Metrohm 763PVC User Manual
CH-9101 Herisau/Switzerland
Phone ++41 71 353 85 85
Fax ++41 71 353 89 01
Internet www.metrohm.ch
E-Mail info@metrohm.ch
763 PVC Thermomat
with «763 PVC Thermomat 1.0» PC program
763 PVC Thermomat
8.763.1003 Instructions for Use
26.10.1999 / dö
Contents
Table of contents
1 Introduction............................................................................................................1
1.1 Determination of thermal stability........................................................1
1.2 Instrument description.................................................................................2
1.3 Operating elements........................................................................................3
1.4 Information about these Instructions for Use................................6
1.4.1 Organization................................................................................................. 6
1.4.2 Notation and pictograms............................................................................ 7
1.5 Safety notes.........................................................................................................8
1.5.1 Electrical safety ........................................................................................... 8
1.5.2 General precautionary rules...................................................................... 8
2 Installation..............................................................................................................9
2.1 Setting up the instrument...........................................................................9
2.1.1 Packaging ..................................................................................................... 9
2.1.2 Check............................................................................................................. 9
2.1.3 Location ........................................................................................................ 9
2.2 Attaching the accessories.......................................................................10
2.2.1 Accessories for external gas supply...................................................... 10
2.2.2 Reaction and measuring vessels............................................................ 10
2.2.3 Exhaust collection tube (option)............................................................. 11
2.3 Mains connection..........................................................................................13
2.3.1 Checking the mains voltage....................................................................13
2.3.2 Exchange of fuses.....................................................................................13
2.3.3 Mains cable and mains connection........................................................ 14
2.3.4 Switching the instrument on/off ............................................................. 14
2.4 Connection to the PC..................................................................................15
2.4.1 Connection PVC Thermomat – PC.......................................................... 15
2.4.2 Software installation.................................................................................15
2.4.3 Basic settings............................................................................................. 16
3 Operating tutorial....................................................................................... 19
3.1 Determinations...............................................................................................19
3.1.1 Installation..................................................................................................19
3.1.2 Preparing for determinations .................................................................. 20
3.1.3 Carrying out determinations.................................................................... 22
3.2 Results .................................................................................................................24
3.2.1 Determination overview............................................................................ 24
3.2.2 Determination and method data ............................................................. 26
3.2.3 Graphics......................................................................................................28
763 PVC Thermomat I
Contents
4 Operation...............................................................................................................31
4.1 Fundamentals of the operation............................................................ 31
4.1.1 Starting/closing the program.................................................................. 31
Start the «763 PVC Thermomat» program................................................31
Close the «763 PVC Thermomat» program..............................................31
4.1.2 Glossary...................................................................................................... 32
4.1.3 Control window ......................................................................................... 33
Open ........................................................................................................33
Arrangement.............................................................................................33
Menus ......................................................................................................33
Icons.........................................................................................................34
Close ........................................................................................................34
4.1.4 Results window ......................................................................................... 35
Open ........................................................................................................35
Arrangement.............................................................................................35
Menus ......................................................................................................35
Icons.........................................................................................................36
Close ........................................................................................................36
4.1.5 Overview of file types............................................................................... 37
4.1.6 Context-sensitive menus......................................................................... 37
4.1.7 Mouse functions........................................................................................ 37
4.1.8 Help.............................................................................................................. 37
4.2 Instrument and software settings...................................................... 38
4.2.1 Communication ......................................................................................... 38
4.2.2 User permissions...................................................................................... 39
Functions for groups................................................................................39
Functions for users ..................................................................................40
4.2.3 Timer............................................................................................................ 41
4.2.4 Gas flow control........................................................................................ 41
4.2.5 Recording temperature ............................................................................ 42
4.2.6 Options........................................................................................................ 43
Save settings............................................................................................43
Clear sample ID1 history..........................................................................43
4.3 Program information................................................................................... 44
4.3.1 Unit information......................................................................................... 44
4.3.2 Status overview......................................................................................... 45
4.3.3 Events overview ........................................................................................ 46
Event window ...........................................................................................46
Menus ......................................................................................................47
Icons.........................................................................................................47
Filter..........................................................................................................47
Parameter for event recording .................................................................47
763 PVC ThermomatII
Contents
4.4 Calibration functions ..................................................................................48
4.4.1 Determination of cell constants.............................................................. 48
Manual entry of cell constants ................................................................ 48
Automatic determination of cell constants.............................................. 48
4.4.2 Determination of Delta T .......................................................................... 50
Preparations ............................................................................................ 50
Carrying out............................................................................................. 52
4.5 Methods...............................................................................................................54
4.5.1 Method handling........................................................................................ 54
Create method......................................................................................... 54
Open method .......................................................................................... 54
