Registration Dossier

Administrative data

Endpoint:
vapour pressure
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Testing was conducted between 03 November 2009 and 17 November 2009.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of the relevant results.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2010
Report Date:
2010

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
EU Method A.4 (Vapour Pressure)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
Date of inspection: 15-09-2009 Date of Signature:26-11-2009
Type of method:
other: vapour pressure balance

Test material

Reference
Name:
Unnamed
Type:
Constituent
Details on test material:
Sponsor's identification: DMH
Description: white crystalline solid
Batch number: N5439431
Date received: 24 February 2006
Storage conditions: room temperature in the dark

Results and discussion

Vapour pressure
Temp.:
25 °C
Vapour pressure:
0 Pa
Remarks on result:
other: The vapour pressure of the test material has been determined to be 3.8 x 10-4 Pa at 25ºC.
Transition / decomposition
Transition / decomposition:
no

Any other information on results incl. tables

Results

Run1

Temperature (ºC)

Temperature (K)

Reciprocal Temperature (K-1)

Mass Difference (µg)

Mass Difference (kg)

Vapour Pressure (Pa)

Log10Vp

101

374.15

0.002672725

927.10

9.271E-07

1.287052322

0.109596202

102

375.15

0.002665600

996.02

9.960E-07

1.382730939

0.140737680

103

376.15

0.002658514

1095.47

1.095E-06

1.520793018

0.182070110

104

377.15

0.002651465

1187.39

1.187E-06

1.648401528

0.217063008

105

378.15

0.002644453

1316.91

1.317E-06

1.828208470

0.262025717

106

379.15

0.002637479

1413.14

1.413E-06

1.961800364

0.292654811

107

380.15

0.002630541

1540.30

1.540E-06

2.138331023

0.330074937

A plot of Log10(vapour pressure (Pa)) versus reciprocal temperature (1/T(K)) for Run 1 gives the following statistical data using an unweighted least squares treatment.

Slope                                      -5309.481
Standard deviation in slope     91.611

Intercept                                       14.297
Standard deviation in intercept  0.243

The results obtained indicate the following vapour pressure relationship:

Log10(Vp (Pa)) = -5309.481/temp(K) + 14.297

The above yields a vapour pressure (Pa) at 298.15 K with a common logarithm of -3.511.


Run 1 - Graph of Log10Vapour Pressure vs Reciprocal Temperature (please see attached Run 1 to Run 4 Graphs of log10Vapour Pressure vs Reciprocal Temperature)


Run 2

Temperature (ºC)

Temperature (K)

Reciprocal Temperature (K-1)

Mass Difference (µg)

Mass Difference (kg)

Vapour Pressure (Pa)

Log10Vp

101

374.15

0.002672725

927.73

9.277E-07

1.287926923

0.109891222

102

375.15

0.002665600

999.71

9.997E-07

1.387853604

0.142343658

103

376.15

0.002658514

1092.33

1.092E-06

1.516433893

0.180823483

104

377.15

0.002651465

1185.98

1.186E-06

1.646444086

0.216546987

105

378.15

0.002644453

1286.37

1.286E-06

1.785811126

0.251835524

106

379.15

0.002637479

1392.65

1.393E-06

1.933354995

0.286311605

107

380.15

0.002630541

1516.75

1.517E-06

2.105637589

0.323383625

A plot of Log10(vapour pressure (Pa)) versus reciprocal temperature (1/T(K)) for Run 2 gives the following statistical data using an unweighted least squares treatment.

Slope                                      -5076.768
Standard deviation in slope     36.058

Intercept                                       13.677
Standard deviation in intercept  0.096

The results obtained indicate the following vapour pressure relationship:

Log10(Vp (Pa)) = -5076.768/temp(K) + 13.677

The above yields a vapour pressure (Pa) at 298.15 K with a common logarithm of -3.350.


Run 2 - Graph of Log10Vapour Pressure vs Reciprocal Temperature (please see attached Run 1 to Run 4 Graphs of log10Vapour Pressure vs Reciprocal Temperature)


Run 3

Temperature (ºC)

Temperature (K)

Reciprocal Temperature (K-1)

Mass Difference (µg)

Mass Difference (kg)

Vapour Pressure (Pa)

Log10Vp

101

374.15

0.002672725

927.10

9.271E-07

1.287052322

0.109596202

102

375.15

0.002665600

1001.36

1.001E-06

1.390144227

0.143059860

103

376.15

0.002658514

1089.19

1.089E-06

1.512074769

0.179573267

104

377.15

0.002651465

1199.01

1.199E-06

1.664533065

0.221292426

105

378.15

0.002644453

1286.92

1.287E-06

1.786574667

0.252021172

106

379.15

0.002637479

1399.25

1.399E-06

1.942517486

0.288364937

107

380.15

0.002630541

1520.60

1.521E-06

2.110982376

0.324484607

A plot of Log10(vapour pressure (Pa)) versus reciprocal temperature (1/T(K)) for Run 3 gives the following statistical data using an unweighted least squares treatment.

