Reaction mass of (2E)-Tridec-2-enenitrile and (2Z)-Tridec-2-enenitrile and (3E)-Tridec-3-enenitrile and (3Z)-Tridec-3-enenitrile

Melting point / freezing point

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2015-05-13 to 2015-12-18

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

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

no

Remarks:

The study was conducted under supervision of a quality assurance unit which had ensured e.g instrumentation validation, reagent/materials certification, analyst certification and providing standard operating procedures.

Type of method:

differential scanning calorimetry

Key result

Melting / freezing pt.:

>= -40 - <= -37 °C

Atm. press.:

>= 1 005 - <= 1 014 hPa

Decomposition:

no

Sublimation:

no

During the cooling phase, an exothermal effect was observed at a temperature of approx. -40 °C, which was associated with the freezing of the test item. During the subsequent heating phase a distinct endothermic effect was observed in the temperature range of -60 to -10 °C, which was associated with the melting of the test item. As the onset temperatures in both tests deviate by more than 0.5 K from their mean value of -39.18 °C, a melting range of -42 to -37 °C was determined.

 

Sample weight / mg	Onset of Effect / °C	Range of effect / °C	Weight loss / mg	Atmospheric pressure / hPa
6.58	-36.8	-55 to -10 (endo)	6.73	1005.8
13.32	-41.56	-60 to -10 (endo)	13.08	1013.7

 

Conclusions:

The melting point of the test item was determined to bein range from -42 to -37 °C at 1005 and 1014 hPa.

Executive summary:

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1 and EPA OCSPP test guideline 830.7200 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with about 7 - 13 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. The substance is a liquid at ambient conditions. Therefore the crucibles were cooled down from ambient temperature to -100 °C with a constant cooling rate of 0.25 K/min under an inert atmosphere. After a waiting period of 30 min at -100 °C, the temperature was increased up to 500 °C at a constant heating rate of 10 K/min. In the temperature range of -60 to -10 °C, an endothermic effect (melting) was observed. As the onset temperatures in both tests deviate by more than 0.5 K from their mean value of -39.18 °C, a melting range of -42 to -37 °C was determined.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2015-05-13 to 2015-05-19

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

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Deviations:

no

GLP compliance:

no

Remarks:

The study was conducted under supervision of a quality assurance unit which had ensured e.g instrumentation validation, reagent/materials certification, analyst certification and providing standard operating procedures.

Type of method:

thermal analysis

Key result

Melting / freezing pt.:

-34.7 °C

Atm. press.:

1 013.25 hPa

Decomposition:

no

Sublimation:

no

During the cooling phase, an exothermal effect was observed at a temperature of approx. -50 °C, which was associated with the freezing of the test item. During the subsequent heating phase a distinct endothermic effect was observed in the temperature range of -50 to -10 °C, which was associated with the melting of the test item. The onset temperatures in both tests did not deviate by more than 0.5 K from their mean value of -34.74 °C. Thus, this temperature was determined as melting point.

Sample weight / mg	Onset of Effect / °C	Range of effect / °C	Weight loss / mg	Atmospheric pressure / hPa
8.80	-34.58	-45 to -10 (endo)	8.77	1005.2
9.79	-34.90	-50 to -15 (endo)	9.71	996.7

Conclusions:

The melting point of the test item was determined to be -34.7 °C at 1013.25 hPa.

Executive summary:

A study was conducted according to OECD test guideline 102, Regulation (EC) No 440/2008 method A.1 and EPA OCSPP test guideline 830.7200 to determine the melting point of the test item using differential scanning calorimetry. The test item was weighed out into an aluminium crucible under an inert atmosphere (nitrogen). Two tests with about 9 - 10 mg of the test item were performed. As reference crucible, an empty aluminium crucible was used. The substance is a liquid at ambient conditions. Therefore the crucibles were cooled down from ambient temperature to -50 °C with a constant cooling rate of 0.25 K/min under an inert atmosphere. After a waiting period of 30 min at -100 °C, the temperature was increased up to 500 °C at a constant heating rate of 10 K/min. In the temperature range of -50 to -10 °C, an endothermic effect (melting) was observed. The onset temperatures in both tests did not deviate by more than 0.5 K from their mean value of -34.74 °C. Thus, this temperature was determined as melting point of the test item.

Description of key information

The melting point was determined to be in range from -40 to -37 °C for Composition A and -34.7 °C at 1013.25 hPa for Composition B.

Additional information

Isomeric Composition A

A study was conducted according to OECD TG 102 to determine the melting point of the test item using differential scanning calorimetry. The onset temperatures in both tests deviate by more than 0.5 K from their mean value of -39.18 °C, thus a melting range of -42 to -37 °C was determined.

 

Isomeric Composition B

A study was conducted according to OECD TG 102 to determine the melting point of the test item using differential scanning calorimetry. The melting point of the test item was determined as mean of two independent measurements which did not deviate by more than 0.5 K from the mean value of -34.74 °C. Thus, this temperature was determined as melting point.