Method manager..................................................................................... 54
Save method ........................................................................................... 55
Print method report.................................................................................. 55
4.5.2 Method parameters ................................................................................... 55
Overview.................................................................................................. 55
Parameters .............................................................................................. 56
Evaluation ................................................................................................ 58
Induction time.......................................................................................... 59
Stability time ............................................................................................ 59
Curves ..................................................................................................... 60
Formulas.................................................................................................. 61
Standards ................................................................................................ 62
Documentation........................................................................................ 63
Description .............................................................................................. 64
4.6 Determinations............................................................................................... 65
4.6.1 Flow chart ................................................................................................... 65
4.6.2 Sample preparation................................................................................... 66
4.6.3 Prepare instruments and accessories................................................... 66
Clean instruments and accessories........................................................ 66
Prepare measuring vessels..................................................................... 67
Prepare reaction vessels......................................................................... 68
4.6.4 Carry out determinations......................................................................... 69
Select method ........................................................................................ 69
Switch on heating.................................................................................... 69
Enter sample identifiers........................................................................... 70
Insert reaction vessels............................................................................. 70
Start determination .................................................................................. 70
Live curve ................................................................................................ 71
Live parameters....................................................................................... 71
Stop determination .................................................................................. 72
4.7 Results..................................................................................................................73
4.7.1 Determination overview............................................................................ 73
Open determination overview ................................................................. 73
Format determination overview............................................................... 74
Mark determinations................................................................................ 78
Find determination .................................................................................. 78
Delete determinations ............................................................................. 79
Sort and filter determinations .................................................................. 80
763 PVC Thermomat III
Contents
4.7.2 Determination and method data............................................................. 84
Open view ................................................................................................84
Determination...........................................................................................84
Results......................................................................................................85
Method .....................................................................................................86
Parameters...............................................................................................87
Evaluation.................................................................................................88
Formulas ..................................................................................................89
Standards.................................................................................................90
Curves ......................................................................................................90
Documentation.........................................................................................91
Warnings ..................................................................................................92
4.7.3 Graphics and reevaluation ...................................................................... 93
Single graph.............................................................................................93
Multiple graph ..........................................................................................93
Live graph.................................................................................................94
Switch zoom on/off ..................................................................................95
Switch autoscaling on/off.........................................................................95
Switch offset on/off...................................................................................95
Copy graph to clipboard..........................................................................95
Print graph................................................................................................95
Reevaluation.............................................................................................96
4.7.4 Extrapolation.............................................................................................. 99
Extrapolation window ...............................................................................99
Print extrapolation results.......................................................................100
Settings for extrapolation .......................................................................101
Parameters for extrapolation..................................................................101
4.7.5 Recalculation ........................................................................................... 102
Recalculation window ............................................................................102
Method ...................................................................................................102
Formulas ................................................................................................103
Standards...............................................................................................104
4.7.6 Data export and printing........................................................................ 106
Copy to clipboard ..................................................................................106
Export to other database........................................................................106
Export to Microsoft Word .......................................................................106
Export to Microsoft Excel .......................................................................106
Export of measured values ....................................................................107
Export of determination and method data.............................................107
Printing of results in the control window ................................................108
Printing of data in the results window ....................................................109
4.7.7 Options...................................................................................................... 110
Program settings....................................................................................110
Report settings.......................................................................................110
Company settings..................................................................................111
Results....................................................................................................112
Scaling....................................................................................................112
Extrapolation ..........................................................................................113
Live graph...............................................................................................114
Options for the administrator .................................................................114
Save settings..........................................................................................115
4.7.8 Windows................................................................................................... 115
Tile windows vertically............................................................................115
Tile windows horizontally........................................................................115
Cascade windows..................................................................................115
Arrange icons.........................................................................................115
Close all windows ..................................................................................115
763 PVC ThermomatIV
Contents
4.8 GLP ...................................................................................................................... 116
