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Physical & Chemical properties

Melting point / freezing point

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Link to relevant study record(s)

Reference
Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
14 September 2015 - 13 February 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Principles of method if other than guideline:
not applicable
GLP compliance:
yes (incl. QA statement)
Remarks:
GLP certificate attached
Other quality assurance:
ISO/IEC 17025 (General requirements for the competence of testing and calibration laboratories)
Type of method:
thermal analysis
Specific details on test material used for the study:
Test item without emulsifier was investigated.

Amidoamine (UVCB)
Pulcra ID: DE07_2014_012_BEL66 (amidoamine without emulsifier)
Physical state: pale yellowish solid at 20 °C
Batch No.: K8 4309 L481
Expiry date of batch: 09 March 2018
Purity: 100 % (UVCB)
Stability: stable under test conditions
Storage condition of test material: Room temperature, protected from light
Key result
Melting / freezing pt.:
98.7 °C
Decomposition:
yes
Decomp. temp.:
ca. 213 °C

Aliquots of test item were placed in aluminum crucibles and were subjected to a thermal program as shown in the following table. The appearance of the samples (residue) was recorded after the test.

The thermograms showed a broad endotherm consistent with softening and melting of a waxy substance. The extrapolated onset of the endotherm peak was reported as the melting temperature. Additional testing was performed to obtain a definitive melting temperature using a temperature gradient of 1 °C/minute up to 120 °C.

However, since these thermograms demonstrated a low response over the melting range, it was considered acceptable to report the extrapolated onset of determinations 1 and 2 as the melting temperature (see table 2).

Table 1

 Determination Mass taken [g]  Temperature program  Atmosphere  Crucible lid
 1  0.0053   25 to 400 °C at 20.0 °C/min  Nitrogen  Manually pierced x2
 2  0.0049  25 to 400 °C at 20.0 °C/min  Nitrogen  Manually pierced x2

Table 2

 Thermal event  Interpretation Temperature
             Endotherm   Determination 1 Determination 2  
   °C °C
 Start of melting/softening  59.8  333  59.8 333 
 Extrapolated onset (melting temperature)  98.9  372  98.6 372 
 Endotherm peak  102.9  376  103.3 376 
Conclusions:
The melting temperature of the test item was determined to be 98.7 ± 0.5 °C (372 ± 0.5 K).
Executive summary:

In the Klimisch 1 GLP study the melting point of amidoamine test item was determined with the DSC method according to OECD 102 and EU method A.1. The test item did not show melting up to 98 °C. From 213 °C the test item shows most probably a thermal decomposition with change in color. This study is considered relevant for the risk assessment.

Description of key information

The melting temperature of the test item was determined to be 98.7 ± 0.5 °C (372 ± 0.5 K).

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:
98.7 °C

Additional information