Metrohm 763PVC User Manual

Download

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.

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

1010

1111

763 PVC Thermomat

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.:

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

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

3030

3131 3232

3333

3434

2222

2323 2424

2525

2626

2727

2828

2929

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

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

• 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

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

Serial number Cell constant User

01109 1 Administrator

1.27

1.33

6.45

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

0.00 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

min

per 2 channels per block

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

200

µS/cm

0.00

763 PVC Thermomat 23

3 Operating tutorial

3.2 Results

The demo database Demo.mrd is used as an example for the display and further processing of the results of recorded determinations. Please note that the steps and parameter settings described apply only to this database. If you use a different database, the procedures described in the tutorial must be modified appropriately.

3.2.1 Determination overview

The determination overview displays an overview table with selected data fields of all the determinations contained in the opened database.

1 Open database "demo.mrd"

⇒ Click on or File / Results in the control window in order to

open the 763 PVC THERMOMAT RESULTS window. This loads the Repos.mrd database and opens the determination overview as standard.

⇒ Click on File / Open database in the results window. Select the

demo.mrd database in the Open database window and click on <Open>. A sub-window opens in the results window which

shows the data from 5 determinations in an overview table.

2 Format determination overview

⇒ Select fields: Click on or Format / Select fields in the

results window. In the Display fields window move the fields until the fields required for the determination overview are visible in the Display field and then click on <OK>.

⇒ Adjust field width: Mark the column in the determination

overview whose width is to be altered. Click on Format / Adjust

width in the results window. Enter the column width in the Column width window or click on <Best fit> in order to automati-

cally adapt the column width to the longest field contents. Alternatively the column width can also be set directly by using the mouse. This is done by moving the cursor between two columns in the title line of the table until it appears as . The column can now be pulled to the required width with the left-hand mouse key pressed down. A double-click on the

763 PVC Thermomat24

selected column automatically adapts the column width to the longest field contents (including title).

⇒ Format fields: Click on Format / Fields in the results window.

Set down the format for the fields in the determination overview in the Cells effects window and click on <OK>.

⇒ Select fonts: Click on Format / Fonts in the results window.

Select the font to be used in the determination overview in the

Font window and click on <OK>.

⇒ Save settings: Click on Options / Save settings now to save

the new format of the determination overview permanently.

3 Print determination overview

⇒ Click on or File / Print in the results window to open the

Printing of window.

3.2 Results

⇒ Select Overview table if the determination overview is to be

printed out in tabular form.

⇒ Select Overview list if the determination overview is to be

printed out as a list with all the fields selected in the determination overview.

⇒ Click on <Print>. ⇒ In the Print window select the printer, printing area and num-

ber of copies and click on <Print>.

763 PVC Thermomat 25

3 Operating tutorial

4 Export determination overview

⇒ Copy to clipboard: Mark the lines or columns in the deter-

mination overview which are to be copied. Click on or

Edit / Copy. The marked texts are loaded into the clipboard

from where they can be further processed with other programs.

⇒ Export to other database: Mark the determinations (lines)

which are to be exported in the determination overview. Click on Determination / Export / Export to database. In the Export data

to... window select the database to which the determinations

are to be exported and click on <Save>.

⇒ Export to Word: Mark the lines or columns in the determina-

tion overview which are to be exported. Click on or De-

termination / Export / Export to MS Word. The marked texts are

loaded into an RTF file which is automatically opened with Microsoft Word.

⇒ Export to Excel: Mark the lines or columns in the determina-

tion overview which are to be exported. Click on or De-

termination / Export / Export to MS Excel. The marked texts are

loaded into an XLS file which is automatically opened with Microsoft Excel.

3.2.2 Determination and method data

All the determination and method data of each determination in a determination overview can be shown, printed out and exported.

1 Display determination and method data

⇒ In the opened determination overview mark the determination

for which all parameters and results are to be displayed.

⇒ Click on or View / Determination and method data in the

results window or double-click on the required line in the determination overview. The Determination and method data window opens in which the data are shown on several register cards.

763 PVC Thermomat26

3.2 Results

2 Print determination and method data

⇒ Click on or File / Print in the results window to open the

Printing of window (see section 3.2.1).

⇒ Select the All determination and method data option. ⇒ Click on <Print>. ⇒ In the Print window select the printer, printing area and num-

ber of copies and click on <Print>.

3 Export determination and method data

⇒ Mark the determinations (lines) in the determination overview

from which all data is to be exported.

⇒ Click on or Determination / Export / Determination and

method data.

⇒ In the Save to export file window select the required folder and

the file name of the *.txt export file under which the data are to be stored and click on <Save>.

763 PVC Thermomat 27

3 Operating tutorial

3.2.3 Graphics

Curves for each determination in a determination overview can be shown, printed out and copied.

1 Open single graph

⇒ Mark the determination in the determination overview whose

single curve is to be displayed.

⇒ Click on or Determination / Graphics / Single graph in the

results window. A new window is opened in which the single graph for the determination selected in the determination overview is shown. The sample identifiers ID 1 and ID 2 are shown in the window title. If present then the determined In-

duction time (red vertical line and numbers) and Stability time

(black vertical line and numbers) will be shown in the graphics window as well as the measuring curve (green).

2 Open multiple graph

⇒ Mark the determinations in the determination overview whose

curves are to be displayed in a multiple graph.

⇒ Click on or Determination / Graphics / Multiple graph in the

results window. A new window is opened in which all curves for the determinations marked in the determination overview are shown. The individual measuring curves are shown in color, the legends referring to the colors (ID 1 and ID 2) are located in the graph header. If present the determined Induc-

tion time ( ) and Stability time ( ) will also be shown.

763 PVC Thermomat28

3 Open live graph

⇒ Mark the determination in the determination overview whose

curve is to be displayed.

3.2 Results

⇒ Click on or Determination / Graphics / Live graph with

reevaluation in the results window. A new window is opened in

which the measuring curve of the marked determination is shown. If a different determination is marked in the determination overview then the curve is automatically updated. If present then the determined Induction time (red vertical line and numbers) and Stability time (black vertical line and numbers) will be shown in the graphics window as well as the measuring curve (green). With <2nd derivative> the second derivative of the measuring curve can be shown as a blue line. The live graph offers the possibility of the manual ree-

valuation of the measuring curves (see section 4.7.3).

763 PVC Thermomat 29

3 Operating tutorial

4 Print graphics

⇒ Open the required graph in the results window which is to be

printed.

⇒ Click on or File / Print in the results window. The curve

shown in the active graph window will be printed out.

⇒ If you want to print several single or multiple curves at the

same time first mark the required determinations in the determination overview. Click on or File / Print (see sec-

tion 3.2.1). In the Printing of... window select the option Single

graph or Multiple graph and click on <Print>.

5 Copy graphics

⇒ Open the required graph in the results window which is to be

copied.

⇒ Use the right-hand mouse key to click on the graph window

and select the option Copy in the context-sensitive menu. The selected curve is copied into the clipboard where it can be further processed with other programs.

763 PVC Thermomat30

4.1 Fundamentals of the operation

4 Operation

This section describes the most important points concerning the operation of the 763 PVC Thermomat. For further details please refer to the on-line help in the PC program which can provide you with the required information rapidly and conveniently from any place in the program.

4.1 Fundamentals of the operation

4.1.1 Starting/closing the program

Start the «763 PVC Thermomat» program

Start the program

Double-click this icon or the PvcTm.exe file to start the «763 PVC Thermomat 1.0» program. The Login window appears:

Select the desired User name and enter the Password. Then click on <OK>.

After software installation, the program can be started without entering a Password. For the definition of users, see section 4.2.2.

Close the «763 PVC Thermomat» program

763 PVC THERMOMAT CONTROL / File / Exit

Exit the «763 PVC Thermomat» program. The program is also quitted by clicking on in the upper right

part of the 763 PVC THERMOMAT CONTROL window.

763 PVC Thermomat 31

4 Operation

4.1.2 Glossary

Control window

Method

Determination

Results

The main window 763 PVC THERMOMAT CONTROL is known as the control window. It contains all the functions required for controlling the 763 PVC Thermomats connected to the PC.

A method includes all parameters for carrying out and evaluating a determination.

A determination is understood to be the automatic determination of the induction time and/or stability time of a sample. In order to carry out a determination a suitable method must be selected for the samples.