4.8.1 General information about GLP and validation.................................. 116
4.8.2 GLP properties.........................................................................................117
4.8.3 GLP status................................................................................................117
4.8.4 GLP tests...................................................................................................118
GLP temperature test ............................................................................ 118
GLP conductivity test............................................................................. 123
GLP gas flow test .................................................................................. 126
4.8.5 GLP results............................................................................................... 128
Print GLP certificate............................................................................... 128
View GLP results.................................................................................... 128
Print GLP results.................................................................................... 130
5 Maintenance – Faults..........................................................................131
5.1 Maintenance and service......................................................................131
5.1.1 Care............................................................................................................131
5.1.2 Maintenance by Metrohm service.........................................................131
5.2 Faults and malfunctions........................................................................ 132
5.2.1 Error messages in the PC program...................................................... 132
5.2.2 Status and error messages on the instrument................................... 132
6 Appendix .............................................................................................................135
6.1 Technical data ............................................................................................. 135
6.1.1 General information................................................................................135
6.1.2 Temperature regulation and measurement......................................... 135
6.1.3 Conductivity measurement.................................................................... 136
6.1.4 Gas flow regulation................................................................................. 136
6.1.5 GLP test set.............................................................................................. 136
6.1.6 RS232 interface........................................................................................136
6.1.7 Mains connection....................................................................................137
6.1.8 Safety specifications............................................................................... 137
6.1.9 Electromagnetic compatibility (EMC) .................................................. 137
6.1.10 Ambient temperature.............................................................................. 138
6.1.11 Housing..................................................................................................... 138
6.2 Standard equipment................................................................................. 139
6.3 Optional accessories............................................................................... 142
6.4 Warranty and conformity....................................................................... 143
6.4.1 Warranty....................................................................................................143
6.4.2 Software license ...................................................................................... 143
6.4.3 EU Declaration of conformity................................................................ 144
6.4.4 Certificate of conformity and system validation................................ 145
6.5 Index...................................................................................................................146
763 PVC Thermomat V
Contents
List of figures
Fig. 1: Schematic measuring arrangement ............................................................... 1
Fig. 2: Front of the 763 PVC Thermomat ................................................................... 3
Fig. 3: Rear of the 763 PVC Thermomat.................................................................... 4
Fig. 4: Installation of reaction and measuring vessels ............................................ 12
Fig. 5: Accessories for Delta-T determination ......................................................... 51
Fig. 6: Accessories for GLP temperature test........................................................ 121
Fig. 7: Indicator lamps ........................................................................................... 132
List of numbered parts and controls
11 Reaction vessel............................. 3,12,51
22 Reaction vessel cover................... 3,12,51
33 Connecting tubing ............................. 3,13
44 Measuring vessel............................... 3,13
55 Measuring vessel cover.....................3,13
66 Connecting tubing ....................... 3,12,51
77 Mains pilot lamp ..............................3,132
88 Gas flow display .............................3,132
99 Temperature display........................ 3,132
1010 Error display.....................................3,132
1111 Instrument display ...........................3,132
1212 Mains switch........................................... 5
1313 Mains connection plug ........................... 5
1414 Fuse holder.............................................5
1515 Model plate............................................. 5
1616 PC connection ........................................5
1717 Pt100 connection....................................5
1818 Connection "N2 in"................................... 5
2222 Connection piece..................................12
2323 Opening "Out" .......................................12
2424 Opening "In" ..........................................12
2525 Marking field..........................................12
2626 Connection plug....................................12
2727 PTFE tube..............................................12
2828 Electrodes .............................................12
2929 Protective ring .......................................12
3030 Connection nipple............................12,51
3131 Connection.......................................12,51
3232 Gas inlet tube (short) ............................12
3333 Sealing ring ......................................12,51
3434 Connection.......................................12,51
3535 Gas inlet tube (long)..............................51
3636 Temperature sensor Pt100.............51,121
3737 Distance piece ...............................51,121
3838 PTFE cylinder ......................................121
3939 Hexagonal screw.................................121
1919 Gas supply connection........................... 5
2020 Electrode connection.............................. 5
2121 Mounting for exhaust collection tube .....5
4040 Allen key..............................................121
4141 Aluminium cylinder..............................121
763 PVC ThermomatVI
1.1 Determination of thermal stability
1 Introduction
1.1 Determination of thermal stability
The determination of the thermal stability of polyvinyl chloride according
to DIN 53 381, part 1, is based on the fact that PVC decomposes at
higher temperatures with the release of HCl. The hydrochloric acid
formed is taken up by a gas stream (normally N2) and transferred into
the measuring vessel where it is absorbed in the measuring solution
(dist. water). The decomposition process is monitored by measuring
the conductivity of the aqueous HCl solution. Both the stability time and
the induction time are determined. The stability time is defined as the
time required to achieve a conductivity difference of 50 µS/cm. The in-
duction time is the time that elapses before the conductivity starts to
rise sharply. The method is used for testing PVC in all stages of processing as well as for testing stabilizers.
N
2
Reaction vessel
PVC
Heating block
Fig. 1: Schematic measuring arrangement
Measuring
vessel
Conductivity
measuring cell
Measuring
solution
763 PVC Thermomat 1
1 Introduction
1.2 Instrument description
The 763 PVC Thermomat is a PC-controlled instrument for determining the thermal stability of PVC and similar halogenated plastics and is
available in the following two versions:
• 2.763.0014 PVC Thermomat for 230 V, 50……60 Hz
• 2.763.0015 PVC Thermomat for 115 V, 50……60 Hz
The 763 PVC Thermomat is equipped with two heating blocks each
with 4 measuring positions. Each block can be individually heated, i.e.
2 sets of 4 samples can be measured at two different temperatures or 8
samples can be measured at the same temperature. Measurements at
the individual measuring positions can be started individually.
The complete operation of the 763 PVC Thermomat is carried out via a
PC connected to the RS232 interface with the aid of the «763 PVC
Thermomat» control and evaluation program. Up to 4 instruments can
be connected to 1 PC allowing a maximum of 32 samples to be analyzed at the same time. The evaluation algorithm of the PC program
determines the point of inflection of the Thermomat curve and therefore
the induction time fully automatically. Apart from the induction time,
the so-called stability time, i.e. the time taken until a certain alteration
in the conductivity is reached, can also be determined. The results obtained can be subjected to further mathematical processes. In particular, induction times can be converted to the standard temperatures
contained in the relevant standards.
Each Thermomat curve can also be evaluated manually. A PC-supported tangent method is available for this in which the tangents can be
applied to the curve as required. This means that evaluations are possible even in extreme cases.
