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Auto flammability

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Reference
Endpoint:
auto-flammability
Type of information:
experimental study
Adequacy of study:
key study
Study period:
13-20 Oct 2015
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))
GLP compliance:
yes (incl. certificate)
Remarks:
Rheinland-Pfalz Landesamt für Umwelt, Wasserwirtschaft und Gewerbeaufsicht, Kaiser-Friedrich-Strasse 7, D-55116 Mainz
Auto-ignition temperature:
280 °C
Atm. press.:
ca. 1 000 hPa

Pre-determination:

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

T vessel (°C)

No. of drops used

Ignition y/n

Observation

200.7

5

n

fume

222.5

5

n

fume

246.2

5

n

fume

269.4

5

n

lots of fume

291.8

5

n

lots of fume

315.1

5

y

flame and plop ignition after 13 s

Selected T: 300 °C. The temperature was selected at the ZPA3 corresponding to an initial oven temperature of 200 °C. Using a constant heating rate, the subsequent ignition trials were conducted every 20 ± 5 K.

Atmospheric pressure during the pre-test was 99468 Pa.

First test series:

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

Used program

Selected T*

T vessel (°C)

No. of drops used

Ignition y/n

Observations

H-A1

333

333.4

5

y

flame and plop ignition after 11 s

H-A1

328

328.1

5

y

flame and plop ignition after 9 s

H-A1

323

323.3

5

y

flame and plop ignition after 9 s

H-A1

318

318.3

5

y

flame and plop ignition after 9 s

H-A1

313

313.3

5

y

flame and plop ignition after 9 s

H-A1

308

308.4

5

y

flame and plop ignition after 10 s

H-A1

303

303.4

5

n

fume

H-A1

303

302.5

9

n

lots of fume

H-A1

303

303.4

13

n

lots of fume

H-A1

303

303.4

17

n

lots of fume

H-A2

306

305.0

5

y

flame and plop ignition after 18 s

H-A2

304

303.5

5

y

flame and plop ignition after 12 s

H-A2

302

301.5

5

y

flame and plop ignition after 15 s

H-A2

300

300.5

5

y

flame and plop ignition after 25 s

H-A2

298

298.0

5

y

flame and plop ignition after 19 s

H-A2

296

296.1

5

y

flame and plop ignition after 22 s

H-A2

294

293.6

5

n

fume

H-A2

294

294.0

9

n

fume

H-A2

294

293.8

13

n

fume

H-A2

294

294.0

17

n

fume

* The selected temperature was suggested automatically by the ZPA3.

The first 10 ignition trials were conducted on 13. Oct. 2015 (atmospheric pressure during the trials 99468 Pa) and the other ones on 14. Oct. 2015 (atmospheric pressure during the trials 99706 Pa). Lowest value of the first test series is 296 °C.

Second test series:

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

Used program

Selected T*

T vessel (°C)

No. of drops used

Ignition y/n

Observations

H-A1

313

312.8

5

y

flame and plop ignition after 12 s

H-A1

308

308.2

5

y

flame and plop ignition after 12 s

H-A1

303

303.4

5

y

flame and plop ignition after 16 s

H-A1

298

298.2

5

n

lots of fume

H-A1

298

298.3

9

y

flame and plop ignition after 20 s

H-A1

293

293.1

9

y

flame and plop ignition after 21 s

H-A1

288

288.1

9

n

lots of fume

H-A1

288

288.4

5

y

flame and plop ignition after 25 s

H-A1

283

283.4

5

n

lots of fume

H-A1

283

283.4

9

n

lots of fume

H-A1

283

283.4

13

n

lots of fume

H-A1

283

283.4

17

n

lots of fume

H-A2

286

286.4

5

n

lots of fume

H-A2

286

286.4

9

y

flame and plop ignition after 29 s

H-A2

284

283.4

9

y

flame and plop ignition after 41 s

H-A2

282

282.2

9

n

lots of fume

H-A2

282

281.9

5

n

lots of fume

H-A2

282

282.4

13

y

lots of fume

H-A2

282

282.2

17

y

lots of fume

* The selected temperature was suggested automatically by the ZPA3.

