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Diss Factsheets

Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
27 August - 11 September 2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019
Report date:
2019

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
EC No. 440/2008
Deviations:
no
Qualifier:
according to guideline
Guideline:
OECD Guideline 102 (Melting point / Melting Range)
Version / remarks:
1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7200 (Melting Point / Melting Range)
Version / remarks:
1998
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
differential scanning calorimetry

Test material

Constituent 1
Chemical structure
Reference substance name:
5-amino-2-nitrobenzoic acid
EC Number:
236-283-4
EC Name:
5-amino-2-nitrobenzoic acid
Cas Number:
13280-60-9
Molecular formula:
C7H6N2O4
IUPAC Name:
5-amino-2-nitrobenzoic acid
impurity 1
Chemical structure
Reference substance name:
Water
EC Number:
231-791-2
EC Name:
Water
Cas Number:
7732-18-5
Molecular formula:
H2O
IUPAC Name:
Oxidane
impurity 2
Reference substance name:
Unknown impurities.
Molecular formula:
Not available as unknown impurities.
IUPAC Name:
Unknown impurities.
Test material form:
solid
Details on test material:
Batch / Lot No. 10044431
Specific details on test material used for the study:
Batch No.: 10044431
Storage Conditions: Room temperature (approx. 15 to 25 °C)

Results and discussion

Melting / freezing point
Key result
Melting / freezing pt.:
249.5 °C
Atm. press.:
1 004.3 hPa
Decomposition:
yes
Decomp. temp.:
ca. 250 °C

Any other information on results incl. tables

During the heating phase a distinct endothermic effect was observed in the temperature range of 240 – 250 °C, which can be assigned to the melting of the test item. The endothermic effect was directly followed by an exothermic effect starting at a temperature of approx. 250 °C with an average decomposition energy of -750 J/g.

 No.  Sample weight (mg)  Onset of effect (°C)  Range of effect (°C)  Weight loss (mg)  Atmospheric pressure (hPa)
 PN18264
 9.44 249.65

240 - 250 (endo)

250 - 320 (exo)

5.04  1004.3
 PN18265 10.58  249.26

240 - 250 (endo)

250 - 320 (exo)

4.69

 1004.3

As the onset temperatures in both tests deviate by less than 0.5 K from their mean value of 249.46 °C, this temperature can be used as melting point. The test item has a melting point of 249.5 °C accompanied by its decomposition.

Optical verification using the capillary method

To verify the results of the DSC measurement, an additional measurement in a melting capillary was performed in the temperature range of 200 °C to 260 °C with a heating rate of 10 K/min. Starting at a temperature of 240 °C change in colour to a darker tone could be observed. At a temperature of 250 °C the test item was completely molten and turned black. The test was terminated at a maximum temperature of 260 °C. After the measurement a black residue remained in the capillary.

According to the observations during the test in the capillary method, the effects in the DSC measurements with open crucibles can be assigned to the melting of the test item accompanied by its decomposition in the temperature range of 240 °C to 250 °C.

Applicant's summary and conclusion

Conclusions:
The test item 5-Amino-2-nitrobenzoic acid (CAS no. 13280-60-9) has a melting point of 249.5 °C at atmospheric pressure (1004.3 hPa) accompanied by its decomposition starting at a temperature of approx. 250 °C as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).
Executive summary:

The test item 5-Amino-2-nitrobenzoic acid (CAS no. 13280-60-9) has a melting point of 249.5 °C at atmospheric pressure (1004.3 hPa) accompanied by its decomposition starting at a temperature of approx. 250 °C as determined by differential scanning calorimetry and capillary method according to Regulation EC No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).