The results of the determinations are stored in a database together
with all the data concerning the method and determination. In the results display part of the program determinations can be searched for,
sorted, filtered, exported and printed out. Apart from the graphical display of single and multiple curves it is also possible to carry out recalculations with altered parameters and to extrapolate the results to a
particular temperature.
GLP (Good Laboratory Practice) and instrument validation are continuously increasing in importance. In the 763 PVC Thermomat GLP tests
are provided for the measurement of temperature, conductivity and gas
flow. They determine whether and which tests are to be carried out. The
time interval between the tests and the required accuracy can also be
laid down as required. If the GLP function is selected then on each result report a remark will be made as to whether the GLP test requirements have been fulfilled. As an option Metrohm offers a GLP test set
(6.5616.000), with which the most important tests can be carried out.
763 PVC Thermomat2
1.3 Operating elements
1.3 Operating elements
77
88
99
1010
1111
763 PVC Thermomat
66
55
44
33
22
11
Fig. 2: Front of the 763 PVC Thermomat
11 Reaction vessel (6.1429.040) 77 Mains pilot lamp
lit up when instrument switched on
22 Reaction vessel cover (6.2753.100) 88 Gas flow display
lit up when gas flow switched on
33 Connecting tubing (6.1816.010)
between reaction vessel and measuring
vessel
44 Measuring vessel (6.1428.100) 1010 Error display (red)
55 Measuring vessel cover (6.0913.130)
with built-in conductivity measuring cell
66 Connecting tubing (6.1805.080)
for gas supply into reaction vessel
99 Temperature display
flashes when heating switched on
lit up when temperature reached
lit up at error
1111 Instrument display
indicates numbers (1…4) of units
connected
763 PVC Thermomat 3
1 Introduction
2121
Made by Metrohm Herisau Switzerland
2020
1919
Type:
Nr.:
f:
U:
S:
N in
Fuse
100-115V: 4A(TH)
220-240V: 2A(TH)
WARNING - Fire Hazard -
For continued protection replace only
with the same type and rating of fuse
RS 232
Pt 100
1212 1313 1414 1515 1616 1717 1818
Fig. 3: Rear of the 763 PVC Thermomat
2
763 PVC Thermomat4
1212 Mains switch
to switch instrument on and off:
I = ON 0 = OFF
1313 Mains connection plug
mains connection, see section 2.3
1414 Fuse holder
changing the fuses, see section 2.3
1515 Model plate
indicating mains voltage and serial
number
1616 PC connection
RS232 interface
1.3 Operating elements
1717 Pt100 connection
Connection for external temperature
sensor
1818 Connection "N2 in"
1919 Gas supply connection
for connection tubing 66
2020 Electrode connection
for measuring vessel cover 55
2121 Mounting
for 6.2757.000 Exhaust collection tube
(option)
763 PVC Thermomat 5
1 Introduction
1.4 Information about these Instructions for Use
Please read through these Instructions for Use carefully before you put
the 763 PVC Thermomat into operation. The Instructions for Use
contain information and warnings to which the user must pay attention
in order to assure safe operation of the instrument.
1.4.1 Organization
These 8.763.1003 Instructions for Use for the 763 PVC Thermomat
provide a comprehensive overview of the installation, startup procedure, operation, fault rectification and technical specifications of this instrument. The Instructions for Use are organized as follows:
Section 1 Introduction
Measuring method, description of instrument,
operating elements and safety notes
Section 2 Installation
Installation of accessories, mains connection,
connection to PC
Section 3 Operating tutorial
Introduction to the operation using an example
Section 4 Operation
Detailed description of the operation
Section 5 Maintenance – Faults
Maintenance, fault display and fault rectification
Section 6 Appendix
Technical data, standard equipment, options, warranty, declarations of conformity, index
To find the required information on the instruments, you will find it an
advantage to use either the Table of contents or the Index at the
back.
You will find additional information on the PVC Thermomat method in
the relevant "Application Bulletins", which are available on request
free of charge from your Metrohm agency, as well as in the
"Application Notes" concerning the PVC Thermomat method, which
can be downloaded from the Internet under «www.metrohm.ch».
763 PVC Thermomat6
1.4.2 Notation and pictograms
The following notations and pictograms (symbols) are used in these Instructions for Use:
Range Menu item, parameter or
763 PVC THERMOMAT RESULTS Program window
<OK> Button
[ Ctrl ] Key
3535 Operating element of 763
1.4 Information about these Instructions for Use
entry value
Hazard
This symbol draws attention to a
possible danger to life or of injury if
the associated directions are not
followed correctly.
Warning
This symbol draws attention to
possible damage to instruments or
instrument parts if the associated
directions are not followed correctly.
Caution
This symbol marks important information. First read the associated
directions before you continue.
Comment
This symbol marks additional information and tips.
763 PVC Thermomat 7
1 Introduction
1.5 Safety notes
1.5.1 Electrical safety
While electrical safety in the handling of the 763 PVC Thermomat is assured in the context of the specifications IEC 1010-1 (protection class 1,
degree of protection IP20), the following points should be noted:
• Mains connection
Setting of the mains voltage, checking the mains fuse and the
mains connection must be effected in accordance with the instruc-
tions in section 2.3.
