1-Butanethiol, 4-[(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)thio]-

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

07 May 2015 - 16 November 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP-compliant study in accordance with EC A.1.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2015

Report date:

2015

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

(2008)

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

(1995)

Deviations:

no

Test guideline 3

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

(1998)

Deviations:

no

GLP compliance:

yes

Type of method:

thermal analysis

Remarks:

(differential scanning calorimetry)

Test material

Test material information

Constituent 1

Reference substance name:

4-[(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)thio]butane-1-thiol

EC Number:

811-734-3

Cas Number:

36097-07-1

Molecular formula:

C12 H13 F13 S2

IUPAC Name:

4-[(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)thio]butane-1-thiol

Test material form:

gas under pressure: refrigerated liquefied gas

Details on test material:

- Name of test material (as cited in study report): IN-1000
- Appearance: Dark amber liquid

Results and discussion

Melting / freezing point

Melting / freezing point 1

Melting / freezing pt.:

-31 °C

Decomposition:

yes

Decomp. temp.:

100 °C

Remarks on result:

other: Melt. pt: 243 K.

Melting / freezing point 2

Melting / freezing pt.:

-3 °C

Decomposition:

yes

Decomp. temp.:

100 °C

Remarks on result:

other: Melt. pt: 270 K.

Any other information on results incl. tables

TGA EXPERIMENT

From 200°C upwards the weight of the sample decreased significantly. At 302°C the sample weight had decreased by 25%. After the experiment, a brown/black residue remained in the sample container. The change of the colour indicated reaction and/or decomposition of the test substance.

DSC EXPERIMENT 1

During cooling two exothermic peaks were observed between -10°C and -60°C. The effects were obtained due to crystallization of the test substance. During heating an endothermic effect with two peaks between -75°C and 25°C was observed. The peak maxima of the peaks were -30.59°C and -3.09°C. The effect was most likely obtained due to melting of the test substance. An endothermic peak was observed from 175°C. The effect was due to reaction and/or decomposition of the test substance. After the experiment, a dark brown residue remained in the sample container.

DSC EXPERIMENT 2

Experiment 2 was performed to determine the duplicate melting temperature of the test substance. The peak maxima of the melting peaks were -30.52°C and -2.90°C. An endothermic peak was observed from 100°C. The effect was due to reaction and/or decomposition of the test substance. After the experiment, a dark brown residue remained in the sample container.

DSC EXPERIMENTS 3 and 4

A repeated heating cycle in hermetically closed cups was applied in Experiment 3 and 4 to further investigate the melting temperatures. In Experiment 3, with the first heating the peak maxima of the endothermic peaks were -30.37°C and - 2.74°C. With the second heating the peak maxima of the endothermic peaks were -30.47°C and -2.96°C. In Experiment 4, with the first heating the peak maxima of the endothermic peaks were -30.43°C and -2.99°C. With the second heating the peak maxima of the endothermic peaks were -30.45°C and -2.94°C. The similar endothermic peaks were observed as in Experiment 1 and 2, therefore it was concluded that two melting temperatures are not an artefact. Obtained values were not used in the calculation (as hermetically closed cups were applied).

MELTING TEMPERATURES

The melting temperatures were determined as the average melting temperatures obtained from Experiment 1 (-30.59°C and -3.09°C) and Experiment 2 (-30.52°C and -2.90°C).

Applicant's summary and conclusion

Conclusions:

Using differential scanning calorimetry, a melting/freezing range of -31°C/-3°C was determined. Reaction and/or decomposition started at 100°C. The study was performed in accordance with EC A.1, OECD 102 and EPA OPPTS 830.7200 guidelines and in compliance with GLP.