4-chloroformylphthalic anhydride

Melting point / freezing point

Link to relevant study record(s)

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 15 July 2015 to 30 September 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Study performed according to recognized international guidelines. No deviation from the guideline was observed in the study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

July 27, 1995

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

Regulation (EC) 440/2008

Deviations:

no

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

March 1998

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

other: differential scanning calorimetry

Specific details on test material used for the study:

4-chloroformylphthalic anhydride

Key result

Melting / freezing pt.:

66 °C

Preliminary test:

The test substance was heated at a rate of 20°C/minute from 25°C to 342°C. At this point, 70% weight loss of the test substance was observed.

Main test:

Three experiments have been performed, under nitrogen and at atmospheric pressure:

Experiment	1	2	3
Sample amount (mg)	3.78	3.02	3.42
Crucible	Aluminium, pierced	Aluminium, pierced	Aluminium, pierced
Initial temperature (°C)	25	-25	-25
Rate (°C/min)	20	20	20
Temperature 2 (°C)	---	100	---
Rate (°C/min)	---	-5	---
Temperature 3 (°C)	---	-50	---
Rate (°C/min)	---	20	---
End temperature (°C)	316	150	150

In experiment 1, an endothermic peak between 50°C and 100°C was observed. The extrapolated onset temperature of the peak could not be determined since it was observed within 2 minutes from the start of the experiment. The effect was most likely obtained due to melting of the test item.

To investigate this peak, a repeated heating cycle was applied in the experiment 2, starting at a lower temperature.

With the first heating phase, the extrapolated onset temperature of the melting peak was 66.25°C.

During cooling, no effects were observed which were due to crystallization of the test substance.

With the second heating, an exothermic peak between 0°C and 50°C was observed. The effect was obtained due to crystallization of the test item. Second heating in combination with cooling provides enough time for test item to crystalize at lower temperatures. Then, a further endothermic effect, due to melting of the test item, was recorded with an extrapolated onset temperature of 65.67°C. This value was not used for calculation of the melting temperature, since it was obtained by melting of non-original test substance. After the experiment, a colourless molten residue remained in the sample container.

Experiment 3 was performed to determine the duplicate melting temperature of the test item. The extrapolated onset of the melting peak was 66.10°C. After the experiment, a colourless molten residue remained in the sample container.

The melting temperature was determined as the average melting temperature obtained from Experiment 2 (66.25°C) and Experiment 3 (66.10°C).

Conclusions:

The melting point of the test item is 66°C.

Executive summary:

The melting point of the test item was determined with Differential Scanning Calorimetry (DSC), according to recognized guidelines (OECD Guideline 102, EU Method A.1 and EPA OPPTS 830.7200) and under GLP. No deviations from the guidelines have been observed during the test.

Two consistent determinations, under nitrogen atmosphere, provided an average melting point of 66°C.

Description of key information

The melting point of the test item is 66°C.

Key value for chemical safety assessment

Melting / freezing point at 101 325 Pa:

66 °C

Additional information

The melting point of the test item was determined with Differential Scanning Calorimetry (DSC), according to recognized guidelines (OECD Guideline 102, EU Method A.1 and EPA OPPTS 830.7200) and under GLP. No deviations from the guidelines have been observed during the test.