• Opening the 763 PVC Thermomat
If the 763 PVC Thermomat is connected to the power supply, the
instrument must not be opened nor must parts be removed from it,
otherwise there is a danger of coming into contact with components
which are live. Hence, always disconnect the instrument from all
voltage sources before you open it and ensure that the mains cable
is disconnected from mains connection 1313 !
• Protection against static charges
Electronic components are sensitive to static charging and can be
destroyed by discharges. Before you touch any of the components
inside the 763 PVC Thermomat, you should earth yourself and any
tools you are using by touching an earthed object (e.g. housing of the
instrument or a radiator) to eliminate any static charges which exist.
1.5.2 General precautionary rules
• Take care with hot reaction vessels
Avoid any contact with hot reaction vessels. Place them in the supplied vessel holder to cool them down.
763 PVC Thermomat8
2 Installation
2.1 Setting up the instrument
2.1.1 Packaging
The 763 PVC Thermomat is supplied together with the separately
packed accessories in special packaging containing shock-absorbing
foam linings designed to provide excellent protection. The instrument
itself is packed in an evacuated polyethylene bag to prevent the ingress
of dust. Please store all these special packaging as only they assure
transport of the instrument free from damage.
2.1.2 Check
2.1 Setting up the instrument
2.1.3 Location
After receipt, immediately check whether the shipment is complete and
has arrived without damage (compare with delivery note and list of
accessories in section 6.2). In the case of transport damage, see
instructions in section 6.4.1 "Warranty".
Position the instrument in the laboratory at a location convenient for operation, free from vibrations and protected against a corrosive atmosphere and contamination by chemicals. It is advisable to set up the instrument in a fume cupboard to guard against odor emission, but the
PC can be positioned outside on the regular laboratory bench.
In order to improve accessibility to the measuring places the instrument can also be placed on the 6.2059.000 Rotation ring, which is
available as an option.
763 PVC Thermomat 9
2 Installation
2.2 Attaching the accessories
2.2.1 Accessories for external gas supply
Nitrogen (N2) is required for external gas supply to the 763 PVC Thermomat. The following accessories must be mounted on the rear panel
of the PVC Thermomat:
1 Fitting the connecting tubing
• Screw one end of connecting tubing 6.1805.030 (150 cm)
onto connection 1818 "N2 in" on the rear panel of the PVC
Thermomat (see Fig. 3).
• Screw the 6.1808.020 connection piece onto the other end of
connecting tubing 6.1805.030.
2 Connect up gas supply
• Attach the gas supply from the cylinder containing nitrogen to
the tubing nozzle of 6.1808.020 Connection piece.
• Set gas pressure at the nitrogen cylinder to ca. 1.5 bar using
the reducing valve.
2.2.2 Reaction and measuring vessels
Fig. 4 shows the details of how the accessories for measuring the thermal stability are to be attached and connected to each other. Proceed
as follows:
1 Fitting the measuring vessel cover
• Insert PTFE tube 2727 from above into opening 2424 "In" of
measuring vessel cover 55.
• Screw connection piece 2222 into opening 24 24 of measuring
vessel cover 55.
2 Inserting the measuring vessel in the instrument
• Fill 60 mL dist. water into measuring vessel 44.
• Place measuring vessel cover 55 on measuring vessel 44.
• Insert measuring vessel 44 with attached measuring vessel
cover 55 into the opening provided for it on the 763 PVC
Thermomat and connect measuring vessel cover 55 with con-
nection plug 2626 to electrode connection 2020 (see Fig. 3).
3 Fitting the reaction vessel
• Insert gas inlet tube 3232 from below into connection 3434 of
reaction vessel cover 22.
• Push sealing ring 3333 over the upper end of gas inlet tube 3232.
• Screw connection nipple 3030 loosely into connection 3434 and
press gas inlet tube 3232 against connection nipple 3030 from
below; then fix gas inlet tube 3232 to reaction vessel cover 22 by
firmly tightening connection nipple 3030.
763 PVC Thermomat10
2.2 Attaching the accessories
• Place reaction vessel cover 22 on reaction vessel 11.
• Connect the white connecting tubing 33 to connection 3131 of
reaction vessel cover 22 (see Fig. 3).
4 Inserting the reaction vessel into the instrument
• Place the sample in the reaction vessel (see section 4.6.2).
• When the required temperature has been reached insert
reaction vessel 11 with attached reaction vessel cover 22 in the
openings provided for it on the 763 PVC Thermomat.
5 Making the tubing connections
• Connect the white connecting tubing 3 3 attached to reaction
vessel cover 22 to connection piece 2222 of measuring vessel
cover 55.
• Screw one end of brown connecting tubing 66 to connection
nipple 3030 of reaction vessel cover 22.
• Screw the other end of brown connecting tubing 66 to the
corresponding connection 1919 on the 763 PVC Thermomat
(see Fig. 3).
The 6.1428.020 transparent glass measuring vessel
available as an option can be used instead of the
6.1428.100 polycarbonate measuring vessel; in
contrast to the polycarbonate vessel this can be
cleaned with acetone.