The results of a determination are automatically stored in the Repos.mrd database and can be observed in the results window.

Reevaluation

Reevaluation is the subsequent reprocessing of determinations, in particular the manual determination of the induction time with the aid of tangents.

Recalculation

Recalculation means that results, equations and standards can be calculated again at a later date.

Extrapolation

Extrapolation can be used to convert the results obtained at various temperatures to a required target temperature. In addition, this method can be used for converting the induction time to the standard time.

763 PVC Thermomat32

4.1.3 Control window

The 763 PVC THERMOMAT CONTROL window is used for controlling the PVC Thermomats, managing methods, displaying the live curves and accessing various program functions.

Open

The 763 PVC THERMOMAT CONTROL window is opened automatically when the program is started (see section 4.1.1).

Arrangement

The elements of the control window are the menu bar, the toolbar and the status bar, indicating prompts, the logged-in user and the instrument status. The operating area contains a diagram of the measuring unit of the 763 PVC Thermomat which can be used to start, display and stop determinations.

Window title Menu bar Toolbar

4.1 Fundamentals of the operation

Operating area

Status bar

Logged-in user Unit statusPrompt

Menus

The control window contains the following main menus:

File Management of method files, opening the results window,

printing, new log in.

View View of toolbar and status bar, unit information, live pa-

rameters, status overview, event log overview, unit selection.

763 PVC Thermomat 33

4 Operation

Tools Cell constants, GLP test, timer, gas flow control, start all

channels, determination of Delta T, temperature recording, service diagnosis.

Options General settings, instrument configuration, user permis-

sions.

Help Program-specific on-line help.

Icons

The following icons are displayed in the control window:

Create new method (see section 4.5.1). Open existing method (see section 4.5.1). Method manager (see section 4.5.1). Print results (see section 4.7.6).

Open results window (see section 4.1.4).

Live parameters, which can be altered during a run (see section 4.6.4).

Status overview of the connected instruments (see section 4.3.2).

Unit information (see section 4.3.1). Display GLP status (see section 4.8.3).

Select unit 1...4.

Start all channels of Block A (see section 4.6.4). Start all channels of Block B (see section 4.6.4).

Call up help.

The control window is closed by clicking on 763 PVC THERMOMAT CON-

TROL / File / Exit or in the upper right part of the window.

763 PVC Thermomat34

4.1.4 Results window

The 763 PVC THERMOMAT RESULTS window is used to display, output and recalculate the results of determinations recorded by the 763 PVC Thermomat. The determination data are stored in the *.mrd database files and can be shown in this window as an overview table and as curves. The results window can run even when the control window is closed.

Open

The 763 PVC THERMOMAT RESULTS window is opened by clicking on

or 763 PVC THERMOMAT CONTROL / File / Results in the control win-

dow.

Arrangement

The elements of the results window are the menu bar, the toolbar and the status bar. Within the results window sub-windows can be opened showing determination overviews, single, multiple and live graphs.

Window title Menu bar

Toolbar

4.1 Fundamentals of the operation

Determination overview

Single graph

Live graph

Multiple graph

Status bar

Menus

The results window contains the following main menus:

File Open database, print, close window. Edit Copy, mark, delete filter. View Select display: determination overview,

method and determination data, GLP.

763 PVC Thermomat 35

4 Operation

Determination Seek, sort, filter, graphics, extrapolation,

recalculation, export, delete.

Format Format determination overview. Options General program settings. Window Display of windows. Help Program-specific on-line help.

Icons

The following icons are shown in the results window:

Print results, curves and overview lists

Filter selection (see section 4.7.1).

(see section 4.7.6). Copy to clipboard

(see section 4.7.6). Select fields for determi-

nation overview

Selection not in filter (see section 4.7.1).

Single graph (see section 4.7.3).

(see section 4.7.1). Show determination

overview

Multiple graph (see section 4.7.3).

(see section 4.7.1). Show all method and

determination data (see section 4.7.2).

Single graph with possibility of reevaluation (see section 4.7.3).

Find (see section 4.7.1). Export to MS Word

(see section 4.7.6).

Sort ascending (see section 4.7.1).

Sort descending (see section 4.7.1).

Export to MS Excel (see section 4.7.6).

Export measured values (see section 4.7.6).

Selection based filter (see section 4.7.1).

Export determination and method data (see section 4.7.6).

Special filter/sorting (see section 4.7.1).

Apply filter/sorting (see section 4.7.1).

Remove filter/sorting

Tile windows vertically (see section 4.7.8).

Tile windows horizontally (see section 4.7.8).

Close results window.

(see section 4.7.1). Delete filter

(see section 4.7.1).

The results window is closed by clicking on or 763 PVC THERMO-

MAT RESULTS / File / Return.

763 PVC Thermomat36

4.1.5 Overview of file types

The following file types are produced by the «763 PVC Thermomat» program:

*.mrd Database file

Contains measuring data and results. *.mrd files are automatically stored in the Database folder.

*.mel Event log file

This file contains a protocol of all events which have occurred with the connected PVC Thermomats. *.mel files are automatically stored in the Log folder.

*.txt Measurement table file

Contains measurement tables in ASCII format. *.txt files are automatically stored in the Log folder.

4.1.6 Context-sensitive menus

4.1 Fundamentals of the operation

A lot of menu functions of the program window can also be selected by clicking the required window or element with the right-hand mouse key. The menu options which are then opened depend on the selected active window or element

4.1.7 Mouse functions

The mouse can be used to carry out the normal program operating functions such as the selection of menu items and fields. It can additionally be used for magnifying a section of a curve (zooming). To zoom a portion of the curve place the mouse cursor to the upper left corner of the square to zoom, press the left mouse button and drag the cursor to the lower right corner of the rectangle. After releasing of the left mouse button the selected region will be zoomed full-screen.

4.1.8 Help

By clicking on or Help / Help or by pressing the [ F1 ] key you can get on-line help on the current topic anywhere in the program.

Green texts can be clicked to jump to a different Help topic. Violet texts identify dialog items, parameters or buttons in

the corresponding window.

Blue texts Identify titles and important information.

763 PVC Thermomat 37

4 Operation

4.2 Instrument and software settings

4.2.1 Communication

763 PVC THERMOMAT CONTROL / Options / Communication

This menu item is used for the configuration of the communication between the PC and up to 4 connected 763 PVC Thermomats.

The Select number of units window appears first; the number of 763 PVC Thermomats connected to the PC must be entered here.

Then the Unit configuration window opens; the following parameters can be selected here for each instrument which is connected:

COM port Selects the COM port (1...8) to which the in-

strument or the softswitch is connected.

Softswitch

Softswitch in use Use a softswitch between PC and instrument. Softswitch port Selects the port (1...4) on the softswitch to

which the instrument is connected.

Two softswitches are available as options from Metrohm: 2.145.0014 (for 230 V) or 2.145.0015 (for 115 V). 4 PVC Thermomats can be connected to a softswitch.

763 PVC Thermomat38

4.2.2 User permissions

The «763 PVC Thermomat» program is equipped with a comprehensive password protection system which allows each menu item to be individually provided with access rights. The access rights are issued for various groups. The individual user can then be assigned to a group

763 PVC THERMOMAT CONTROL / Options / User permissions

This menu item is used to issue access rights and is reserved for the

Administrator only. The Users and groups manager window opens in which

the already defined groups with their users are listed.

4.2 Instrument and software settings

The following menu items are available by clicking on the entries with the right-hand mouse key.

Functions for groups

Add user Adds a new user to the selected group. The

name of the new user must be entered in the

Enter new user name window.

Add group Adds a new group to the previous groups. The

name of the new group must be entered in the

Enter new group name window. Delete group Deletes the selected group. Properties The Group permissions window opens in which

access to all program functions can be

switched on or off individually.

763 PVC Thermomat 39

4 Operation

Functions for users

Delete user Deletes the selected user.

It is recommended to make user lists and enter passwords as a first action after software installation.

The Administrator is not included in the list of operators but possesses all rights of access and cannot be deleted.

After configuration of user permissions the program prompts for the selection of the user name and entry of the password in the Login window every time the program starts. The user name stamps all methods, determinations and reports. It is possible at any time to change the user with the menu item 763 PVC THERMOMAT CONTROL / File / New login.

763 PVC Thermomat40

4.2.3 Timer

763 PVC THERMOMAT CONTROL / Tools / Timer function...

4.2 Instrument and software settings

The Automatic heater start window opens in which the automatic start of heating at a predetermined time can be entered independently for block A or block B.