Slope                                      -5119.079
Standard deviation in slope     60.228

Intercept                                       13.790
Standard deviation in intercept  0.160

The results obtained indicate the following vapour pressure relationship:

Log10(Vp (Pa)) = -5119.079/temp(K) + 13.790

The above yields a vapour pressure (Pa) at 298.15 K with a common logarithm of -3.379.


Run 3 - Graph of Log10Vapour Pressure vs Reciprocal Temperature (please see attached Run 1 to Run 4 Graphs of log10Vapour Pressure vs Reciprocal Temperature)


Run 4

Temperature (ºC)

Temperature (K)

Reciprocal Temperature (K-1)

Mass Difference (µg)

Mass Difference (kg)

Vapour Pressure (Pa)

Log10Vp

101

374.15

0.002672725

911.72

9.117E-07

1.265700941

0.102331103

102

375.15

0.002665600

996.73

9.967E-07

1.383716601

0.141047151

103

376.15

0.002658514

1077.18

1.077E-06

1.495401812

0.174757903

104

377.15

0.002651465

1182.21

1.182E-06

1.641210360

0.215164250

105

378.15

0.002644453

1273.66

1.274E-06

1.768166390

0.247523131

106

379.15

0.002637479

1393.75

1.394E-06

1.934882077

0.286654502

107

380.15

0.002630541

1496.27

1.496E-06

2.077206102

0.317479590

108

381.15

0.002623639

1652.39

1.652E-06

2.293940660

0.360582179

A plot of Log10(vapour pressure (Pa)) versus reciprocal temperature (1/T(K)) for Run 4 gives the following statistical data using an unweighted least squares treatment.

Slope                                      -5191.484
Standard deviation in slope     57.608

Intercept                                       13.978
Standard deviation in intercept  0.153

The results obtained indicate the following vapour pressure relationship:

Log10(Vp (Pa)) = -5191.484/temp(K) + 13.978

The above yields a vapour pressure (Pa) at 298.15 K with a common logarithm of -3.434.


Run 4- Graph of Log10Vapour Pressure vs Reciprocal Temperature (please see attached Run 1 to Run 4 Graphs of log10Vapour Pressure vs Reciprocal Temperature)

Summary of Results

Run

Log10[Vp(25ºC)]

1

-3.511

2

-3.350

3

-3.379

4

-3.434

Mean

-3.418

Vapour Pressure

3.8 x 10-4Pa

The test material did not change in appearance under the conditions used in the determination.

Applicant's summary and conclusion

Conclusions:
The vapour pressure of the test material has been determined to be 3.8 x 10-4 Pa at 25ºC.
Executive summary:

Method

The vapour pressure was determined using a vapour pressure balance withasurents being made at several temperatures and linear regression analysis used to calculate the vapour pressure at 25°C. Testing was conducted using Method A4 Vapour Pressure of Commission Regulation (EC) No 440/2008 of 30 May 2008.

Procedure

The vapour pressure was determined using a vapour pressure balance. The temperature of the sample was controlled electronically. The mass and temperature readings were recorded automatically into a computer file.

A diagram of the cross-section of the vapour pressure balance is represented in attached Figure 4.1. After evacuating the system, opening the shutter above the sample oven causes the escaping vapour jet to be directed at the scale pan. The difference in mass readings with the orifice covered and uncovered is proportional to the vapour pressure at the given oven temperature.

A sequence of runs was started after a sample of test material had been under vacuum for approximately 68 hours. Temperature and pressure readings were taken between 100 and 110 ºC with a one hour dwell at 100 ºC between runs.

Summary of Results

Run

Log10[Vp(25ºC)]

1

-3.511

2

-3.350

3

-3.379

4

-3.434

Mean

-3.418

Vapour Pressure

3.8 x 10-4Pa

The test material did not change in appearance under the conditions used in the determination.

Discussion

The unshaded points on the graphshave not been used when plotting the line. It is quite common for the first point of a run to be non linear as the system equilibrates after the dwell time.

Conclusion

The vapour pressure of the test material has been determined to be 3.8 x 10-4 Pa at 25ºC.