The first 14 ignition trials were conducted on 15. Oct. 2015 (atmospheric pressure during the trials 99500 Pa) and the other ones on 16. Oct. 2015 (atmospheric pressure during the trials 99744 Pa). Lowest value of the second test series is 283 ° C.

Third test series:

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

Used program

Selected T*

T vessel (°C)

No. of drops used

Ignition y/n

Observations

H-A1

293

293.1

12

y

flame and plop ignition after 22 s

H-A1

288

288.2

12

n

lots of fume

H-A1

288

288.2

8

y

flame and plop ignition after 39 s

H-A1

283

282.5

8

n

lots of fume

H-A1

283

283.0

4

n

lots of fume

H-A1

283

283.0

12

n

lots of fume

H-A1

283

283.2

16

n

lots of fume

H-A1

283

283.2

20

n

lots of fume

H-A2

286

285.6

8

y

flame and plop ignition after 29 s

H-A2

284

284.0

8

y

flame and plop ignition after 34 s

H-A2

282

281.5

8

n

lots of fume

H-A2

282

281.7

4

n

lots of fume

H-A2

282

281.5

12

n

lots of fume

H-A2

282

281.9

16

n

lots of fume

H-A2

282

282.0

20

n

lots of fume

* The selected temperature was suggested automatically by the ZPA3.

The ignition trials were conducted on 19. Oct. 2015 (atmospheric pressure during the trials 100133 Pa). Lowest value of the third test series is 284 °C. As the difference of the three test series was more than 10 K, a fourth test series was also performed and the results of the last three test series were used for evaluation.

Fourth test series:

The ignition attempts of the fourth test series of the main determination are presented in the following table:

Used program

Selected T*

T vessel (°C)

No. of drops used

Ignition y/n

Observations

H-A1

293

292.8

8

y

flame and plop ignition after 29 s

H-A1

288

288.3

8

y

flame and plop ignition after 73 s

H-A1

283

288.2

8

y

flame and plop ignition after 60 s

H-A1

278

278.3

8

n

lots of fume

H-A1

278

278.2

4

n

lots of fume

H-A1

278

278.3

12

n

lots of fume

H-A1

278

278.2

16

n

lots of fume

H-A1

278

278.3

20

n

lots of fume

H-A2

281

281.2

8

y

flame and plop ignition after 50 s

H-A2

279

279.2

8

n

lots of fume

H-A2

279

279.2

4

n

lots of fume

H-A2

279

279.2

12

n

lots of fume

H-A2

279

279.4

16

n

lots of fume

H-A2

279

279.0

20

n

lots of fume

*The selected temperature was suggested automatically by the ZPA3. The ignition trials were conducted on 20. Oct. 2015 (atmospheric pressure during the trials 100219 Pa). Lowest value of the fourth test series is 281 °C.

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 below 300 °C) respectively 20 K (if auto ignition temperature is above 300 °C). The following lowest values were recorded:

Experiment

Value

Ignition delay

Drops used

First test series*

296°C

22 s

5

Second test series

283 °C

41 s

9

Third test series

284 °C

34 s

8

Fourth test series

281 °C

50 s

8

*The first test series was not used for evaluation because the deviation was too high in comparison to other test series.

The lowest value of the auto ignition temperature is 281 °C. This value was determined using 8 drops test item. The test item showed auto ignition after 50 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 280 °C.

As three lowest values of the main test have to lie within a range of 10 K (if auto ignition temperature is below 300 °C) respectively 20 K (if auto ignition temperature is above 300 °C), and the largest difference between measured ignition temperatures was 3 K, the result is considered valid.

Description of key information

280 °C (EU A.15)

Key value for chemical safety assessment

Autoflammability / Self-ignition temperature at 101 325 Pa:
280 °C

Additional information

The self-ignition temperature of the substance trihexyl phosphate (CAS No. 2528-39-4) was determined according to procedure and demands of EU-Method A.15 and DIN 51 794. The acceptable range which is demanded in the DIN standard was fulfilled.