Start heater

Never No automatic start of heating. Once Automatic start of heating at the time defined in

Daily Automatic start of heating on the day selected

<Which days> This button opens the Select days window in

Start at... If Once has been selected then the time and

4.2.4 Gas flow control

The flow of gas through the reaction vessels to the measuring vessels can be switched on and off manually and shown in a separate window.

the Start at... field.

in the <Which days> field at the time defined in

the Start at... field.

which the required day can be selected.

date for the automatic start of heating can be

entered, if Daily has been selected the time.

763 PVC THERMOMAT CONTROL / Tools / Gas flow control / Gas flow on

Switches on gas flow.

763 PVC THERMOMAT CONTROL / Tools / Gas flow control / Gas flow off

Switches off gas flow.

763 PVC Thermomat 41

4 Operation

763 PVC THERMOMAT CONTROL / Tools / Gas flow control / Display gas flow...

The Gas flow display window opens in which the actual gas flow is shown. This function is only available if no determination is running.

4.2.5 Recording temperature

763 PVC THERMOMAT CONTROL / Tools / Temp. logging / Block A on

Switches on temperature recording for block A and external temperature sensor.

763 PVC THERMOMAT CONTROL / Tools / Temp. logging / Block A off

Switches off temperature recording for block A and external temperature sensor.

763 PVC THERMOMAT CONTROL / Tools / Temp. logging / Block B on

Switches on temperature recording for block B and external temperature sensor.

763 PVC THERMOMAT CONTROL / Tools / Temp. logging / Block B off

Switches off temperature recording for block B and external temperature sensor.

The temperature can be individually recorded at any time for each heating block. The measured values are written in a text file which contains the following values:

t(s) Time in s Block [°C] Measured temperature in heating block Ext. Sensor [°C] Measured temperature with the external tem-

perature sensor

The text file is stored under the name U#X-YYMMDD-HHMMSS.txt in the folder Log; # stands for the instrument number (1...4), X for the block (A or B) and YYMMDD-HHMMSS for the date and time of the start of data recording.

763 PVC Thermomat42

4.2.6 Options

Save settings

763 PVC THERMOMAT CONTROL / Options / Save settings on exit

763 PVC THERMOMAT CONTROL / Options / Save settings now

Clear sample ID1 history

763 PVC THERMOMAT CONTROL / Options / Clear sample ID history

4.2 Instrument and software settings

The program and window settings can be saved with the two following menu items:

If this option is switched on then the current program and window settings will be automatically saved each time the program is shut down.

The current program and window settings will be saved immediately.

This menu item is used to delete the list automatically formed from the entered sample identifiers ID1.

763 PVC Thermomat 43

4 Operation

4.3 Program information

4.3.1 Unit information

763 PVC THERMOMAT CONTROL / View / Unit information

The Unit information and Service diagnosis window opens.

Serial number Serial number of the selected 763 PVC Ther-

momat.

Program number Number of the EEPROM program of the se-

lected 763 PVC Thermomat.

Last maintenance Date of the last maintenance with the signature

of the service technician who carried out the maintenance work.

Last calibration Date of the last adjustment with signature and

code of the office which carried it out.

Unit operating hours Number of hours that the instrument has been

switched on.

Pump operating hours Number of hours that the gas flow has been

switched on.

<Print report> Print out unit information report.

The Service Diagnosis block is password-protected and is only accessible to trained service personnel.

763 PVC Thermomat44

4.3.2 Status overview

763 PVC THERMOMAT CONTROL / View / Status overview

The STATUS - 763 PVC THERMOMAT CONTROL window opens and displays an overview of all available channels of the instruments connected to the PC.

4.3 Program information

This window contains the following columns:

Unit Instrument number (1...4).

Block Instrument block (A, B).

Channel Channel (1...4).

Method Method name.

Sample ID1 Sample identifier 1.

Status Status of channel:

ready No active measurement. The channel is ready

for the start of a determination.

running Running measurement. finished Determination finished. The channel is ready for

the start of a new determination.

error Communication error between instrument and

PC.

Stab. time Determined stability time.

Induc. time Determined induction time.

Set temp. Set temperature defined in method.

Current temp. Actual block temperature.

The width of the columns in the STATUS - 763 PVC THERMOMAT CONTROL window can be altered by pulling the right-hand field margin of the column title with the mouse. These settings together with the window size and window position can be permanently stored with 763 PVC THERMO-

MAT CONTROL / Options / Save settings now.

763 PVC Thermomat 45

4 Operation

4.3.3 Events overview

Event window

763 PVC THERMOMAT CONTROL / View / Event log overview

The PVCTM.MEL - MLOGVIEW window opens in which an overview of all the events concerning the 763 PVC Thermomats connected to the PC is displayed.

This window contains the following columns:

Type Type of event:

Information about an event which has taken place properly.

Warning about a special event. Error message about the faulty event.

Date Date of the event. The format depends on the

settings defined under Regional Settings / Date in Windows.

Time Time of the event. The format depends on the

settings defined under Regional Settings / Time in Windows.

User Name of the operator logged in when the event

occurred.

Unit Instrument number(1...4).

Event Description of the event.

763 PVC Thermomat46

Menus

The events window contains the following main menus:

File Open and save event log files. View View toolbar and status bar, update. Filter Filter the events. Help Program-specific on-line help.

Icons

The following icons are shown in the events window:

Open existing event log file (*.mel).

Save event log file as text file (*.mel).

Update event overview.

4.3 Program information

Selection-based filter.

Remove filter.

Filter

PVCTM.MEL - MLOGVIEW / Filter / Selection based filter

The selection-based filter is a method for filtering records rapidly and conveniently. This is done by first marking an entry in a field in the determination overview. After activating the selection-based filter the table is filtered so that only records which contain the marked entry are shown.

PVCTM.MEL - MLOGVIEW / Filter / Remove filter

The filter used on the event overview is removed and all events are shown again.

Parameter for event recording

763 PVC THERMOMAT CONTROL / Options / Event log

The Log settings window opens:

Delete entries older than...

Number of days before events are automati-

cally deleted.

Range: 1 ... 365

763 PVC Thermomat 47

4 Operation

4.4 Calibration functions

4.4.1 Determination of cell constants

As in PVC Thermomat measurements only the alterations in the conductivity are measured and evaluated, the cell constants of the conductivity cells used in the PVC Thermomat, which are normally in the range 1.00...1.20, only need to be entered exactly if the absolute value for the conductivity is to be shown correctly. The exact entry is also required before carrying out the GLP test for conductivity. The cell constants can either be entered manually or determined automatically with the aid of a defined standard solution.

Manual entry of cell constants

763 PVC THERMOMAT CONTROL / Tools / Cell constants / Manual...

The Enter/check cell constants window appears in which the cell constant for the conductivity cell can be entered for each Channel.

Automatic determination of cell constants

763 PVC THERMOMAT CONTROL / Tools / Cell constants / Automatic...

The Determine cell constants window appears:

763 PVC Thermomat48

4.4 Calibration functions

Block A

Channel 1...4 Each channel of Block A for which the cell con-

stant of the conductivity cell is to be determined

can be marked.

Block B

Channel 1...4 Each channel of Block B for which the cell con-

stant of the conductivity cell is to be determined

can be marked.

Conductivity of standard solution

Conductivity of the standard solution in µS/cm

which is filled into all measuring vessels for

which the cell constant of the conductivity cell

is to be determined.

A solution of c(KCL) = 1 mmol/L, prepared

from the 6.2301.060 Conductivity standard (KCl

0.1 mol/L) available as an option, can be used

as standard solution. The conductivity of this

standard solution is:

Temperature Conductivity

18 °C 127 µS/cm 19 °C 130 µS/cm 20 °C 133 µS/cm 21 °C 136 µS/cm 22 °C 138 µS/cm 23 °C 141 µS/cm 24 °C 144 µS/cm 25 °C 147 µS/cm

<Start> Starts the automatic determination of the cell

constants. When the determination has ended

the Enter/check cell constants window appears in

which the automatically determined cell con-

stants have been entered:

Click on <OK> to accept these values or on

<Cancel> to retain the previous values.

