Quaternary ammonium compounds, coco alkyltrimethyl, chlorides

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:

supporting study

Study period:

From February 14 to February 21, 2011

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

GLP compliance:

yes (incl. QA statement)

Type of method:

other: Capillary tube in a metal block

Key result

Decomposition:

yes

Decomp. temp.:

>= 200 °C

Remarks on result:

not determinable

Definitive Test, First Cycle

Replicate 1	Replicate 2	Replicate 3
163.5 °C: discolouration over orange to brown, beginning on the top	155 °C: discoloration over orange to brown, beginning on the top	161.7 °C: discolouration over orange to brown, beginning on the top
	200 °C: discoloured upper part melted to black liquid
	214 °C: bubbles in the black liquid arose
204 °C: upper part of the sample was carried out of the inspection window	218.8 °C: upper part of the sample was carried out of the inspection window	197.8 °C: upper part of the sample was carried out of the inspection window
230.7 °C: remaining test substance was carried out of the inspection window	230.2 °C: remaining test  substance was carried out of the inspection window	227.4 °C: remaining test  substance was carried out of the inspection window
1st cycle cancelled: no more test substance remained in the inspection window

Definitive Test, Second Cycle

Replicate 1	Replicate 2	Replicate 3
191.8 °C: begin of melting	ca. 162 °C: begin of melting	189.2 °C: begin of melting
209.8 °C: formation of gas		202.4 °C: formation of gas
210.2 °C: test item was carried out of the inspection window	209.8 °C: test item was carried out of the inspection window	215.3 °C: test item was carried out of the inspection window
2^ndcycle cancelled: no more test substance remained in the inspection window

At start temperature (100°C) of the third cycle all replicates were dark-brown to black liquids containing dark-brown solids.

Definitive Test, Third Cycle

Replicate 1	Replicate 2	Replicate 3
192.6 °C: test substance liquid and violent gas formation	194.5 °C: test substance liquid and violent gas formation	186.4 °C: test substance liquid and violent gas formation
3^rdcycle cancelled: no more test substance remained in the inspection window

In the fourth cycle the test substance appeared to be dark-brown to black. Starting at 200°C the test substance level started to sink. At 300°C only a small amount of the test substance remained. The test was cancelled since the test substance appears to be completely decomposed.

Validity criteria

It was not possible to obtain two independent measurements within ± 0.3 K. The lowest begin of melting of the test item TMAC (=lyophilised Arquad C-35) in the first cycle was determined to be 200°C. During three further repetitions a constant melting temperature was not observed. This indicates decomposition during the melting process. This conclusion was confirmed by the fact that the test item changed its colour to brown during the four heating cycles.

Conclusions:

Under study conditions, melting point of test substance was not determined due to decomposition at ≥200°C.

Executive summary:

A study was conducted to determine the melting point of the test substance, Coco TMAC, using a capillary tube in a metal block apparatus, according to OECD 102 and EU 440/2008 Method A.1, in compliance with GLP. It was not possible to obtain two independent measurements within ± 0.3 K. The lowest begin of melting of the test substance in the first cycle was determined to be 200 °C. During three further repetitions a constant melting temperature was not observed, which indicated decomposition during the melting process. This conclusion was confirmed by the fact that the test substance changed its colour to brown during the four heating cycles. Under study conditions, melting point of test substance was not determined due to decomposition at ≥200°C.

Reference 2

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 08 February, 2012 to 07 March, 2012

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

GLP compliance:

yes (incl. QA statement)

Type of method:

other: Differential scanning calorimetry as well as capillary method

Key result

Decomposition:

yes

Decomp. temp.:

> 160 °C

Remarks on result:

other: The test substance has no melting point at atmospheric pressure (1013 hPa) as it decomposes at a temperature >160°C.

First test series:

RT-80°C: In the temperature range of 42-70°C an endothermic effect was detected. At 80°C the test substance was still solid and its colour was unchanged. No mass loss of could be measured.

