Formamide, N,N'-1,4-phenylenebis-, reaction products with 4-methyl-1,3-benzenediamine and sulfur, leuco derivatives

Melting point / freezing point

Administrative data

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-05-02 - 2017-09-15

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

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 (incl. QA statement)

Type of method:

thermal analysis

Test material

Test material information

Constituent 1

Reference substance name:

Formamide, N,N'-1,4-phenylenebis-, reaction products with 4-methyl-1,3-benzenediamine and sulfur, leuco derivatives

EC Number:

276-059-3

EC Name:

Formamide, N,N'-1,4-phenylenebis-, reaction products with 4-methyl-1,3-benzenediamine and sulfur, leuco derivatives

Cas Number:

71838-68-1

Molecular formula:

not applicable

IUPAC Name:

Reaction product of formamide, N,N'-1,4-phenylenebis- with 4-methyl-1,3-benzenediamine and sulfur, leuco derivatives

Test material form:

solid: particulate/powder

Details on test material:

Test Item: Leuco Sulfur Brown 26
Appearance: Dark, near black powder

Results and discussion

Melting / freezing point

Key result

Decomposition:

yes

Decomp. temp.:

ca. 250 °C

Remarks on result:

other: no melting point up to decomposition

Any other information on results incl. tables

1.1                  Melting and Boiling Point (DSC)

The test item showed two endothermic effects in the temperature ranges of 60 – 190 °C and 220 – 390 °C. No further thermal effects could be observed up to the maximum test temperature of 500 °C.

Table 1:    Results of the DSC-measurements

No.	Sample weight / mg	Onset of Effect / °C	Range of effect / °C	Weight loss / mg	Atmospheric pressure / hPa	Remark
PN13331	15.34	103.23 248.33	60 – 190 (endo) 220 – 390 (endo)	3.00	1007.1	Figure 1
PN13335	14.99	105.26 238.55	60 – 190 (endo) 220 – 390 (endo)	3.40	1004.6	Figure 2

During the heating phase two endothermic effects were detected the temperature ranges of 60 – 190 °C and 220 – 390 °C, which cannot be clearly assigned to a melting or a boiling of the test item.

1.2                  Measurements by the Capillary Method

To verify the results of the DSC measurement, two additional measurements with the capillary method (Apparatus:Stuart Melting Point SMP30) were performed in the temperature range of 50 – 400 °C with a heating rate of 10 K/min. According to the observationsduring the tests with the capillary method, the first endothermic effect in the temperature range of 60 – 190°C in the DSC measurements with open crucibles cannot be assigned to the melting of the test item, since the test item did not change its appearance.Since the test item contains 4.22 % water, it can be assumed, that the endothermic effect is caused by the drying of the test item.Starting at a temperature of approx. 250 °C the colour of the test item gets darker. Due to the fact that a small exothermic effect was observed in the DSC measurements for the determination of the thermal stability starting at a temperature of approx. 250 °C, it can be stated that the test item has no melting and boiling point up to its decomposition.

Applicant's summary and conclusion

Conclusions:

The test item Leuco Sulfur Brown 26 has no melting point up to its decomposition starting at a temperature of approx. 250 °C as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).

Executive summary:

Summary

The test item Leuco Sulfur Brown 26 has nomelting point up to its decomposition starting at a temperature of approx. 250 °C as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1., OECD Test Guideline 102 (1995), EPA OCSPP 830.7200 (1998) and CIPAC MT 1 (2009).