763 PVC Thermomat 49

4 Operation

4.4.2 Determination of Delta T

The temperature correction Delta T describes the variation of the actual sample temperature from the temperature in the heating block and is a parameter of the method (see section 4.5.2). It can be automatically determined with the 6.1111.010 Calibrated external temperature sensor (part of the 6.5616.000 GLP test set available from Metrohm as an option). Since the direct temperature measurement in PVC samples is impossible, silicone oil must be used as sample instead of PVC.

Preparations

Fig. 5 shows in detail how to install the accessories for Delta T determination. Proceed as follows:

1 Prepare reaction vessel cover

• Install gas inlet tube 3535 (part of the 6.5616.000 GLP test set, length = 148 mm) on the reaction vessel cover 22 (see section

2.2.2).

• Fasten distance piece 37 37 to the gas inlet tube 3535 so that it is located at a distance of approx. 2 cm from the upper end of the reaction vessel.

• Fasten distance piece 37 37 to the gas inlet tube 3535 so that it is located at a distance of approx. 5 cm from the lower end of the reaction vessel.

• Insert temperature sensor 3636 from above in opening 3131 of the reaction vessel cover 22 and fasten it in the corresponding openings of the distance pieces 3737.

2 Prepare reaction vessel

• Fill reaction vessel 11 with 5 g silicone oil (e.g. FLUKA

85409).

• Place the reaction vessel cover 22 with temperature sensor 3636 on the reaction vessel 11.

• Slide the temperature sensor 3636 right down (the sensor must touch the base of the vessel).

3 Insert and connect reaction vessel

• Place the prepared reaction vessel 11 in channel 2 or 3 of the heating block.

• Attach one end of the brown connecting tubing 66 at connec- tion nipple 3030 on the reaction vessel cover 22.

• Attach the other end of the brown connecting tubing 66 at the connection 1919 on the 763 PVC Thermomat (see Fig. 3).

4 Modify method parameters

• In the control window select the required Method for the heating block for which the temperature correction Delta T is to be determined.

763 PVC Thermomat50

4.4 Calibration functions

11 Reaction vessel (6.1429.040)

3636 3030

3131 3535

3333

3434

3737

22 Reaction vessel cover (6.2753.100)

66 Connecting tubing (6.1805.080)

for gas supply to reaction vessel

3030 Connection nipple (6.1808.090)

3131 Connection

Feedthrough for temperature sensor 3636

3333 Sealing ring (6.1454.040)

3434 Connection

for connection nipple 3030

3535 Gas inlet tube (6.2418.000)

length = 148 mm

3636 Temperature sensor Pt100 (6.1111.010)

3737 Distance piece (6.2042.040)

Fig. 5: Accessories for Delta T determination

• Click on to open the Method parameters window. Enter the

required set temperature for the sample under Temperature and set Delta T to 0°C. Set Gas flow to the desired value and click on <Save>.

5 Start gas flow and heating

• Switch on gas flow manually.

• Start heating for the selected block manually.

763 PVC Thermomat 51

4 Operation

Carrying out

763 PVC THERMOMAT CONTROL / Tools / Determine Delta T / Block A 763 PVC THERMOMAT CONTROL / Tools / Determine Delta T / Block B

These menu items are used to start the automatic determination of

Delta T for Block A or Block B. The External temperature sensor window

first appears in which the calibration data of the temperature sensor used can be entered (once data have been entered they are retained):

Sensor name Name of temperature sensor. Point 1...3 Calibration points 1...3 of the temperature sen-

sor.

T Temperature at the calibration point in °C. R Resistance at the calibration point in ohms.

When the external temperature sensor data have been entered the De-

termination of Delta T window appears.

763 PVC Thermomat52

4.4 Calibration functions

If the temperature defined in the method has not been reached then the heating is started automatically. The message Waiting until temperature is

reached... appears in the window.

When the temperature defined in the method has been reached the message Measuring temperature. Please wait... appears in the window. The three following values are shown below this message:

Block temperature The temperature in the heating block measured

by the internal temperature sensor.

Temperature ext. sensor The temperature in the reaction vessel meas-

ured by the external temperature sensor.

Delta T The temperature correction determined from

the difference between Block temperature – Tem-

perature ext. sensor.

As soon as both the measured temperatures are stable the message

Measured temperature is now stable! appears. The determined tempera-

ture correction Delta T can now be included in the method with <Accept>. The message Delta T is now set in the corresponding method then appears.

763 PVC Thermomat 53

4 Operation

4.5 Methods

4.5.1 Method handling

Create method

763 PVC THERMOMAT CONTROL / File / New method

Creates a new method. A window opens for the input of the method parameters (see section 4.5.2). When all parameters have been entered the method must be stored under a new name with <Save as...>.

Open method

763 PVC THERMOMAT CONTROL / File / Open method

Opens an existing method. The Open method window opens for method selection.

Method name Name of the method. Creation date Date and time at method creation.

Creator Name of the logged-in user at method creation.

<Open> Open the method parameters window (see

section 4.5.2).

Method manager

763 PVC THERMOMAT CONTROL / File / Method manager

The Method manager window opens for renaming, deleting and opening methods.

763 PVC Thermomat54

Method name Name of the method. Creation date Date and time at method creation.

Creator Name of the logged-in user at method creation.

<Rename> Rename the selected method.

<Delete> Delete the selected method.

<Open> Open the method parameters window (see

section 4.5.2).

Save method

In the Method parameters window (see section 4.5.2) the two following buttons are available for storing an opened method:

<Save> Saves the method under the same name.

<Save as...> Saves the method under a new name. The old

method is retained. Methods can also be copied in this way.

4.5 Methods

Print method report

The following button is available in the Method parameters window (see section 4.5.2) for printing out all the method parameters of the opened method:

<Print> Prints out method report.

4.5.2 Method parameters

Overview

763 PVC THERMOMAT CONTROL / File / Open method

By clicking on this menu item or on beside the method name in the operating field of the 763 PVC THERMOMAT CONTROL window the window with the method parameters opens; it contains the following tabs:

Parameters Measuring parameters. Evaluation Parameters for curve evaluation. Curves Parameters for scaling the axes. Formulas Equation input for further calculation of the

Standards Parameters for calculating the standard time. Documentation Parameters for report output. Description Freely-definable comments about method.

induction and stability times.

763 PVC Thermomat 55

4 Operation

The Method parameters window contains the following buttons:

<Save> Saves method under the same name. <Save as> Saves method under a new name; the old

method is retained.

<Print> Prints out method report.

<Cancel> Closes method parameter window without

saving the modified parameters.

Parameters

Tab Parameters of the Method parameters window with measuring parameters.

Temperature Set temperature of the sample.

Range: 50...220 °C

Delta T Temperature correction: Correction value for

increasing the block temperature in order to reach the set temperature in the sample. This value is determined by measuring the variation of the actual sample temperature from the block temperature using a calibrated external temperature sensor (see section 4.4.2). Range: -9.9...9.9 °C

763 PVC Thermomat56

4.5 Methods

If no temperature sensor is available for the

Delta T determination, a value of +0.6 °C can be

entered for temperatures of 160 °C to 200 °C (this value was determined using 5 g silicone oil and a gas flow of 7 L/h nitrogen).

Gas flow Gas flow through sample. It cannot be set in-

dividually for each block; the flow rate for both blocks depends always on the value entered in the method loaded for Block A. Range: 4...15 L/h

Start options

Start delay Delay period until start of measurement.

Range: 0...1000 min

Start mode Mode for start and stop of the channels:

per channel All 8 channels can be started and stopped indi-

vidually.

per 2 channels Each 2 channels can be started and stopped

together.

per block The 4 channels in one block can be started and

stopped together.

Stop criteria

Time Time until automatic termination of the determi-

nation. Range: 0.1...100 h

Conductivity Limit value for conductivity. If this value is

reached then the determination is terminated automatically. Range: 1...400 µµS/cm

Endpoint(s) Automatic termination of the determination

when each active channel has reached all endpoints.

Shut off at end of determinations

Heater Automatically switches off the heating at the

end of the determination.

Gas flow Automatically switches off the gas flow at the

end of the determination.

If the gas flow is automatically switched off, the reaction vessels must be removed immediately from the PVC Thermomat after the end of the determination. If the reaction vessels are not removed, the instrument can be damaged.

763 PVC Thermomat 57

4 Operation

Evaluation

Tab Evaluation of the Method parameters window with parameters for curve evaluation.

Evaluate induction time Determines the induction time (see below). Evaluate stability time Determines the stability time (see below).