2.2.3 Exhaust collection tube (option)
For selective exhaust lead off the 6.2757.000 Exhaust collection
tube available as an option can be fitted to the 763 PVC Thermomat. In
addition to the exhaust collection tube 8 x 6.1816.010 Silicone tubing
(22 cm) must also be ordered. Attach the exhaust collection tube as
described below:
1 Positioning the exhaust collection tube
• Place the exhaust collection tube with the two supports in the
two mountings 2121 (see Fig. 3) on the 763 PVC Thermomat so
that the connection for leading off the exhaust is located to
the rear.
2 Connecting the measuring vessel
• Screw a connection piece 2222 into opening 2323 of the measur-
ing vessel cover 55.
763 PVC Thermomat 11
2 Installation
66
3030
3131
3232
3333
3434
33
2222
2323
2424
2525
2626
55
22
2727
2828
2929
11
44
Fig. 4: Installation of reaction and measuring vessels
11 Reaction vessel (6.1429.040) 2626 Connection plug
22 Reaction vessel cover (6.2753.100) 2727 PTFE tube (6.1819.080)
for air supply into measuring vessel
33 Connecting tubing (6.1816.010) 2828 Electrodes
44 Measuring vessel (6.1428.100) 2929 Protective ring (4.422.0520)
55 Measuring vessel cover (6.0913.130)
with built-in conductivity measuring cell
66 Connecting tubing (6.1805.080)
for gas supply to reaction vessel
2222 Connection piece (6.1808.050) 3232 Gas inlet tube (6.2418.110)
2323 Opening "Out"
for measuring vessel exhaust
2424 Opening "In"
for measuring vessel inlet
3030 Connection nipple (6.1808.090)
3131 Connection
for connecting tubing 33
3333 Sealing ring (6.1454.040)
3434 Connection
for connection nipple 3030
2525 Marking field
for entering the cell constant
763 PVC Thermomat12
• Connect one end of the 6.1816.010 Silicone tubing to connection piece 2222.
• Plug the other end of the 6.1816.010 Silicone tubing into the
corresponding exhaust collection tube opening.
• Close the unused openings on the exhaust collection tube
with the included E.400.0010 stoppers.
3 Connecting the exhaust collection tube
• Attach a piece of suitable tubing to the exhaust collection
tube connection and connect it to an active aspirating device
(e.g. water-jet pump).
2.3 Mains connection
2.3 Mains connection
Follow the instructions below for connecting to the power supply. If
the instrument is operated with a mains voltage set wrongly and/or
wrong mains fuse, there is a danger of fire!
2.3.1 Checking the mains voltage
Before switching on the 763 PVC Thermomat for the first time, check
that the mains voltage indicated on the model plate 1515 (see Fig. 3)
matches the local mains voltage. If this is not the case, call the
Metrohm service.
2.3.2 Exchange of fuses
Two fuses 4 A/slow-blow for 115 V or 2 A/slow-blow for 230 V are installed in fuse holder 1414 of the 763 PVC Thermomat as standard.
Ensure that the instrument is never put into operation with fuses of
another type, otherwise there is danger of fire!
For changing fuses, proceed as follows:
1 Disconnect mains cable
Disconnect mains cable from mains connection plug 1313 of the
763 PVC Thermomat.
2 Remove fuse holder
Using a screwdriver, loosen fuse holder 1414 above the mains
connection plug 1313 and take out completely.
763 PVC Thermomat 13
2 Installation
3 Change fuses
Remove old fuses carefully from fuse holder 1414 and replace
them with two new fuses which are suitable for the set mains
voltage, type TH (slow-blow, with high switching capacity):
115 V 4 A (TH) Metrohm-No. U.600.0022
230 V 2 A (TH) Metrohm-No. U.600.0107
4 Install fuse holder
Push fuse holder 1414 back into the instrument until it clicks into
position.
2.3.3 Mains cable and mains connection
Mains cable
The instrument is supplied with one of three mains cables
• 6.2122.020 with plug SEV 12 (Switzerland, …)
• 6.2122.040 with plug CEE(7), VII (Germany, …)
• 6.2133.070 with plug NEMA 5-15 (USA, …)
which are three-cored and fitted with a plug with an earthing pin. If a
different plug has to be fitted, the yellow/green lead (IEC standard)
must be connected to protective earth (protection class 1).
Any break in the earthing inside or outside the instrument can make it
a hazard!
Mains connection
Plug the mains cable into mains connection plug 1313 of the 763 PVC
Thermomat (see Fig. 3).
2.3.4 Switching the instrument on/off
The 763 PVC Thermomat is switched on and off using mains switch 1212.
When the instrument is switched on, the mains pilot lamp 77 "ON" (see
Fig. 2) lights up.
763 PVC Thermomat14
2.4 Connection to the PC
2.4.1 Connection PVC Thermomat – PC
Always switch off 763 PVC Thermomat and PC before you connect the
two instruments with the 6.2134.100 Cable.
