11 Power connection ............................................................... 83
9.12 Ambient temperature ......................................................... 83
9.13 Reference conditions .......................................................... 83
9.14 Housing data ....................................................................... 84
10 Accessories 85
Index 86

Table of figures ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
VI ￭￭￭￭￭￭￭￭ 894 Professional CVS
Table of figures
Figure 1 894 Professional CVS front ................................................................ 7
Figure 2 894 Professional CVS rear .................................................................. 8
Figure 3 RDE measuring head - Overview ...................................................... 10
Figure 4 Measuring head connector plate ..................................................... 11
Figure 5 Measuring head insert ..................................................................... 13
Figure 6 Tubing connector (measuring head arm) .......................................... 14
Figure 7 Do not touch the drive disk ............................................................. 17
Figure 8 Inserting the measuring head .......................................................... 17
Figure 9 Removing the stopper from the pipetting opening ........................... 18
Figure 10 Removing the measuring head cover ............................................... 18
Figure 11 Inserting the gas inlet ...................................................................... 20
Figure 12 Connecting the gas inlet .................................................................. 21
Figure 13 Removing the protective cap from the electrode tip ......................... 22
Figure 14 Tightening the electrode tip to the driving axle ................................ 22
Figure 15 Working electrode, installed ............................................................ 23
Figure 16 Fastening the drive belt ................................................................... 23
Figure 17 Connecting the working electrode ................................................... 24
Figure 18 Assembling the reference electrode with the electrolyte vessel ......... 25
Figure 19 Connecting a reference electrode .................................................... 26
Figure 20 Connecting the auxiliary electrode ................................................... 27
Figure 21 Inserting the four-way micro dosing tip ........................................... 29
Figure 22 Screwing a PTFE capillary to a dosing unit ........................................ 29
Figure 23 Sealing the PTFE capillary of a four-way micro dosing tip ................. 30
Figure 24 Inserting a PEEK capillary into the measuring head ........................... 31
Figure 25 Screwing a capillary to a dosing unit ................................................ 33
Figure 26 Inserting a piece of FEP tubing into the measuring head .................. 35
Figure 27 Installing the measuring head cover ................................................. 36
Figure 28 Inserting the stopper in the pipetting opening ................................. 37
Figure 29 Installing a bottle cap with pieces of tubing on a rinsing canister ..... 38
Figure 30 Connecting the five-way tubing connector to a waste canister ........ 39
Figure 31 Connecting FEP tubing to the dosing unit (auxiliary solution) ........... 40
Figure 32 Connecting a dosing device to an MSB socket ................................. 43
Figure 33 Manual operation - Electrical connection ......................................... 51
Figure 34 Semiautomated operation – Electrical connections .......................... 52
Figure 35 Semiautomated operation – Tubing setup with two dosing units ..... 53
Figure 36 Semiautomated operation – Tubing setup with four dosing units ..... 54
Figure 37 Semiautomated operation – Tubing setup – Details 894 Professional
CVS ................................................................................................. 55
Figure 38 Automated operation – Electrical connections ................................. 57
Figure 39 Automated operation – Tubing setup – Overview ............................ 59
Figure 40 Automated operation – Tubing setup – Details 894 Professional
CVS ................................................................................................. 60
Figure 41 Automated operation – Tubing setup – 800 Dosino details .............. 61
Figure 42 Automated operation – Tubing setup – 858 Professional Sample Pro-
cessor details – Guide chain ............................................................. 62

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures
894 Professional CVS ￭￭￭￭￭￭￭￭ VII
Figure 43 Automated operation – Tubing setup – Adding rinsing solution and
pumping out the waste solution ...................................................... 63
Figure 44 Automated operation – Tubing configuration – Rinsing and waste solu-
tions – Details 894 Professional CVS ................................................ 64
Figure 45 Removing the measuring head ........................................................ 67
Figure 46 Do not touch the drive disk ............................................................. 68
Figure 47 Dummy cell test – Ideal curve progression ....................................... 69
Figure 48 Replacing electrode cables ............................................................... 70
Figure 49 Adjusting the sample needle in the Sample Processor ...................... 71

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
894 Professional CVS ￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Instrument description
The 894 Professional CVS is a PC-controlled voltammetric measuring
instrument. Together with the viva PC software, it represents a measuring
system specifically designed for the determination of additives in electro-
plating baths. In the electroplating industry, the determination of additives
is an indispensable step in the production process and plays a significant
role in quality assurance. The additives can be quantitatively determined
by means of CVS (Cyclic Voltammetric Stripping).
The 894 Professional CVS is very compact in size and requires little space
for operation. The measuring head can be removed from the instrument
and put back in place again with a simple hand movement. This allows
you to exchange the measuring head with all the electrodes and tubing
quickly. The measuring head arm can be tilted upwards, thus enabling
convenient placement of the measuring vessel in the holder. A rotating
disk electrode (RDE) serves as a working electrode.
The measuring instrument uses the potentiostatic three-electrode princi-
ple. This principle means that the potential at the working electrode is
gauged to the predefined setpoint value with the aid of a reference elec-
trode to which no current is applied. The current flows through a separate
auxiliary electrode.
The 894 Professional CVS can be used both for single determinations and
sample series. Various sample processors are suitable for this measuring
instrument. Furthermore, you can automate the addition of reagents and
auxiliary solutions by using dosing devices of the type 800 Dosino.
The 894 Professional CVS must be started, operated and controlled via the
viva PC software. The data transfer between the measuring instrument
and the PC takes place via a USB connection. At the end of every determi-
nation, the data (voltammogram, results, etc.) is saved in a database.
The present manual describes the hardware of the 894 Professional CVS
(installation, start-up, etc.). Operation by means of the viva PC software is
described in the software documentation (online help and Tutorial CVS).