Delta Kappa Conductivity alteration for the determination of

the stability time. Range: 1...400 µµS/cm

Evaluation delay (option for the induction time)

Delay period until start of the curve evaluation. Range: 0...100 h

Evaluation suppression (option for the induction time)

Start Time from start of the determination up to start

of the evaluation suppression. Range: 0...100 h

End Time from start of the determination up to end

of the evaluation suppression. Range: 0...100 h

763 PVC Thermomat58

Induction time

The induction time is the time up to the inflection point of the conductivity vs. time curve recorded by the PVC Thermomat. The induction

time is a characteristic value for the thermal stability of the sample under investigation.

For automatic evaluation of the induction time the second derivative of the measured curve is used. This derivative has a maximum at the inflection point and can be displayed in the Live graph window. In order to recognize an inflection point certain criteria concerning the height and width of the peak in the second derivative must be fulfilled. The inflection point can also be evaluated manually as point of intersection of the two tangents of the extended straight arms of the curve.

Conductivity

Evaluation

delay

suppression

Start

End

4.5 Methods

Induction time

With certain samples it is possible for the conductivity to increase in small steps a long time before the induction time itself. In order that this increase is not evaluated as the endpoint the operator can delay the evaluation or suppress it in a particular range.

Stability time

The stability time is the time required to achieve a given conductivity alteration of Delta Kappa.

Conductivity

Inflection point

Time

Delta Kappa

Stability time

Time

The input of an evaluation delay or evaluation suppression has no influence on this evaluation mode; the calculation is always carried out from the time that the measurement was started.

763 PVC Thermomat 59

4 Operation

Curves

Tab Curves of the Method parameters window with parameters for scaling the curve axes.

Time axis(x)

Auto scaling Automatic fixing of the initial and final values of

the time axis.

Manual scaling Manual fixing of the final value of the time axis. End value Final value of the time axis.

Range: 0.5...100 h

Conductivity axis(y)

Auto scaling Automatic fixing of the initial and final values of

the conductivity axis.

Manual scaling Manual fixing of the final value of the conductiv-

ity axis.

End value Final value of the conductivity axis.

Range: 10...400 µµS/cm

763 PVC Thermomat60

Formulas

Tab Formulas of the Method parameters window with parameters for entering equations for further calculations with the induction and stability times.

4.5 Methods

Formula 1 for induction time

If this option is switched on then the automatically determined Induction time will be calculated from the values entered in the equation by the operator and then stored as the Formula 1 result under the name entered in the first field.

Formula 2 for stability time

If this option is switched on then the automatically determined Stability time will be calculated from the values entered in the equation by the operator and then stored as the Formula 2 result under the name entered in the first field.

Formula 3 for stability time

If this option is switched on then the automatically determined Stability time will be calculated from the values entered in the equation by the operator and then stored as the Formula 3 result under the name entered in the first field.

763 PVC Thermomat 61

4 Operation

Standards

Tab Standards of the Method parameters window with parameters for calculating the standard time.

Calculate standard time Switches the calculation of the standard time

according to the following equation on/off:

Standard time = Factor

Formula parameters

Factor Parameter for calculating the standard time

(Temperature - Target temperature)/10

×× Induction time

which gives the factor by which the time changes by 10 °C. This value can be determined by the extrapolation (see section 4.7.8) of results obtained at different temperatures.

Target temperature Target temperature for calculating the standard

time.

763 PVC Thermomat62

Documentation

Tab Documentation of the Method parameters window with parameters for the report output.

4.5 Methods

Include in report

Header Output of the header with company settings (if

defined), printout date, sample identifications, instrument information, determination date, user, cell constant and serial number.

Method parameters Output of the method parameters. Curve(s) Output of curves. Method description Output of the method description given on the

Description tab.

Results Output of the selected results: Induction time,

Stability time, Standard time, Formula 1...3.

Automatic report

Send to printer immediately

Automatic printout of the reports defined under

Include in report following the end of the deter-

mination.

Send to file Automatic output of determination and method

data following the end of the determination as a text file *.txt for further processing in other programs. The contents of this report does not depend on the report elements defined under In-

clude in report.

<Browse> Selection of the Directory for storing this file.

763 PVC Thermomat 63

4 Operation

Description

Tab Description of the Method parameters window with freely-definable

comments about the method.

Enter description text Comments about the method.

763 PVC Thermomat64

4.6 Determinations

4.6.1 Flow chart

The following flow chart provides an overview of all steps for carrying out determinations of the oxidative stability.

Prepare samples sect. 4.6.2

Prepare instruments + accessories sect. 4.6.3

Select method sect. 4.6.4

Start heating sect. 4.6.4

4.6 Determinations

Modify method parameters sect. 4.5.2

Enter sample identifiers sect. 4.6.4

temperature

reached?

yes

Insert reaction vessels sect. 4.6.4

Start determination sect. 4.6.4

stop crit.

reached?

yes

Determination finished

Modify live parameters sect. 4.6.4

Stop determination manually sect. 4.6.4

Automatic report output sect. 4.5.2

Result display sect. 4.7

763 PVC Thermomat 65

4 Operation

4.6.2 Sample preparation

PVC or other plastics which decompose through the action of heat with cleavage of hydrogen halides are prepared in accordance with DIN 53'381 as follows:

1 Powdery samples

• Polymers, dry blends and coating powders need no special sample pretreatment.

2 Pastes

• Pastes are fused on a glass plate in a drying oven to a sheet with a thickness of about 0.5 mm. After cooling, the sheet is cut into pieces of edge length about 2 mm.

3 Solid samples

• Molding compounds in granular form, molded and finished parts, semi-finished products as well as coatings separated from the substrate are pulverized in accordance with DIN 53'733 and screened to separate the screening fraction between the analytical screens with wire mesh screen DIN 4188-

1.4 (wire mesh of stainless steel with 1.4 mm inside diameter mesh size) and wire mesh screen DIN 4188-2 (wire mesh of stainless steel with 2 mm inside diameter mesh size) for the experiments.

4 Sheets

• Sheets are cut into pieces with an edge length of about 2 mm.

According to DIN 53'581, the samples are to be added directly into the prewarmed reaction vessels inserted in the heating block. Nevertheless, comparative measurements have shown identical results for sample addition to cold or hot reaction vessels.

4.6.3 Prepare instruments and accessories

Clean instruments and accessories

The cleanness of instruments and accessories is an absolute necessity for achieving reliable, reproducible and correct analytical results. Even minute contamination can catalytically accelerate the thermal decomposition and lead to completely false results. Make sure that the following checks and cleaning procedures are carried out before the start of a determination:

1 Openings for reaction vessels

• Check whether the openings for the reaction vessels are clean and empty. Blow out any dust in the openings with nitrogen.

763 PVC Thermomat66

4.6 Determinations

• When the instrument is not in use always close the openings

with stoppers.

2 Measuring vessels and accessories

• After the contents have been discarded clean used meas-

uring vessels 44 several times with alcohol and distilled water (do not use acetone!).

• Rinse the measuring vessel cover 55 complete with elec-

trodes 2828 and PTFE tube 2727 several times with distilled water and acetone. If necessary, remove the protective ring 2929 for better access to the electrodes 28 28 (see Fig. 4).

• Rinse the connecting tubing 33 between reaction vessel and

measuring vessel several times with distilled water and acetone.

3 Reaction vessels and accessories

• It is recommended to use new reaction vessels 11 and gas

inlet tubes 3232 for each determination. Blow out new reaction

vessels with nitrogen.

• Used and not too strongly contaminated reaction vessels and

gas inlet tubes can be cleaned by immersion in boiling RBS solution for 1 h or a similar laboratory flushing agent. They must then be thoroughly rinsed with distilled water and acetone.

RBS attacks glass. Reaction vessels and gas inlet tubes therefore cannot be cleaned ad infinitum.

• Remove the gas inlet tube 3232 from the reaction vessel

cover 22 and rinse it several times with distilled water and

acetone. Dry the cover at 80 °C in a drying oven.

Reaction vessel covers which have not been dried properly can falsify the results of the following determinations.

Prepare measuring vessels

The cleaned measuring vessels must always be prepared as follows before the start of a determination (see Fig. 4):

1 Fill measuring vessels

• Fill each cleaned measuring vessel 44 with 60 mL distilled

water. For analysis times >24 h more than 60 mL distilled

water must be added to take the evaporation losses of approx. 7 mL/d into account and to ensure that the electrodes remain adequately immersed.

