Triethyl orthoacetate

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 2017-06-06 to 2017-06-07

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:

no

Qualifier:

according to guideline

Guideline:

DIN 51794 (Testing of mineral oil hydrocarbons - Determination of ignition temperature)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Key result

Auto-ignition temperature:

410 °C

Atm. press.:

1 013.25 hPa

Findings

Pre-Determination

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

Table 1: Ignition attempts pre-test

Selected T*	T Vessel	Drops used	Ignition?	Observations
°C	°C	#	yes/no
300	200.5	5	no	-
300	224.7	5	no	-
300	246.5	5	no	-
300	269.0	5	no	Fizzle at dropping
300	290.8	5	no	-
300	313.4	5	no	-
300	335.8	5	no	-
300	357.8	5	no	-
300	380.4	5	no	-
500	401.6	5	no	-
500	424.0	5	yes	Ignition after 8 s

* The temperature was selected at the ZPA3 corresponding to an initial oven temperature of 200 °C. As the test item showed no ignition at 380.4 °C, a higher temperature was selected for the subsequent ignition trials corresponding to a new initial oven temperature of 400 °C. Using a constant heating rate, the subsequent ignition trials were conducted every 20 ± 5 K. Atmospheric pressure during the pre-test was 98585 Pa.

First test series

The ignition attempts of the first test series of the main determination (using programs HA-1 and H-A2) are presented in the following table.

Table 2: ignition attempts first test series

Used program	Selected T*	T Vessel	Drops used	Ignition?	Observations
	°C	°C	#	yes/no
H-A1	420	419.3	5	yes	Plop and flame, ignition after 8 s
H-A1	415	415.5	5	no	-
H-A1	415	414.4	9	no	-
H-A1	415	414.2	13	no	-
H-A1	415	414.4	17	yes	Light plop, ignition after 13 s
H-A1	410	410.1	17	no	-
H-A1	410	409.1	13	yes	Light plop, ignition after 53 s
H-A1	405	404.7	13	no	**
H-A1	400	400.8	13	no	-
H-A1	400	400.8	9	no	-
H-A1	400	400.8	5	no	-
H-A1	400	400.5	17	no	-
H-A2	403	402.3	13	no	-
H-A2	403	402.4	9	no	-
H-A2	403	402.5	5	no	-
H-A2	403	402.3	17	no	-

* The selected temperature was suggested automatically by the ZPA3.

The atmospheric pressure during the trials was 98585 Pa.

Lowest value of the first test series was 410 °C.

** At 405 °C the detector detected hot vapour. Therefore, the measurement was a backfire and was not used for the value.

Second test series

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

Table 3: Ignition attempts second test series

Used program	Selected T*	T Vessel	Drops used	Ignition?	Observations
	°C	°C	#	yes/no
H-A1	410	409.8	13	no	-
H-A1	410	409.8	9	no	-
H-A1	410	409.8	5	no	-
H-A1	410	409.6	17	no	-
H-A1	415	414.9	13	no	-
H-A1	415	414.4	9	no	-
H-A1	415	415.0	5	no	-
H-A1	415	414.9	17	no	-
H-A1	420	420.1	13	no	-
H-A1	420	419.9	9	no	-
H-A1	420	419.8	5	yes	Plop and flame, Ignition after 12s
H-A1	415	415.7	5	no	-
H-A1	415	415.0	9	no	-
H-A1	415	415.2	13	no	-
H-A1	415	415.2	17	no	-
H-A2	418	418.0	5	no
H-A2	418	418.1	9	no	-
H-A2	418	418.1	13	no	-
H-A2	418	418.4	17	no	-

* The selected temperature was suggested automatically by the ZPA3.

The atmospheric pressure during the trials was 99631 Pa. Lowest value of the second test series is 420 °C.

Third test series

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

Table 4: Ignition attempts third test series

Used program	Selected T*	T Vessel	Drops used	Ignition?	Observations
	°C	°C	#	yes/no
H-A1	425	425.1	5	yes	Plop and flame, ignition after 14 s
H-A1	420	420.1	5	yes	Plop and flame, ignition after 15 s
H-A1	415	415.1	5	yes	Plop and flame, ignition after 11s
H-A1	410	410.1	5	no	-
H-A1	410	409.9	9	no	-
H-A1	410	409.7	13	no	-
H-A1	410	410.3	17	no	-
H-A2	413	412.4	5	no	-
H-A2	413	413.1	9	no	-
H-A2	413	413.1	13	no	-
H-A2	413	412.7	17	no	-

* The selected temperature was suggested automatically by the ZPA3.

The atmospheric pressure during the trials was 99631 Pa). Lowest value of the third test series is 415 °C.

Final Results

The requirements for repeatability of the DIN standard are stated as follows: Three lowest values of the main test had to lie within a range of 20 K (if auto-ignition temperature is above 300 °C).

The following lowest values were recorded:

Table 1: Lowest values main test

Experiment	Value	Ignition delay	Drops used
First test series	410 °C	53 s	13
Second test series	420 °C	12 s	5
Third test series	415 °C	11 s	5

The lowest value of the auto-ignition temperature is 410 °C. This value was determined using 13 drops test item. The test item showed auto-ignition after 53 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 410 °C.

Validity

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

Table 2: 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 autoignition temperatures above 300 °C). The largest difference between measured ignition temperatures was 10 K.

Conclusions:

The self-ignition temperature of the test item was determined to be 410 °C (rounded down to a whole multiple of 5 °C).

Executive summary:

A study was performed according to EU method A.15 (referring to DIN 51794 of May 2003) in order to determine the self-ignition temperature of the test item by using an ZPA-3 oven. The test item showed a self-ignition after 53 seconds. The lowest temperature, which was determined from three experiments with several replicates each, was defined as self-ignition temperature of the test item. Rounded down to a whole multiple of 5 °C, the self-ignition temperature of the test item was determined to be 410 °C.

Description of key information

The self-ignition temperature of the test item was determined to be 410 °C (rounded down to a whole multiple of 5 °C).

Key value for chemical safety assessment

Autoflammability / Self-ignition temperature at 101 325 Pa:

410 °C

Additional information

A study was performed according to EU method A.15 (referring to DIN 51794 of May 2003) in order to determine the self-ignition temperature of the test item by using an ZPA-3 oven. The test item showed a self-ignition after 53 seconds. The lowest temperature, which was determined from three experiments with several replicates each, was defined as self-ignition temperature of the test item. Rounded down to a whole multiple of 5 °C, the self-ignition temperature of the test item was determined to be 410 °C (reference 4.12-1).