Sodium 4-(4-substitutedanilino)-4-substituedbut-2-enoate

Boiling point

Administrative data

Endpoint:

boiling point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

27 Jul - 16 Aug 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

GLP guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

EU Method A.2 (Boiling Temperature)

Version / remarks:

adopted in 2008

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

OECD Guideline 103 (Boiling Point)

Version / remarks:

adopted in 1995

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

Department of Health, London, UK

Type of method:

differential scanning calorimetry

Test material

Test material information

Constituent 1

Specific details on test material used for the study:

Storage conditions: room temperature in the dark

Results and discussion

Boiling point

Key result

Atm. press.:

ca. 1 013 hPa

Decomposition:

yes

Decomp. temp.:

> 224.8 °C

Any other information on results incl. tables

Results

The thermographic data for determinations 1 to 6 are shown in the following table.

Table 2

Thermal event	Interpretation	Temperature
		Determination 1		Determination 2
		[°C]	[K]	[°C]	[K]
Sharp endotherm	Loss of volatiles	89.78	362.9	89.47	362.6
Sharp endotherm	Loss of volatiles / water	112.31	385.5	111.90	385.1
Sharp endotherm	Loss of volatiles	224.88	498.0	224.11	497.3
Thermal event	Interpretation	Temperature
		Determination 3		Determination 4
		[°C]	[K]	[°C]	[K]
Sharp endotherm	Loss of volatiles	89.54	362.7	89.54	362.7
Sharp endotherm	Loss of volatiles / water	111.96	385.11	112.07	385.2
Sharp endotherm	Loss of volatiles	225.19	498.3	225.15	498.3
Thermal event	Interpretation	Temperature
		Determination 5		Determination 6
		[°C]	[K]	[°C]	[K]
Broad endotherm	Loss of volatiles	70.66	343.8	68.32	341.5

 

 

Overall result: The test item does not melt or boil before decomposition occurs above 224.8 °C (498.0 K). As the test item did not melt, no melting point could be determined. As the test item decomposed, no value for boiling point could be determined.

 

Discussion

Determinations were carried out in pre-pierced crucibles from ambient to 450 °C in nitrogen and air at a rate of 20 °C/min to determine if there was a boiling point (determinations 1 to 4), the residues obtained were a black solid with approximately 50% loss in weight. Manually pierced crucibles were used for testing from ambient to 140 °C in air at a rate of 1 °C/min to establish if there was a melting point (determinations 5 to 6), the residues obtained were a yellow powder with approximately 10-15% loss in weight.

Similar thermographic profiles were obtained using air and nitrogen atmospheres. This indicated that the decomposition seen at 224.8 °C (498.0 K) was probably thermal and not oxidative.

Thermographic profiles (determinations 1 to 4) show transitions at 89.6 °C (362.7 K) and 112.1 °C (385.2 K), combine these transitions with the information from determinations 5 and 6, test item heated to only 140 °C, providing a residue after heating of a yellow powder with approximately 10-15% loss of weight for all determinations. A metal block determination providing visual investigation for this temperature region, showing that the test item began to “sweat” within the same temperature regions. The sample contains approximately 13% water, information supplied by sponsor, therefore these transitions can be concluded to be the loss of low boiling point volatiles and/or water within the test item.

Conclusion

The test item did not melt or boil before decomposition occurs above 224.8 °C (498.0 K). As the test item decomposed prior to melting, the melting and boiling points could not be determined.