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Auto flammability

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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:
EU Method A.15 (Auto-Ignition Temperature (Liquids and Gases))
Deviations:
no
Qualifier:
according to
Guideline:
DIN 51794 (Testing of mineral oil hydrocarbons - Determination of ignition temperature)
Deviations:
no
GLP compliance:
yes (incl. certificate)
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).