The PC program «763 PVC Thermomat» allows a maximum of 4 PVC
Thermomats to be controlled. The following possibilities exist for connecting these PVC Thermomats to serial PC interfaces:
• Connection to built-in COM interfaces on the PC
• Connection to an additional built-in interface extension board
• Connection to a softswitch (order number: 2.145.0014 for 230 V,
2.145.0015 for 115 V) which is connected to one of the COM interfaces.
Connect the PC connection 1616 at the 763 PVC Thermomat to one of the
serial COM ports at the PC or to a softswitch using the 6.2134.100 Cable (9 pin/9 pin). If only a 25-pin COM interface is available on the PC
then the 6.2125.110 Adapter cable or a commercially available adapter
must be used.
2.4 Connection to the PC
2.4.2 Software installation
The PC program «763 PVC Thermomat 1.0» is required for the operation of the 763 PVC Thermomat; this is contained on the 6.6037.000
CD included in the accessories. This program runs under Windows NT
(recommended, especially if several instruments are connected), Windows 95 and Windows 98 operating systems and is installed as follows:
1 Install program
• For Windows NT: log in as operator with administrator rights.
• Insert 6.6037.000 Installation CD into CD drive.
• Select <Start> and Run. Browse for the setup.exe file on the
installation CD and click on <OK>.
• Click on "763" and follow the instructions given in the setup
program.
The software package will be installed in the desired directory. In addition to the program files, the following folders are
installed:
Database Folder for database files (*.mrd)
Log Folder for event log files (*.mel) and temperature
Template Folder with empty database (Default.mrd) and
recording files (*.txt)
copy of the result program (Nachaus.prg)
2 Registration
• Please send us your 8.763.8007 Registration card as soon as
possible.
763 PVC Thermomat 15
2 Installation
2.4.3 Basic settings
When the program is started for the first time several basic settings
must be made for the 763 PVC Thermomat. Proceed as follows:
1 Switch on instruments
2 Start program and login
• Check if the PVC Thermomat has been connected correctly to
the PC (see section 2.4.1).
• Switch on the PVC Thermomat using mains switch 1212.
• Switch on the PC.
• Double-click the software icon to start the program. The
program window with the opening picture is opened and the
Login window appears on the screen:
• Do not enter any password here, just click on <Change pass-
word>. The following window appears:
• Leave the Old password field empty. Under New password enter
the required password which will in future allow you to log in
as Administrator. Confirm the new password by renewed entry
in the Confirm new password field and click on <OK>.
• Enter the new Password again in the Login window. You are
now logged in as Administrator.
• Confirm the message There are no units configured yet with
<OK>. The 763 PVC THERMOMAT CONTROL window appears.
763 PVC Thermomat16
2.4 Connection to the PC
3 Communication settings
• Click on 763 PVC THERMOMAT CONTROL / Options / Communica-
tion to open the Select number of units window:
• Enter the number of PVC Thermomats (1…4) connected to
the PC and click on <OK>. The Unit configuration window appears:
• Under COM port select for each instrument the number of the
serial interface (1…8) to which this instrument is connected. If
a softswitch is used then the option Softswitch in use must be
switched on. Under COM port the number of the serial interface to which the softswitch is connected is selected; under
Softswitch port the number of the interface on the softswitch to
which the instrument is connected is selected.
• Click on <OK> to close the Unit configuration window.
• Confirm the message which then appears with <OK>.
4 Close the program and start it up again
• Close the program with 763 PVC THERMOMAT CONTROL / File /
Exit.
• Restart the «PVC Thermomat 1.0» program by double-
clicking the program icon.
• In the Login window enter the Password for the administrator.
The control window appears. In the status line the message
Unit#: Ready should appear for all connected instruments.
763 PVC Thermomat 17
2 Installation
763 PVC Thermomat18
3 Operating tutorial
This section introduces you to the operation of the 763 PVC Thermomat by means of a brief operating tutorial which describes the basic
operating steps needed for performing determinations and display of
results.
For further explanations of the operation, please refer to section 4.
3.1 Determinations
3.1 Determinations
The determination of induction and stability time of a PVC sample at
200 °C and a gas flow of 7 L/h is used an illustrative example. Please
note that the steps and parameter settings described apply only to
this example. If you use a different sample and different parameters,
the procedures described in the tutorial must be modified appropriately.
3.1.1 Installation
Before you start this brief tutorial, the 763 PVC Thermomat must be
correctly installed as described in section 2. In what follows, the most
important points for the installation are listed once again (for details,
see the sections mentioned).
⇒ Setting up instrument section 2.1
⇒ Installing air supply accessories section 2.2.1
⇒ Installing reaction and measuring vessels section 2.2.2
⇒ Mains connection section 2.3
⇒ Connection to PC section 2.4
763 PVC Thermomat 19
3 Operating tutorial
3.1.2 Preparing for determinations
Before starting determinations, the method must be selected, the
heating must be started and the reaction and measuring vessels must
be prepared. Proceed as follows:
1 Switch on 763 PVC Thermomat
⇒ Switch on 763 PVC Thermomat with mains switch 1212 on the
rear of the instrument. After the instrument has been switched
on the mains pilot lamp 77 lights up.
2 Switch on PC
⇒ Switch on PC and start «763 PVC Thermomat» program.