763 PVC Thermomat 67

4 Operation

2 Insert measuring vessels

• Place the measuring vessel cover 55 fitted with a gas inlet tube on the measuring vessel 4 4 (see Fig. 4).

• Place the measuring vessel 44 with its cover in one of the openings provided for it on the 763 PVC Thermomat and connect the electrode plugs 2626 on the cover to the corre- sponding sockets 2020 on the 763 PVC Thermomat (see Fig. 3).

Prepare reaction vessels

Before the start of a determination the reaction vessels are filled with the samples and prepared as follows (see Fig. 4):

1 Weighing in the samples

• Weigh out 0.5 g of each of the prepared samples into the cold reaction vessels 1 1.

2 Mount accessories

• Take the upper rim of the reaction vessel 11 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 3232 (length = 98 mm) into the reac- tion vessel cover 22 and fasten it by screwing down the con- nection nipple 30 30.

• Place the reaction vessel cover 22 on the reaction vessel 1 1. Rotate the cover so that the gas inlet tube 3232 is as close as possible to the vessel wall.

• Fasten the white connecting tubing 33 to the measuring vessel 44 on to the corresponding connection 3131 on the reac- tion vessel cover 2 2.

• Place the prepared reaction vessel 11 into the vessel holder.

763 PVC Thermomat68

4.6.4 Carry out determinations

Select method

The determination method is selected in the Method field in the control window.

Different methods with different temperatures can be selected for Block A and Block B. In contrast, the gas flow which is defined in the method loaded for Block A also applies to Block B.

By clicking on the method parameters (see section 4.5.2) can be altered as required.

Switch on heating

The heating of the two blocks A and B to the temperature set in the method can be switched on individually for each block. This is done by clicking on the following button.

4.6 Determinations

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" on the 763 PVC Thermomat starts to blink for the selected block.

If this button is clicked on again during the heating-up phase then the heating will be switched off.

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.

When the selected temperature has been reached the temperature display 99 "TEMPERATURE" stops blinking and the LED remains lit up. At the same time the color of the frame of the button switches to green. The block is now ready for receiving the samples and starting the determination.

If this button is clicked on the heating is switched off.

763 PVC Thermomat 69

4 Operation

Enter sample identifiers

The sample identifiers ID1 and ID2 can be entered in the corresponding fields of the operating area in the control window before or after starting the determination.

The entry for ID1 can be selected from the automatically formed list of identifiers which have already been entered. This list can be deleted again with 763 PVC THERMOMAT CONTROL / Options / Clear sample ID his-

tory.

Insert reaction vessels

When the heating block reaches the temperature defined in the method (frame color of the <Heat to...> button turns green) the reaction vessels can be inserted into the PVC Thermomat 763 as follows (see Fig. 4):

1 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 in use with stoppers or empty reaction vessels to prevent contamination.

2 Connect reaction vessels

• Connect the white connecting tubing 33 fastened to the reac- tion vessel cover 22 to the corresponding connection piece 2222 on the measuring vessel cover 55.

• Screw the brown gas supply tubing 66 onto the reaction vessel cover 22 and the corresponding connection 1919 on the 763 PVC Thermomat (see Fig. 3).

Start determinations

Determinations can be started by clicking on the following buttons in the operating area of the 763 PVC THERMOMAT CONTROL window:

Starts a single determination for the corresponding channel.

Starts a double determination for channels 1 and 2.

Starts a double determination for channels 3 and 4.

Starts a multiple determination for channels 1 to 4.

Starts all Block A channels.

Starts all Block B channels.

763 PVC Thermomat70

4.6 Determinations

Live curve

The live curve of a started determination is shown in the operating window beside the channel number. Either a status message or the actual measured value appears above the curve. A differentiation is made between the following conditions:

No active measurement. The channel is ready for the start of a determination.

Determination started.

The first value is being measured.

No active measurement. Communication error between instrument and PC.

Running measurement.

Measured value and time are shown above the live curve.

Determination finished.

The channel is ready for the start of a new determination.

Live parameters

763 PVC THERMOMAT CONTROL / View / Live parameters

The Live parameters window opens for altering method parameters during a running determination.

763 PVC Thermomat 71

4 Operation

The following parameters for Block A or Block B can be altered live:

Stop criteria

Time Time up to automatic termination of the deter-

mination. Range: 0.1...100 h

Conductivity Conductivity limit value. When this value is

reached the determination is automatically terminated. Range: 1...400 µµS/cm

Endpoint(s) Automatic termination of the determination

when each active channel has reached all endpoints.

Shut off at end of determinations

Heater Automatically switches off the heating at the

end of the determination.

Gas flow Automatically switches off the gas flow at the

end of the determination.

If the gas flow is automatically switched off, the reaction vessels must be removed from the PVC Thermomat within 1 h after the end of the determination. If the reaction vessels are not removed, a vacuum is generated in the course of the time by condensation of the further produced HCl in condensed water vapor from the measuring vessel and the measuring solution is siphoned back into the hot reaction vessel.

Stop determinations

Determinations are normally terminated automatically when the stop criteria defined in the method have been achieved. Running determinations can also be stopped manually be clicking on the following buttons in the operating area of the 763 PVC THERMOMAT CONTROL window:

Stops a single determination for the corresponding channel.

Stops a double determination for channels 1 and 2.

Stops a double determination for channels 3 and 4.

Stops a multiple determination for channels 1 to 4.

If a determination is stopped manually an inquiry Do you want to save this

determination? appears. With No neither measuring data will be saved

nor will results be automatically outputted.

763 PVC Thermomat72

4.7 Results

4.7.1 Determination overview

Open determination overview

The determination overview shows selected information in tabular form about all the determinations which are stored in the opened database. To open a determination overview the results window must be opened first and then the database opened.

763 PVC THERMOMAT CONTROL / File / Results

This menu item is used to open the 763 PVC THERMOMAT RESULTS window. It is used for the display, output and recalculation of results of the determinations recorded by the 763 PVC Thermomat. The determination data are stored in the *.mrd database files and can be shown in this window as an overview table and as curves. The results window can run even when the control window is closed.

4.7 Results

When the results window is opened the Repos.mrd database is automatically loaded; all the recorded determinations are loaded in this database as standard.

The program part for display of the results window is organized as database and saved in the Nachaus.prg file, which normally has approx. 5 MB. If the size of this file exceeds 10 MB it should be newly optimized and compressed. To do this, close the program and select

Optimize / Program from the PVC Thermomat program folder in the Start / Program menu.

763 PVC THERMOMAT RESULTS / File / Open database

Opens an existing database. The Open database window opens for the selection of the database file *.mrd. When the database has been selected the corresponding determination overview is automatically opened. Only one database can be opened at any time.

The Repos.mrd database has to be optimized and compressed from time to time, especially if data records are deleted frequently. To do this, close the program and select Optimize / Database from the PVC Thermomat program folder in the Start / Program menu.

763 PVC THERMOMAT RESULTS / View / Determination overview

Displays an overview table with selected data fields of all the determinations contained in the opened database.

763 PVC Thermomat 73

4 Operation

Format determination overview

763 PVC THERMOMAT RESULTS / Format / Select fields

The Display fields window opens for selection of the fields which are to be shown in the determination overview.

Selection Selection of all the fields which can be used for

the determination overview. The following fields are available:

Block Number of the block used for the determina-

tion.

Cell constant Cell constant of the conductivity cell used for

the determination.

Channel Number of the channel used for the determina-

tion.

Delta Kappa Alteration in conductivity for the determination

of the Stability time.

Determination date Date and time at which the determination was

started.

Formula 1 for induction time

Result for Formula 1.

Formula 2 for stability time

Result for Formula 2.

Formula 3 for stability time

Result for Formula 3.

Gas flow Gas flow through sample. ID 1 Sample identifier 1. ID 2 Sample identifier 2.

763 PVC Thermomat74

4.7 Results

Induction time automatic

Automatically determined induction time.

Induction time manual

Induction time manually determined with the re-

evaluation.

Method name Name of method. Send to file Folder in which the *.txt determination file is to

be stored.

Serial number Serial number of the instrument used for the

determination.

Stability time Automatically determined stability time. Standard time Automatically determined standard time. Temperature Set temperature for the method. Unit Number of the instrument used for the determi-

nation.

