Quaternary ammonium compounds, C12-14 (even numbered) alkyl(hydroxyethyl)dimethyl, C12 alkylbis(hydroxyethyl)methyl, chlorides and amines, C12-14 (even numbered) alkyldimethyl, chlorides

Auto flammability

Link to relevant study record(s)

Reference

Endpoint:

auto-ignition temperature (liquids)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 22 October 2018 to 25 October 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.15 (Auto-Ignition Temperature (Liquids and Gases))

Deviations:

yes

Remarks:

Deviations were considered as uncritical by the study author

GLP compliance:

yes (incl. QA statement)

Key result

Auto-ignition temperature:

ca. 380 °C

Atm. press.:

ca. 101 325 Pa

Findings

Determination of the viscosity

The test substance was visually compared with the standard liquid Viscosity (50 mPa*s).The viscosity of the test substance was below 50 mPa/s.

Pre-Determination

Ignition range for pre-test 1

Selected T*		T Vessel	Drops used	Ignition?	Observations
°C		°C	#	yes/no
200		200.4	5	no	Smoke
300		300.2	5	no	Smoke
400		400.3	5	yes	Plop
Result given by the instrument
-	400.39		5	yes

The ignition attempts of the pre-determination program are presented in the following table.

Ignition attempts pre-test 2

Selected T*		T Vessel	Drops used	Ignition?	Observations
°C		°C	#	yes/no
300		300.2	5	no	Smoke
320		319.9	5	no	Smoke
340		340.2	5	no	Smoke
360		359.9	5	no	Smoke
380		380.4	5	yes	Plop
Result given by the instrument
-	385.11		5	yes

*The temperature was selected at the Zündwertprüfer 10-212-000 corresponding to an initial oventemperature of 300°C. Using a constant heating rate, the subsequent ignition trials were conducted every 20 ± 5 K. The ignition trials were conducted on 22. Oct. 2018. Atmospheric pressure during the pre-test was1011.9 mbar.

 

First Test Series

The ignition attempts of the first test series of the main determination are presented in the following table.

Ignition attempts first test series

Selected T*		T Vessel		Drops used		Ignition?		Observations
°C		°C		#		yes/no
390.1		390.5		5		yes		Plop
385.1		384.9		5		no		Smoke
385.1		385.2		7		no		Smoke
385.1		385.1		9		yes		Plop
383.1		383.4		9		yes		Plop
381.1		380.8		9		no		Smoke
381.1		380.9		7		no		Smoke
381.1		381.4		5		no		Smoke
381.1		381.0		13		yes		Plop
379.1		379.4		13		no		Smoke
379.1		379.2		9		yes		Plop
377.1		377.3		9		no		Smoke
377.1		377.4		13		no		Smoke
377.1		377.2		7		no		Smoke
377.1		376.8		5		no		Smoke
Result given by the instrument
-	379.79		9		yes after 84 seconds

*The selected temperature was suggested automatically by the ZPA3. The ignition trials were conducted on 22. Oct. 2018 (atmospheric pressure during the trials 1011.9 mbar) and the other ones on 23. Oct. 2018 (atmospheric pressure during the trials 1012.2 mbar. Lowest value of the first test series is 379.79 °C, the drops, which needed, are 9 and the time until the ignition was detected, are 84 seconds.

Second Test Series

The ignition attempts of the second test series of the main determination are presented in the following table.

Ignition attempts second test series

Selected T*		T Vessel		Drops used		Ignition?		Observations
°C		°C		#		yes/no
399.8		400.1		5		yes		Plop
394.8		394.7		5		no		Smoke
394.8		394.9		7		yes		Plop
392.8		393.1		7		yes		Plop
390.8		390.6		7		yes		Plop
388.8		388.9		7		yes		Plop
386.8		387.2		7		yes		Plop
384.8		385.1		7		yes		Plop
382.8		382.8		7		no		Smoke
382.8		382.9		9		no		Smoke
382.8		382.7		13		no		Smoke
382.8		382.5		5		no		Smoke
Result given by the instrument
-	384.71		7		yes after 67 seconds

*The selected temperature was suggested automatically by the ZPA3. All the ignition trials were conductedon 24. Oct. 2018 (atmospheric pressure during the trials 1005.5 mbar). Lowest value of the second test series is 384.71°C, the drops, which needed, are 7 and the time until the ignition was detected, are 67 seconds.