RT-140°C: In the temperature range of 35-85°Can endothermic effect was detected. In the temperature range of approx. 125-135°C a very small exothermal effect could be measured, which can be neglected due to its slight energy of <10 J/g. At 140°C the test substance was still solid and its colour was still slightly yellow. A slight mass loss of 0.09 mg (0.4%) could be measured.

RT-210°C: In the temperature range of 40-85°C an endothermic effect was detected. The measurement showed an exothermal effect in the temperature range of 165-210°C. At 210 °C the colour of the test substance changed to black and a minor mass loss of 1.79 mg (6%) could be measured.

RT-240°C: In the temperature range of 35-70°C an endothermic effect was detected. The measurement showed an exothermal effect in the temperature range of 170-200°C, directly followed by a second endothermic effect in the temperature range of 200-240°C. At 240 °C the colour of the test substance changed to black and a mass loss of 25.26 mg (94%) could be measured.

RT-300°C: In the temperature range of 45-85°C an endothermic effect was detected. The measurement showed an exothermal effect in the temperature range of 165-200°C, directly followed by a second endothermic effect in the temperature range of 200-255°C. At 300°C the colour of the test substance changed to black and a mass loss of 22.51 mg (95%) could be measured.

 

Second test series:

0-80 -0-140-0 -210-25°C: During heating up from 0°C to 80°C an endothermic effect in the temperature range of 30-80°C was observed. During cooling down from 80°C to 0°C neither endothermic nor exothermic effects were observed. During heating up again from 0°C to 140°C an endothermic signal was observed at 70-80°C two small exothermal effects in the temperature range of 105-130°C. During cooling down again from 140°C to 0°C neither endothermic nor exothermic effects were observed. During the subsequent heating up to 210°C an endothermic effect could be observed in the temperature range of 70-85°C and an exothermal effect could be observed in the temperature range of approximately 160-210°C. The cooling down to 25°C showed no thermal effect. A mass loss of 3.26 mg (13%) could be measured.

0-240-25°C: During heating up from 0°C to 240°C an endothermic effect in the temperature range from 35- 85°C could be observed. In the temperature range of approximately 1 20-130°C a small exothermal effect was detected. In the temperature range of 160-215°C a second exothermal effect was observed. During cooling down from 240°C to 25°C neither endothermic nor exothermic effects were observed. A mass loss of 28.25 mg (93%) could be measured.

0-300-25 °C: During heating up from 0°C to 300°C an endothermic effect in the temperature range from 35-85°C could be observed. In the temperature range of 160-195°C an exothermal effect was observed, directly followed by a second endothermic effect in the temperature range of 195-250°C. During cooling down from 300°C to 25°C neither endothermic nor exothermic effects were observed. A mass loss of 23.50 mg (94%) could be measured.

Measurements by the capillary method:

	Sample 1
Filling height	5 mm
Start (30˚C)	Slight yellow solid
195˚C	Surface of the sample changes to yellow and brown at increasing temperatures, still soild
240˚C	The brown surface of the sample starts melting and boiling
251˚C	The whole sample starts sintering
255˚C	The top of the sample moves through
259˚C	The whole sample melts after bubbling

The measurement with the capillary method confirmed the results of the DSC-measurements concerning the melting behavior.

Conclusions:

Under the study conditions, the test substance has no melting point at atmospheric pressure (1013 hPa). It undegoes decomposition before melting at a temperature >160°C.

Executive summary:

A study was conducted to determine the melting point of the test substance, TMAC C (98.4% active) using differential scanning calorimetry as well as capillary methods, according to OECD 102 and EU Method A.1 Guidelines in compliance with GLP . Under the study conditions, the test substance has no melting point at atmospheric pressure (1013 hPa). It undergoes decomposition before melting at a temperature >160°C. (Möller, 2012).

Description of key information

No melting point could be determined, as the test substance undergoes decomposition before melting at a temperature >160°C.

Additional information

The melting point was determined using differential scanning calorimetry (DSC) as well as capillary methods according to OECD Guideline 102 and EU Method A.1 (Möller, 2012).