User Name of the user logged in at the start of the

determination.

Display Fields which have been selected for the deter-

mination overview.

Moves all fields in Selection to Display.

Moves the field selected in Selection to Display. The field is inserted at the end of the list.

Moves the field selected in Selection to Display. The field is inserted above the field which is marked in Display.

Moves the field selected in Display to Selection.

Moves all fields in Display to Selection.

763 PVC THERMOMAT RESULTS / Format / Adjust width

The Column width window opens in which the width of the columns selected for the determination overview can be fixed.

763 PVC Thermomat 75

4 Operation

Column Width Column width in characters. Standard width Resets the column width to the default value

(18.5 characters).

<Best fit> Adapts the column width to the longest field

content (including title).

Alternatively the column width can be set directly by using the mousemouse. This is carried out by moving the cursor in the title line of the table between two columns until the cursor appears as . With the left-hand

mouse key the column can then be drawn to the required size. A double-click on the selected column automatically adapts the column

width to the longest field content (including title).

763 PVC THERMOMAT RESULTS / Format / Fields...

The Cells effects window opens in which the format of cells shown in the determination overview can be fixed.

Gridlines shown

Horizontal Shows horizontal grid lines. Vertical Shows vertical grid lines.

Cell effect

Flat Shows flat cells. Raised Shows raised cells. Sunken Shows depressed cells.

Gridline color Color of horizontal and vertical grid lines.

Background color Color of cell background.

Sample Display of the selected format for the cells.

763 PVC Thermomat76

4.7 Results

763 PVC THERMOMAT RESULTS / Format / Fonts...

The Font window opens in which the font used for the determination overview can be fixed.

Font Selects the font from those available in the PC. Font style Selects the typestyle for the selected font.

Size Selects the type size for the selected font in

points.

Effects

Underline Selects that the characters are to be under-

lined.

Color Selects the color for the selected font.

Sample Display of the selected font.

763 PVC Thermomat 77

4 Operation

Mark determinations

763 PVC THERMOMAT RESULTS / Edit / Select record

Marks the record (line) in the determination overview in which the cursor is located.

Alternatively the record can be marked by using the mouse; this is done by clicking on the gray field to the left of the required line. If the left-hand mouse key is kept pressed down then several lines in sequence can be marked.

763 PVC THERMOMAT RESULTS / Edit / Select all records

Marks all records (lines) in the determination overview. This function can be triggered by clicking on the first empty field in the

title line of the determination overview.

Find determination

763 PVC THERMOMAT RESULTS / Determination / Find

The Find window opens in which the search template for the search in the determination overview can be entered.

Find What Search template.

The following wildcards are also allowed:

* any character sequence (e.g. *ab, *ab*, ab*) ? individual character (e.g. a?a, ??a, ab?) # individual number (e.g. ##20, ab###, #23##)

Search Search mode.

All Searches through the whole table. Down Searches downwards to the end of the table. Up Searches upwards to the start of the table.

Match Search area.

Whole field The search is only successful when the whole

field agrees with the search template.

Start of field The search is successful when the start of the

field contents agrees with the search template.

Any part of field The search is successful when part of the field

contents agrees with the search template.

763 PVC Thermomat78

4.7 Results

Match Case If this option is switched on then the search will

only be successful when the upper and lower case characters of the search template and field contents coincide.

Search Fields As Formatted

If this option is switched on then, in searches for the whole field content in fields with units (e.g. °C, h), the unit will also be taken into account. If only the numerical value is being looked for then this option must be switched off (standard setting).

Search Only Current Field

If this option is switched on then the search will be limited to the selected field. The field name is shown in the window title. This option is not available if one or more complete lines are marked.

<Find First> Begins the search at the start of the determina-

tion overview.

<Find Next> Continues the search from the location of the

cursor in the determination overview.

Delete determinations

763 PVC THERMOMAT RESULTS / Determination / Delete

Deletes the marked determinations from the database.

This menu item is reserved for the Administrator.

763 PVC Thermomat 79

4 Operation

Sort and filter determinations

763 PVC THERMOMAT RESULTS / Determination / Sort / Ascending

Sorts the records in the determination overview according to the field contents in the selected column (marked column or column in which the cursor is located) in increasing sequence. If several columns are marked then the records will be sorted beginning with the first marked column from the left. The sorting conditions are stored under Special fil-

ter/sorting.

763 PVC THERMOMAT RESULTS / Determination / Sort / Descending

Sorts the records in the determination overview according to the field contents in the selected column (marked column or column in which the cursor is located) in decreasing sequence. If several columns are marked then the records will be sorted beginning with the first marked column from the left. The sorting conditions are stored under Special fil-

ter/sorting.

The ascending or descending sort can be removed again by clicking on or Determination / Filter / Remove filter/sorting. If the sort is not

removed then it is retained until a new sorting process is carried out.

If sorting has been switched off it can be used again by clicking on or Determination / Filter / Apply filter/sorting.

For complex sorting processes with several columns a Special sorting must be used.

763 PVC THERMOMAT RESULTS / Determination / Filter / Selection based filter

The selection-based filter is a method for filtering records rapidly and conveniently. This is done by first marking a part of an entry or the complete entry in a field in the determination overview. After activating the selection-based filter the table is filtered so that only records which contain the marked entry are shown. The filtering conditions are stored under Special filter/sorting.

The filter can be removed again by clicking on or Determination /

Filter / Remove filter/sorting. If the filter is not removed then it is retained

until a new filtering process is carried out. If filtering has been switched off it can be used again by clicking on

or Determination / Filter / Apply filter/sorting.

For complex filters a Special filter must be used.

763 PVC Thermomat80

4.7 Results

763 PVC THERMOMAT RESULTS / Determination / Filter / Special filter/sorting

The Special filter/sorting window opens in which the complex conditions for filtering and sorting records can be defined.

The lower, important part of the window contains a table for entry of conditions with the following lines:

Field Selects a field (column) in the determination

overview.

Sort Sorts the selected field: Ascending, Descending

or (not sorted).

Criteria Criteria for filtering records.

or Further criteria for filtering records.

In the lines Criteria and or and in all following lines the number of records to be searched for can be limited by the use of expressions. An expression is a combination of operators, functions and field names for laying down a condition for filtering records. Only the most important elements and rules for entering expressions and a few selected examples are given below. For more information please refer to the documentation about Microsoft Access.

Operators, functions, field names

Mathematical operators +, -, =, *, / Comparison operators <, >, <>, <=, >=, Between ... And ... Logical operators And, Or, Not Wildcards *, ?, # (see Find) Current date Date() Current time Now() (date and time) Other fields ["field name"]

763 PVC Thermomat 81

4 Operation

Linkages with different fields

If conditions are fixed in different fields then these conditions can also be linked with And and Or. The following conditions apply:

Criteria in the same line are And-conditions, i.e. only those records are shown which fulfill all conditions.

Criteria in different lines are Or-conditions, i.e. all records which fulfill one of the conditions will be shown.

Examples

>10 Values larger than 10. *PVC* All data with "PVC" as part of their name. ##.##.1998 All data for 1998. Between Date() And (Date() - 7)

all data of previous week.

Newly entered conditions are only saved when they are used with the

Special filter/sorting window open by clicking on or Determination / Filter / Apply filter/sorting.

By clicking on or Edit / Delete filter all the conditions entered in the

Special filter/sorting window are deleted again.

By clicking on or Edit / Undo the last alterations made in the Special

filter/sorting window are canceled.

The filter/sort can be removed again by clicking on or Determina-

tion / Filter / Remove filter/sorting. If the filter/sort is not removed then it is

retained until a new filtering/sorting process is carried out. If filtering has been switched off it can be used again by clicking on

or Determination / Filter / Apply filter/sorting.

763 PVC Thermomat82

4.7 Results

763 PVC THERMOMAT RESULTS / Determination / Filter / Apply filter/sorting

The conditions for filtering and sorting records stored under Special fil-

ter/sorting are applied to the determination overview.

The filter/sorting can be removed again by clicking on or Determi-

nation / Filter / Remove filter/sorting. If the filter/sorting is not removed then

it is retained until a new filtering/sorting process is carried out.

763 PVC THERMOMAT RESULTS / Determination / Filter / Remove filter/sorting

The filter/sorting applied to the determination overview is removed and all records are shown again.

If filter/sorting is switched off it can be switched on again by clicking on

or Determination / Filter / Apply filter/sorting.