1.2 Intended use ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ 894 Professional CVS
1.2 Intended use
The 894 Professional CVS has been designed for use in the analysis of
electroplating baths for the quantitative determination of organic addi-
tives. The main fields of application are the following electroplating bath
types:
￭Acidic copper baths
￭Tin baths
￭Tin-lead baths
￭Alkaline zinc baths
￭Nickel baths
This instrument is suitable for processing various chemicals and flammable
samples. Therefore, the use of the 894 Professional CVS requires the user
to have basic knowledge and experience in handling toxic and caustic
substances. Knowledge regarding the application of fire prevention meas-
ures prescribed for laboratories is also mandatory.
Before performing any analysis, the user should get acquainted with the
hazard and precautionary statements or the risk and safety phrases that
are valid for the chemicals used. The user should also observe the precau-
tionary measures prescribed.
1.3 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 opera-
tion of the instrument.
1.3.1 Further information and literature
You can find further information regarding the 894 Professional CVS in the
following publications:
￭Tutorial CVS
￭Multimedia guide "Electrodes in Voltammetry"
￭Online help for the viva computer software
￭Monograph "Voltammetric analysis methods in electroplating"

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894 Professional CVS ￭￭￭￭￭￭￭￭ 3
1.3.2 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.
Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
[Next] Button or key
WARNING
This symbol draws attention to a possible life-threat-
ening 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.

1.4 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ 894 Professional CVS
1.4 Safety instructions
1.4.1 General notes on safety
WARNING
This instrument may only be operated in accordance with the specifica-
tions 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.
1.4.2 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.
1.4.3 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.
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.

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894 Professional CVS ￭￭￭￭￭￭￭￭ 5
Supply voltage
WARNING
An incorrect supply voltage can damage the instrument.
Only operate this instrument with a supply 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 power cord out of the power socket before you
set up or disconnect electrical plug connections at the rear of the
instrument.
1.4.4 Personnel safety
WARNING
Handling hazardous substances
Hazardous substances may result in injuries.
Wear protective glasses and work clothes suitable for laboratory work.
WARNING
Uncontrolled splashing of reagents
Splashing reagents may result in injuries.
Operate the 894 Professional CVS only with the measuring head in
place and the measuring head arm lowered.

1.4 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
6￭￭￭￭￭￭￭￭ 894 Professional CVS
1.4.5 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 con-
nections. 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 manda-
tory.
1.4.6 Recycling and disposal
This product is covered by European Directive 2012/19/EU, WEEE – Waste
Electrical and Electronic Equipment.
The correct disposal of your old instrument will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old instrument can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

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894 Professional CVS ￭￭￭￭￭￭￭￭ 7
2 Overview of the instrument
The following figures provide a detailed overview of the parts of the 894
Professional CVS. Some of these parts are not specifically relevant for CVS
analyses, but for the sake of completeness they are listed nevertheless;
however, they are grayed out and labeled "Not relevant for CVS analyses".
2.1 Front
1
2
3
4
5
6
8
7
Figure 1 894 Professional CVS front
1"Status" LED
Continuously on: instrument ready for oper-
ation. Blinking regularly: instrument operat-
ing. Blinking pattern "LED on a long time -
off a short time - on a long time - off a short
time, etc.": Standby potential is being
applied to the electrodes. Do not remove
the electrode cables!
2"On" LED
Illuminated if the 894 Professional CVS is
connected to the power grid.

2.2 Rear ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭ 894 Professional CVS
3Holder for measuring vessel
For inserting the measuring vessel.
4Connector plate measuring head arm
For inserting the measuring head.
5Measuring head arm (tiltable) 6Gas washing glass (6.2405.030)
Not relevant for CVS analyses.
7Decanting glass (6.2405.030)
For the deposition of solid materials that
may be present.
8Holder for drip pan
For positioning the drip pan.
2.2 Rear
1
2
3
4
5
6
7
8
9
Figure 2 894 Professional CVS rear
1Temperature sensor connector (Temp.)
For connecting a temperature sensor of the
type Pt1000. Two B sockets, 2 mm.
2Type plates
With serial number.

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894 Professional CVS ￭￭￭￭￭￭￭￭ 9
3Calibrator
For service procedures carried out by Met-
rohm.
4Fan
Runs during operation.
5Tubing connector (measuring head
arm)
See Chapter 2.5, page 14.
6USB connectors (USB 1 and USB 2),
type A
For connecting barcode readers, keyboards,
etc.
7"Controller" connector
For connecting to a PC with the viva com-
puter software installed. Mini DIN, 8-pin.
8MSB connectors (MSB 1 to 4)
Metrohm Serial Bus. For connecting dosing
devices (800 Dosino) and Remote Boxes.
Mini DIN, 8-pin.
9Power socket

2.3 RDE measuring head ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 894 Professional CVS
2.3 RDE measuring head
1
2
3
4
5
Figure 3 RDE measuring head - Overview
1Measuring head insert
With openings for inserting electrodes and
tubing connections (see Figure 5, page 13).
2Measuring head connector plate
For connecting the RDE measuring head to
the connector plate of the measuring head
arm (1-4).
For connecting the electrodes and tubing
(see Figure 4, page 11).