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Physical & Chemical properties

Melting point / freezing point

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Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From October 2, 2009 to November 5, 2009
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
Key result
Melting / freezing pt.:
> 633 K
Remarks on result:
other: Melting temperature could not be definitively determined because of the deliquescent nature of the test substance

Aliquots of the test substance were placed in an aluminium crucilble and assessed:

Determination

 Atmosphere

 Crucible lid

Mass taken(g)

1

Air (static)

Pierced

0.0130

2

nitrogen

Pierced

0.0107

3

Air (static)

Pre-Pierced

0.0138

The temperature was converted into Kelvin (K) using:

T(K)= t(C) + 273.15

Conclusions:
Under the study condition, it was difficult to determine the melting point because of the deliquescent behavior of the test substance. The test substance appeared not to melt below 633⁰K. However liquefaction readily occurs as a result of deliquescence, either due to absorption of atmospheric moisture or release of water from the monohydrated test substance (Fox, 2009).
Executive summary:

A study was conducted to determine the melting point/freezing point of the test substance according to EU Method A.1 and OECD Guideline 102, in compliance with GLP. The test was performed by using DSC (differential scanning calorimetry. Aliquots of the test substance in three replicates were placed in an aluminium crucilble and measured. The endotherm in determinations 1 and 2 at approximately 316⁰K was considered to be liquefaction of the test substance and not melting (residue in the crucibles). This was investigated with a sample of test substance exposed to air at room temperature which changed into a clear and colorless liquid. This process of deliquescence interferes with the measurement of the melting temperature. No endotherm was found at approximately 316⁰K in determination 3. However, at 425⁰K, smaller endotherm (compared to 1 and 2) occurred as a result of the sample being dried (residue in the crucible around the edges).This suggested that the sample liquefied but incompletely (presence of small particles). Under the study condition, it was difficult to determine the melting point because of the deliquescent behavior of the test substance. The test substance appeared not to melt below 633⁰K. However liquefaction readily occurs as a result of deliquescence, either due to absorption of atmospheric moisture or release of water from the monohydrated test substance (Fox, 2009).

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2008
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: Well conducted and well documented study with reliable results but not run according to GLP.
Principles of method if other than guideline:
Data from technical manual
GLP compliance:
no
Type of method:
method to determine freezing temperature
Remarks:
cold-plate method
Key result
Melting / freezing pt.:
>= 0 - <= 5.1 °C
Atm. press.:
1 atm
Conclusions:
Under the study conditions the freezing point (crystallization point) for the test substance ranges between  0-5.1°C depending on the density (Company data, 2008).

Executive summary:

A study was conducted to determine the melting point/freezing point of the test substance using a method from the Technical Manual, part A: chemical and physical properties, section A5: crystallisation temperature. Under the study conditions the freezing point (crystallization point) for the test substance was established to be within range of  0-5.1°C depending on the density (Company data, 2008).

Description of key information

Solid form: the melting point/freezing point was determined according to EU Method A.1 and OECD Guideline 102.

Brine: the melting point/freezing point was established using a method from the Technical Manual, part A: chemical and physical properties, section A5: crystallisation temperature.

Key value for chemical safety assessment

Additional information

Solid form: It was difficult to determine the melting point because of the deliquescent behavior of the test substance. The test substance appeared not to melt below 633⁰K. However liquefaction readily occurs as a result of deliquescence, either due to absorption of atmospheric moisture or release of water from the monohydrated test substance.

Brine: The freezing point (crystallization point) ranges between 0-5.1°C depending on the density.