763 PVC THERMOMAT RESULTS / Edit / Undo

The last alteration made in the Special filter/sorting window is canceled.

763 PVC THERMOMAT RESULTS / Edit / Delete filter

All the conditions entered in the Special filter/sorting window are deleted again.

763 PVC THERMOMAT RESULTS / Determination / Filter / Filter selection

The lines marked in the determination overview are incorporated in the filter, i.e. only those lines which have previously been marked will be shown.

763 PVC THERMOMAT RESULTS / Determination / Filter / Selection not in filter

The lines marked in the determination overview are removed from the filter, i.e. only those lines which were not previously marked will be shown.

763 PVC Thermomat 83

4 Operation

4.7.2 Determination and method data

Open view

763 PVC THERMOMAT RESULTS / View / Determination and method data

The Determination and method data window is opened which contains all parameters and results for the selected determination on the following tabs:

Determination Information about the determination. Results Overview of results of determination. Method Information about the method. Parameters Measuring parameters. Evaluation Parameters for curve evaluation. Formulas Formula input for further calculation of in-

duction and stability times.

Standards Parameters for calculating the standard time. Curves Parameters for scaling the axes. Documentation Parameters for report output. Warnings Warnings about the determination.

If the determination in the determination overview is changed by marking a different determination then the parameters in the Determination

and method window will be updated automatically.

Determination

Determination tab of the Determination and method data window with in-

formation about the determination.

763 PVC Thermomat84

4.7 Results

ID 1 Sample identifier 1. ID 2 Sample identifier 2.

Determination date Date and time at which the determination was

started.

User Name of the user logged in at the start of the

determination.

Serial number Serial number of the instrument used for the

determination.

Cell constant Cell constant of the conductivity cell used for

the determination.

GLP test GLP status at the time the determination was

carried out. The following results are possible:

GLP test not switched on

GLP monitoring was not switched on for either temperature or conductivity or gas flow.

Due GLP test The next GLP test was due. GLP test not passed The last GLP test carried out was failed. GLP test passed The last GLP test carried out was passed.

Display of instrument, block and channel used for the determination

Results

Results tab of the Determination and method data window with results

overview for the determination.

Induction time automatic Automatically determined Induction time. Induction time manual Induction time determined manually by ree-

valuation.

Stability time Determined Stability time for Delta Kappa.

Delta Kappa Alteration in conductivity for the determination

of the Stability time.

Formula 1 for induction time

Result for Formula 1.

Formula 2 for induction time

Result for Formula 2.

Formula 3 for induction time

Result for Formula 3.

Standard time Result for standard time.

763 PVC Thermomat 85

4 Operation

Method

Method tab of the Determination and method data window with information

about the method used for the determination.

Method name Name of the method. Creation date Date on which the method was last saved.

Creator Name of the logged-in used the last time that

the method was saved.

Method description Description of the method (see section 4.5.2).

763 PVC Thermomat86

Parameters

Parameters tab of the Determination and method data window with the dis-

play of the measuring parameters used in the determination.

4.7 Results

Temperature Set temperature of sample. Delta T Temperature correction: Correction value for

increasing the block temperature in order to reach the set temperature in the sample.

Gas flow Gas flow through sample.

Start options

Start delay Delay time until start of measurement. Start mode Mode for starting the channels:

per channel All channels have been started individually. per 2 channels Each 2 channels have been started together. per block 4 channels in one block have been started to-

gether.

Stop criteria

Time Time until automatic termination of determina-

tion.

Conductivity Conductivity limit. When this value is reached

the determination is automatically terminated.

Endpoint(s) Automatic termination of the determination

when each active channel has reached all endpoints.

763 PVC Thermomat 87

4 Operation

Shut off at end of determinations

Heater Heating was switched off automatically at end

of determination.

Gas flow Gas flow was switched off automatically at end

of determination.

Evaluation

Evaluation tab of the Determination and method data window with the dis-

play of the parameters used for curve evaluation.

Evaluate induction time Determination of induction time. Evaluate stability time Determination of stability time.

Delta Kappa Alteration in conductivity for the determination

of the stability time.

Evaluation delay (Option for induction time)

Delay time before the start of curve evaluation.

Evaluation suppression (Option for induction time)

Start Time from start of determination until start of

evaluation suppression.

End Time from start of determination until end of

evaluation suppression.

763 PVC Thermomat88

Formulas

Formulas tab of the Determination and method data window with the dis-

play of the formulas used for the calculation.

4.7 Results

Formula 1 for induction time

The automatically determined Induction time was calculated from the values entered in the equation by the operator and then stored as the

Formula 1 result under the name entered in the

first field.

Formula 2 for induction time

The automatically determined Stability time was calculated from the values entered in the equation by the operator and then stored as the

Formula 2 result under the name entered in the

first field.

Formula 3 for induction time

The automatically determined Stability time was calculated from the values entered in the equation by the operator and then stored as the

Formula 3 result under the name entered in the

first field.

763 PVC Thermomat 89

4 Operation

Standards

Standards tab of the Determination and method data window with the pa-

rameters used for the calculation of the standard time.

Calculation of standard time

Shows whether the standard time was calculated or not.

Formula parameters

Factor Parameter for calculating the standard time

which gives the factor by which the time changes per 10 °C.

Target temperature Target temperature for calculating the standard

time.

Curves

Curves tab of the Determination and method data window with the display

of the parameters used for scaling the axes of the curve.

763 PVC Thermomat90

Time axis (x)

Autoscaling Automatic fixing of the initial and final values of

the time axis.

Manual scaling Manual fixing of the final value of the time axis. End value Final value of the time axis.

Conductivity axis (y)

Autoscaling Automatic fixing of the initial and final values of

the conductivity axis.

Manual scaling Manual fixing of the final value of the conductiv-

ity axis.

End value Final value of the conductivity axis.

Documentation

Documentation tab of the Determination and method data window with dis-

play of the settings used for the report output.

4.7 Results

Include in report

Header Output of the header. Curve Output of curves. Method description Output of the method description entered on

the Description tab.

Results Output of the selected results: Induction time,

Stability time, Standard time, Formula 1...3.

Method parameters Output of method parameters.

763 PVC Thermomat 91

4 Operation

Automatic report output

Send to printer immediately

Automatic printout of the reports defined under

Include in report following the end of the deter-

mination.

Send to file Automatic output of determination and method

data following the end of the determination as a text file *.txt.

Directory Directory in which the report will be stored.

Warnings

Warnings tab of the Determination and method data window with the dis-

play of warnings about the determination.

Description If the determination was not carried out properly

then the following warnings are possible:

Temperature not reached

Set temperature was not reached at start of determination.

Missing measuring points (start time)

Measuring points are missing from the given time (in s) onwards.

Missing measuring points (end time)

Measuring points are again present from the given time (in s) onwards.

Manual stop The determination was stopped manually. Abortion after communication error

Automatic determination stop because connection between the 763 PVC Thermomat and PC was interrupted.

Value Value of the warning (e.g. temperature, time).

763 PVC Thermomat92

4.7.3 Graphics and reevaluation

Single graph

763 PVC THERMOMAT RESULTS / Determination / Graphics / Single graph

Opens a new window in which the single graph for the determination selected in the determination overview is shown. The sample identifiers

ID 1 and ID 2 are shown in the window title.

4.7 Results

If present then the determined induction time (red vertical line and numbers) and stability time (black vertical line and numbers) will be shown in the graphics window as well as the measuring curve (green). A maximum of 16 single graph windows can be displayed.

By clicking the graph using the right mouse key the context-sensitive menu with the following menu items is opened:

Zoom off Switch off zooming. Copy Copy graph to clipboard. Autoscaling Switch on/off autoscaling.

In contrast to the Multiple graph and Live graph windows, the window with the single graph is not automatically updated when the determination in the determination overview is changed.

Multiple graph

763 PVC THERMOMAT RESULTS / Determination / Graphics / Multiple graph

Opens a new Multiple graph window in which all curves for the determinations marked in the determination overview are shown.

The individual measuring curves are shown in color, the legends referring to the colors (sample identifiers ID 1 and ID 2) are located in the graph header. If present the determined induction time ( ) and sta- bility time ( ) will also be shown.

763 PVC Thermomat 93

Metrohm 763PVC User Manual

Specifications and Main Features

Frequently Asked Questions

User Manual