Reaction mass of pentasodium 2-{[4-chloro-6-(ethyl{3-[(2-sulfonatoethyl)sulfonyl]phenyl}amino)-1,3,5-triazin-2-yl]amino}-5-hydroxy-6-({2-sulfonato-4-[(4-sulfonatophenyl)diazenyl]phenyl}diazenyl)naphthalene-1,7-disulfonate and tetrasodium 2-[(4-chloro-6-{ethyl[3-(vinylsulfonyl)phenyl]amino}-1,3,5-triazin-2-yl)amino]-5-hydroxy-6-({2-sulfonato-4-[(4-sulfonatophenyl)diazenyl]phenyl}diazenyl)naphthalene-1,7-disulfonate

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

28 December 2005 to 11 April 2006

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

thermal analysis

Specific details on test material used for the study:

Identity: FAT 40824/A
Batch: Red ROE 805 BOP 04/05
Appearance: dark red powder
Purity: Organic part (Na-salt): approx. 82 %; Main component 1: approx. 36.2 %; Main component 2: approx. 27.5 %; Oligomers: 10 %
Expiration date: 01 October 2010
Storage: At room temperature at about 20 °C in a desiccator (hygroscopic)

Melting / freezing pt.:

> 400 °C

Remarks on result:

other: No additional information was provided

PRELIMINARY TEST

The DSC-curve of the preliminary test (heating rate of 20 K/min from 25 °C to 400 °C). There was an endothermic heat effect observed starting at 80.8 °C. An exothermic reaction started at about 290 °C. After the experiment, the sample was dark in color and formed agglomerates, but was still powdery and lost about 24 % of its mass.

 

MAIN TESTS

In order to determine the endothermic reaction more precisely, a first main test run was performed in the immediate vicinity of the peak temperature with the temperature rise adjusted to 10 K/min. 6.85 mg test item were heated up from 25 °C to 270 °C. A not well defined endothermic reaction started at about 61 °C. This heat effect was not due to melting since the test item was still a powder after the experiment. Further evaluation is beyond the scope of the study. To confirm the result obtained in the first main test, a second run was performed. A test item amount of 13.16 mg was heated up from 25 °C to 400 °C at a rate of 10 K/min. An endothermic reaction could be observed between about 73 °C and 224 °C, followed by an exothermic heat effect starting at about 290 °C. After the experiment, the sample had lost about 24 % of its mass and the sample was a black colored powder forming agglomerates.

Conclusions:

The melting point of the test material was determined to be >400 °C.

Executive summary:

A GLP-compliant melting study with FAT 40824/A was carried out according to OECD guideline 102 using thermal analysis method. The DSC-curve of the preliminary test (heating rate of 20 K/min from 25 °C to 400 °C). There was an endothermic heat effect observed starting at 80.8 °C. An exothermic reaction started at about 290 °C. After the experiment, the sample was dark in color and formed agglomerates, but was still powdery and lost about 24 % of its mass. In main test, An endothermic reaction could be observed between about 73 °C and 224 °C, followed by an exothermic heat effect starting at about 290 °C. After the experiment, the sample had lost about 24 % of its mass and the sample was a black colored powder forming agglomerates. Based on the study results, the melting point of the test material was determined to be >400 °C.

Description of key information

The melting point of the test material was determined to be >400 °C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

400 °C

Additional information

A GLP-compliant melting study with FAT 40824/A was carried out according to OECD guideline 102 using thermal analysis method. The DSC-curve of the preliminary test (heating rate of 20 K/min from 25 °C to 400 °C). There was an endothermic heat effect observed starting at 80.8 °C. An exothermic reaction started at about 290 °C. After the experiment, the sample was dark in color and formed agglomerates, but was still powdery and lost about 24 % of its mass. In main test, an endothermic reaction could be observed between about 73 °C and 224 °C, followed by an exothermic heat effect starting at about 290 °C. After the experiment, the sample had lost about 24 % of its mass and the sample was a black colored powder forming agglomerates. Based on the study results, the melting point of the test material was determined to be >400 °C.