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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:
2018-04-19
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Deviations:
no
Qualifier:
according to
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
signed 2017-02-28
Type of method:
differential scanning calorimetry
Specific details on test material used for the study:
Storage conditions: Ambient temperature, dry, tightly closed in original container
Melting / freezing pt.:
>= 174 - <= 176 °C
Atm. press.:
1 016 hPa
Decomposition:
no
Sublimation:
no

Results

In the temperature range of 140 °C – 290 °C an endothermic effect (melting) was observed. No further thermic effects could be observed up to the maximum measured temperature of 500 °C.

Results of the DSC-measurements

 No. Sample weight [mg] Onset of Effect [°C]

Range of effect [°C]

Weight loss [mg]

Atmospheric pressure [hPa]

PN15513

10.99

 176.40       

 140 – 270 (endo)      

7.22

1016.0

PN15514

11.95

 174.53       

 150 – 290 (endo)       

7.75

1016.0

During the heating phase a distinct endothermic effect was observed in the temperature range of 140 – 290 °C, which can be assigned to the melting of the test item. As the onset temperatures in both tests do deviate by more than 0.5 K from their mean value of 175.47 °C, the test item has a melting range of 174 – 176 °C.

No further endothermic effects could be observed up to the maximum measured temperature of 500 °C.

Conclusions:
The test item di-Ammonium hydrogen citrate has a melting range of 174 – 176 °C at atmospheric pressure (1016 hPa) as determined by differential scanning calorimetry according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).
Endpoint:
melting point/freezing point
Type of information:
other: company data
Adequacy of study:
supporting study
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: company data
Qualifier:
no guideline followed
Principles of method if other than guideline:
DTA measurement with following conditions:
- Inweight: 2.29 mg
- Method: Screen Glas 30-500/3
- Temperature: 30.0 - 500 °C
- Heating rate: 3 °C/min
- single measurement
GLP compliance:
no
Type of method:
thermal analysis
Remarks:
DTA
Melting / freezing pt.:
167.15 °C
Decomposition:
no
Sublimation:
no

The test item showed one peak

Peak
Integral - 764.48 mJ
normalis. - 333.84 J/g
Onset 167.15 °C
Peak 172.38 °C

The test item showed no exothermal decomposition up to 500 °C.

Conclusions:
The test item showed no exothermal decomposition up to 500 °C and a peak with an onset temperature of 167.15 °C, which can be interpreted as the melting of the substance.

Description of key information

The test item di-Ammonium hydrogen citrate has a melting range of 174 – 176 °C at atmospheric pressure (1016 hPa).

Key value for chemical safety assessment

Additional information

In a key study according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995), the test item di-Ammonium hydrogen citrate has a melting range of 174 – 176 °C at atmospheric pressure (1016 hPa) as determined by differential scanning calorimetry.

Furthermore, the test item showed no exothermal decomposition up to 500 °C and a peak with an onset temperature of 167.15 °C (which can be interpreted as the melting of the substance) in a supporting study determined by a differential thermal analysis.