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Administrative data

Endpoint:
melting point/freezing point
Type of information:
experimental study
Adequacy of study:
key study
Study period:
02 June 2015-18 August 2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: GLP-compliant study in accordance with EC A.1 and OECD 102.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2015
Report date:
2015

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
EU Method A.1 (Melting / Freezing Temperature)
Version / remarks:
(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
Type of method:
thermal analysis
Remarks:
(differential scanning calorimetry)

Test material

Constituent 1
Chemical structure
Reference substance name:
(2S)-2-(1,3-DIOXO-2,3-DIHYDRO-1H-ISOINDOL-2-YL)PENTANEDIOIC ACID
EC Number:
608-945-6
Cas Number:
340-90-9
Molecular formula:
C13H11NO6
IUPAC Name:
(2S)-2-(1,3-DIOXO-2,3-DIHYDRO-1H-ISOINDOL-2-YL)PENTANEDIOIC ACID
Test material form:
solid: particulate/powder
Remarks:
migrated information: powder
Details on test material:
- Name (as cited in study report): Phthalyl-L-Glu
- Appearance: white powder
- Storage conditions: room temperature

Results and discussion

Melting / freezing point
Melting / freezing pt.:
161 °C
Decomposition:
yes
Decomp. temp.:
200 °C
Remarks on result:
other: Melt. pt: 434 K. Decomp. temp: 473 K.

Any other information on results incl. tables

TGA EXPERIMENT

From 300°C upwards the weight of the sample decreased significantly. At 359°C, the sample weight had decreased by 25%. After the experiment, a black molten residue remained in the sample container.  

 

DSC EXPERIMENT 1

An endothermic peak between 125°C and 200°C was observed. The endothermic peak had two maxima; with extrapolated onset temperatures of 156.67°C and 160.73°C. The effect was most likely obtained due to melting of the test substance. Two endothermic peaks were observed from 200°C. The effect was most likely obtained due to reaction and/or decomposition of the test substance. After the experiment, a dark brown molten residue remained in the sample container.  

 

DSC EXPERIMENT 2

To investigate reaction and/or decomposition, a lower heating rate of 5°C/minute was applied. The extrapolated onset temperatures were 155.63°C and 160.38°C. The similar result obtained demonstrated that melting of the test substance was the reason for the endothermic effect. Since a lower heating rate was applied, the extrapolated onset temperatures were not used for calculation of the melting temperature. After the experiment, a dark brown molten residue remained in the sample container.

 

DSC EXPERIMENT 3

To investigate the melting peak, a repeated heating cycle was applied. With the first heating the extrapolated onset temperatures were 156.69°C and 160.30°C.  During cooling a glass transition was observed between 0°C and 50°C.  With the second heating, a glass transition was observed between 25°C and 75°C. The inflection point of the glass temperature was 49.43°C. The results demonstrated that the endothermic effect was due to melting of the test substance. After the experiment, a dark brown molten residue remained in the sample container.

Applicant's summary and conclusion

Conclusions:
In a GLP-compliant study in accordance with EC A.1, OECD 102 and EPA OPPTS 830.7200 using differential scanning calorimetry, the melting temperature of the substance has been determined as 161°C. Decomposition started at 200°C.