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Diss Factsheets

Physical & Chemical properties

Melting point / freezing point

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Administrative data

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Between 20 May 2012 and 04 October 2012.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Remarks:
Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of the relevant results. The study report was conclusive, done to a valid guideline and the study was conducted under GLP conditions, however no formal claim of GLP compliance was made.
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
no
Type of method:
differential scanning calorimetry
Key result
Decomposition:
yes
Remarks:
The test item has been determined to undergo rapid decomposition from approximately 150°C.
Decomp. temp.:
ca. 150 °C
Sublimation:
no

Results

Please see Attachment 1 for Thermograms and Thermographic Data.

Conclusions:
The test item has been determined to undergo rapid decomposition from approximately 150°C.
Executive summary:

The determination was carried out by differential scanning calorimetry (DSC) using a procedure designed to be compatible with Method A1 Melting/Freezing Temperature of Commission Regulation (EC) No 440/2008 of 30 May 2008 and Method 102 of the OECD Guidelines for Testing of Chemicals, 27 July 1995.

      

Discussion

Similar thermographic profiles were obtained using air and nitrogen atmospheres; this indicates that the observed decomposition in both determinations is probably thermal and not oxidative.

 

Conclusion

The test item has been determined undergo rapid decomposition from approximately 150°C.

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
supporting study
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Remarks:
The study was conducted in accordance with a relevant method, but not in compliance with GLP
GLP compliance:
not specified
Type of method:
thermal analysis
Decomposition:
yes
Decomp. temp.:
>= 100 - 300 °C

During the experiment, there were two significant phenomena; starting from 100 - 200°C, weight loss corresponding to 7.5% was obtained. Also, from 200 - 300°C, weight loss of 4.5% was observed, given a total weight loss of 12% for the sample during the thermal analysis.

Conclusions:
A total weight loss of 12% was observed during thermal analysis of the sample from 100 - 300°C. The result is considered to be reliable.

Description of key information

Melting point: The acid form (ATMP-N-Oxide acid) was observed to undergo thermal decomposition from approximately 150°C (Atwal 2012, Andreotti 2012). This conclusion is read across to the salt to indicate that ATMP-N-Oxide-5K will also undergo decomposition when heated.

Key value for chemical safety assessment

Additional information

The melting point of the anhydrous form of the parent acid (ATMP-N-Oxide) was determined using differential scanning calorimetry (DSC) in accordance with EU Method A.1 test method. ATMP-N-Oxide acid (anhydrous form) was observed to undergo thermal decomposition from approximately 150°C. The result is considered to be reliable and is selected as key study.

The key study was supported by a second study where the weight loss of ATMP-N-Oxide acid was measured during heating. A thermal decomposition of the parent acid was observed from 100 -300°C, this amounted to a total weight loss of 12% obtained using a TGA-FTIR method.

This results are read-across to the salt, ATMP-N-Oxide-5K, to indicate that the salt will also undergoes thermal decomposition when heated. Salts would be expected to melt at a higher temperature than the parent acid, and to decompose on heating.

A melting/freezing point value of -15°C was reported for an aqueous solution of ATMP-N-Oxide-5K in a secondary source to which no reliability could be assigned.