Registration Dossier

Administrative data

Endpoint:
boiling point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
15 Jul - 17 Jul 2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019
Report Date:
2019

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
OECD Guideline 103 (Boiling Point)
Deviations:
not specified
Qualifier:
according to
Guideline:
EU Method A.2 (Boiling Temperature)
Deviations:
not specified
GLP compliance:
yes (incl. certificate)
Remarks:
Landesamt für Umwelt Rheinland-Pfalz; Mainz, Germany
Type of method:
differential scanning calorimetry

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder

Results and discussion

Boiling point
Decomposition:
yes
Remarks:
Onset bp under decomposition is 216.96 °C.
Decomp. temp.:
>= 170.05 - <= 271.94 °C

Any other information on results incl. tables

Preliminary Test Results

Pre-test following Siwoloboff-

All observations of the Pre-test following Siwoloboff are presented in the following table.

Note: test substance is a white powder.

Observations

Temperatures in °C

Test item began to shrivel

Since 120

Melted to a clear yellowish liquid with foam

220

Many bubbles were visible, color became darker

234

Bubble chain (Boiling),heating plate turned off

242

the chain of bubbles broke, test item is dark brown

231

After cooling down the test item was petrified as a brown solid.

Security Pre-test for the DSC instrument-

The crucible was found visually unchanged after reaching a temperature of 300 °C. The weight of the crucible was recorded with 47.42 mg.

Values DSC Indium-

Expected Melting point

Measured Melting point

Expected Energy

Measured Energy

Assessment

 

156.6±1.0°C

 

156.44 °C(onset)

 

28.45±1.0J/g

 

27.89J/g

 

OK

The measurement of indium after calibration met the validity criteria.

Values DSC Test Item first determination-

[°C]

Temperature [°C]

Energy

Begin Melting process

60.53(EventMarker)

19.58mW

End Melting process

115.68(EventMarker)

19.63mW

Begin boiling process

184.20(EventMarker)

19.42mW

End boiling process

Notdetected

-

Onset boiling point

217.06(Onset)

19.46mW

As the end of the Peak was not completely detected the end temperature was set to 300°C.

Values DSC Test Item second determination-

[°C]

Temperature [°C]

Heatflow

Begin Melting process

61.25(EventMarker)

19.56mW

End Melting process

113.61(EventMarker)

19.59mW

Begin boiling process

170.05(EventMarker)

19.40mW

End boiling process

271.25(EventMarker)

19.68mW

Onset boiling point

216.73(Onset)

19.49mW(Energy125.14J/g)

 

Values DSC Test Item third determination-

[°C]

Temperature [°C]

Heatflow

Begin Melting process

61.28(EventMarker)

19.92mW

End Melting process

90.20(EventMarker)

20.19mW

Begin boiling process

183.32(EventMarker)

19.37mW

End boiling process

269.71(EventMarker)

19.60mW

Onset boiling point

217.00(Onset)

19.44mW(Energy117.63J/g)

Values DSC Test Item fourth determination-

[°C]

Temperature [°C]

Heatflow

Begin Melting process

65.78(EventMarker)

19.91mW

End Melting Process

90.53(EventMarker)

20.11mW

Begin boiling process

189.72(EventMarker)

19.69mW

End boiling process

270.73(EventMarker)

19.78mW

Onset boiling point

217.07(Onset)

19.66mW(Energy124.24J/g)

Values DSC Test Item fifth determination-

[°C]

Temperature[°C]

Heatflow

Begin Melting process

65.99(EventMarker)

18.90mW

End Melting process

104.38(EventMarker)

19.21mW

Begin boiling process

185.25(EventMarker)

19.11mW

End boiling process

271.94(EventMarker)

19.31mW

Onset boiling point

216.92(Onset)

19.09mW(Energy129.04J/g)

Observations—

 

Mass test item

Mass crucible(before meas-urement):

Mass crucible(after meas-urement):

Observations

First Measurement

 

1.51mg

 

46.95mg

 

46.70mg

After the test the crucible was visually unchanged

Second Measurement

 

1.52mg

 

46.80mg

 

46.41mg

 

After the test the crucible was visually unchanged

Third Measurement

 

1.52mg

 

47.02mg

 

46.52mg

 

After the test the crucible was visually unchanged

FourthMeasurement

 

1.52mg

 

47.25mg

 

46.88mg

 

After the test the crucible was visually unchanged

 

Fifth Measurement

 

 

1.53 mg

 

 

47.14mg

 

 

46.87mg

After the test the crucible was visually unchanged.After the test, the crucible was opened and a brown residue was visible.

Interpretation of the measurements-

Based on the observations of the pre-test, the events between 60.53 °C and 115.68 °C should be interpreted as melting range. The broad peak at the end can be interpreted as boiling point. In the pre-test and after opening the crucible, observations were made which indicate decomposition. Therefore, the boiling point is stated as boiling under decomposition and it will be given in a range.

 

Results Summary-

For the calculation of the values of the mean and the standard deviation, only the second and third determination was taken into account.

Beginning of melting process

in°C(eventmark)

inK

1Determination

60.53

333.68

2Determination

61.25

334.40

3Determination

61.28

334.43

4Determination

65.78

338.93

5Determination

65.99

339.14

Min

60.53

333.68

Endofmeltingprocess

in°C(eventmark)

inK

1Determination

115.68

388.83

2Determination

113.61

386.76

3Determination

90.20

363.35

4Determination

90.53

363.68

5Determination

104.38

377.53

Max

115.68

388.83

Beginning of boiling process under decomposition

 

in °C(eventmark)

 

in K

1Determination

184.20

457.35

2Determination

170.05

443.20

3Determination

183.32

456.47

4Determination

189.72

462.87

5Determination

185.25

458.40

Min

170.05

443.20

End of boiling process

in°C(eventmark)

inK

1Determination

notcompletelydetected

notcompletelydetected

2Determination

271.25

544.40

3Determination

269.71

542.86

4Determination

270.73

543.88

5Determination

271.94

545.09

Max

271.94

545.09

On set boiling point

in°C(onset)

inK

1Determination

217.06

490.21

2Determination

216.73

489.88

3Determination

217.00

490.15

4Determination

217.07

490.22

5Determination

216.92

490.07

Mean

216.96

490.11

SD

0.14

0.14

Discussion-

The determination of the boiling point of W-1108T was performed via DSC (differential scanning calorimetry). Based on the pre-test a boiling point under decomposition was determined under these circumstances as the second, broad endothermic event and it will be given in a range:

 

From 170.05 °C (443.20 K) to 271.94 °C (545.09 K)

with an onset of 216.96 °C (490.11 K)

 

The first endothermic event should be interpreted as melting process and will be given in a range from 60.53 °C to 115.68 °C.These values are the results from five independent determinations.

No observations were made which might cause doubts on the validity of the study outcome. Therefore, the result of the study is considered valid.

Applicant's summary and conclusion