3 Select method "Default"
⇒ In the opened control window, select the determination
method Default for Block A (and – if more than 4 samples are
to be determined – also for Block B) in the Method field.
⇒ Click on , if you want to change the parameters of the
default method (details see section 4.5.2).
The determinations described in this tutorial have been
carried out using the default settings (Temperature = 200 °C,
Delta T = 0.6 °C, Gas flow = 7 L/h, etc.).
4 Start heating
⇒ To start the heating of Block A and – if desired – of Block B
click on the following button:
As soon as the heating is switched on the color of the frame
of this button switches to red. At the same time the temperature display 99 "TEMPERATURE" LED on the 763 PVC Ther-
momat starts to blink for the selected block.
The actual temperature is shown digitally beside the button. A
bar below shows the absolute variation of the actual temperature from the target temperature; the bar length corresponds to 50 °C.
763 PVC Thermomat20
3.1 Determinations
5 Prepare measuring vessels
⇒ Clean the used measuring vessels and their covers (details
see section 4.6.3).
⇒ Fill each cleaned measuring vessel 4 4 with 60 mL distilled
water.
⇒ Place the measuring vessel cover 55 fitted with a PTFE tube
2727 on the measuring vessel 44 (see Fig. 4).
⇒ Place the measuring vessel 44 with its cover 55 in one of the
openings provided for it on the 763 PVC Thermomat and
connect the electrode plug 2626 on the cover to the corre-
sponding socket 2020 on the 763 PVC Thermomat.
6 Prepare reaction vessels
⇒ Weigh out 0.5 g PVC into the reaction vessels 1.
⇒ Take the upper rim of the reaction vessel 1 in your hand (e.g.
in the space between thumb and index finger) and rotate the
glass though 360°. This provides the degreased glass with a
thin grease film, without which it is very difficult to remove the
cover from the vessel after the determination.
⇒ Insert an gas inlet tube 32 into the reaction vessel cover 2
and fasten it by screwing down the connection nipple 30 (see
Fig. 4).
⇒ Place the reaction vessel cover 2 on the reaction vessel 1.
Rotate the cover so that the air inlet tube 32 is as close as
possible to the vessel wall.
⇒ Fasten the white connecting tubing 3 on to the connection 31
of the reaction vessel cover 2.
⇒ Place the prepared reaction vessel into the vessel holder.
7 Enter sample identifiers
⇒ Enter the sample identifiers ID1 and ID2 in the corresponding
fields of the operating area in the control window.
763 PVC Thermomat 21
3 Operating tutorial
3.1.3 Carrying out determinations
When the preparations are complete the determinations can be started.
Proceed as follows:
1 Wait until the temperature has been reached
⇒ Wait until the heating block reaches the temperature defined
in the method. This condition is indicated by temperature display 99 "TEMPERATURE" which stops blinking and remains
lit up. At the same time or after a slight delay the frame color
of the <Heat to...> button turns green.
2 Insert reaction vessels
⇒ Place the prepared reaction vessels 11 in the heating block
openings on the 763 PVC Thermomat. Close any openings
which are not used with stoppers or empty reactions vessels
to protect against contamination.
⇒ Connect the white connecting tubing 33 fastened to the reac-
tion vessel cover 22 to the corresponding connection 2222 on
the measuring vessel cover 55.
⇒ Screw the brown gas supply tubing 66 onto the connection
nipple 3030 of the reaction vessel cover 22 and the correspond-
ing connection 1919 on the 763 PVC Thermomat (see Fig. 3).
3 Start determination
⇒ In the operating field of the control window for every determi-
nation you want to start you must click on the button
.
After the start of a determination the live curve of the started
determination is shown in the operating window beside the
channel number. The actual measured value appears above
the curve.
As soon as a point of inflection is found during the measurement the determination is terminated. The window with the
live curve becomes gray again and the message finished appears.
763 PVC Thermomat22
4 Automatic report output
GLP test passed.
At the end of the determination the report defined in the
method is printed out automatically.
3.1 Determinations
Unit
Block
Channel
1
A
1
ID 1
PVC
Induction time
Stability time
Standard time
200
175
150
125
100
µS/cm
75
50
25
Serial number
Cell constant
User
01109
1
Administrator
1.27
1.33
6.45
h
h
h
Druckdatum
Bestimmungsdatum
ID 2
KA356
Delta Kappa
(F: 2.254; T: 180°C)
09.09.1999 09:34:03
23.06.1999 13:25:52
50 µS/cm
1.27
1.33
0
0.00 0.25 0.50 0.75 1.00 1.25 1.50
Method name
Creator
Temperature
Delta T
Gas flow
Start delay
Start mode
PVC 200°C
Administrator
per channel
200
0.60 °C
7°CL/h
0
min
per 2 channels
per block
h
Creation date
Stop time
Stop at conductivity
Stopat endpoint
Delta Kappa
Evaluation delay
Evaluation suppression start
Evaluation suppression end
Send to file
23.06.1999 08:27:20
0.00
h
200
µS/cm
50
µS/cm
0.00
h
0.00
h
0.00
h
763 PVC Thermomat 23
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