 

Third Test Series

The ignition attempts of the third test series of the main determination are presented in the following table.

Ignition attempts third test series

Selected T*		T Vessel		Drops used		Ignition?		Observations
°C		°C		#		yes/no
404.7		405.1		5		yes		Plop
399.7		400.0		5		yes		Plop
394.7		395.1		5		no		Smoke
394.7		394.5		7		no		Smoke
394.7		395.0		9		yes		Plop
392.7		393.0		9		yes		Plop
390.7		390.7		9		yes		Plop
388.7		388.6		9		yes		Plop
386.7		387.1		9		no		Smoke
386.7		386.8		13		yes		Plop
384.7		385.0		13		yes		Plop
382.7		383.0		13		no		Smoke
382.7		382.6		9		no		Smoke
382.7		382.7		7		no		Smoke
382.7		383.0		5		no		Smoke
Result given by the instrument
-	385.21		13		yes after 39 seconds

*The selected temperature was suggested automatically by the ZPA3. All the ignition trials were conductedon 25. Oct. 2018 (atmospheric pressure during the trials 1004.3 mbar). Lowest value of the third test series is 385.21 °C, the drops, which needed, are 13 and the time until the ignition was detected, are 39 seconds.

 

Result and Validity

Result

The requirements for repeatability of the DIN standard are stated as follows: Three lowest values of the main test have to lie within a range of 10 K (if auto ignition temperature is above 300 °C).

The following lowest values were recorded:

Lowest Values Main Test

Experiment	Value (rounded to integer)	Ignition delay	Drops used
First test series	380 °C	84 s	9
Second test series	385 °C	67 s	7
Third test series	385 °C	39 s	13

The lowest value of the auto ignitiontemperature is 380 °C. This value was determined using 9 drops test substance. The test substance showed auto ignition after 84 seconds. The auto ignition temperature (result of determination) is the lowest value from the lowest values of the three experiments, rounded down to a whole multiple of 5 °C. Therefore, the auto ignition temperature is stated as 380 °C.

Validity

In the DIN, the following limits are applied to the range of lowest values which may be used for evaluation:

Acceptable ranges

Auto ignition temp.	Range
> 300 °C	difference between three values of the main test max. 10 K

The three lowest values of the main test lay within a range of 10 K (as required for auto ignition temperatures above 300 °C). The largest difference between measured ignition temperatures was 5 K.

Discussion

The study was conducted according to procedure and demands of EU-Method A.15 and DIN 51794. The acceptable range which is demanded in the DIN standard was fulfilled. All measured values show good correlation. No observations were made which might cause doubts concerning the validity of the study outcome.

Deviations

Deviations from the Study Plan

No deviations from the study plan were ascertained.

Deviations from the Guideline

The following deviation from the Guideline was ascertained:

The Zündwertprüfer 10-212-000 instrument works with a program according to DIN EN14522. This is a deviation from the EU-Method A.15 “Auto Ignition Temperature (liquids and gases)” as this norm is not mentioned there. An additional deviation occurs, as the method describes, that after one variation of drops the 2°C test modus will start, even when an ignition has occurred (cf. the orange mark in the schema). In the DIN method 51794 steps of 5°C are proposed in this case. As shown in the schema above the endpoint of the different guidelines is the same. It is possible that more ignition trials will be conducted using the EN 14522. Therefore, this can be considered as uncritical.

Conclusions:

Under the study conditions, the auto-ignition temperature of the test substance was determined to be 380°C.

Executive summary:

A study was conducted to determine the auto-ignition temperature of the test substance, C12-14 HEDMAC ( 39.6% active), according to the EU A.15 Method, in compliance with GLP. The auto ignition temperature was determined in three independent determinations. A lowest value of the main test was determined to be 380°C. Under the study conditions, the auto-ignition temperature of the test substance was determined to be 380°C (Krebs, 2018).

Description of key information

The self-ignition temperature of the test substance (39.6% active) was determined according to EU Method A.15 (Krebs, 2019). 

Key value for chemical safety assessment

Autoflammability / Self-ignition temperature at 101 325 Pa:

380 °C