Registration Dossier

Administrative data

Endpoint:
auto-ignition temperature (liquids)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
From 05/04/2018 to 20/09/2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2018

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
EU Method A.15 (Auto-Ignition Temperature (Liquids and Gases))
Deviations:
no
Qualifier:
according to
Guideline:
other: DIN EN 14522 – Determination of the auto ignition temperature of gases and vapours, adopted December, 2005.
Deviations:
no
GLP compliance:
yes (incl. certificate)

Test material

Reference
Name:
Unnamed
Type:
Constituent

Results and discussion

Auto-ignition temperature (liquids / gases)
Key result
Auto-ignition temperature:
227 °C
Atm. press.:
>= 976 - <= 978 hPa

Any other information on results incl. tables

First trial:

 

The preselected auto-ignition temperature was set to 150°C.

Firstly,VORBprogram was used with an amount of 5 droplets for each test.

Ignition occurred for a sample temperature of 242.8°C.

 

Then H-A1 program and H-A2 program were conducted.

For the first determination, H-A1 program was performed from 238°C using 5 droplets by decreasing temperature in 5°C steps as ignition occurred.

At 228°C, ignition did not occur so the amount of test item that is injected was modified. Tests were performed with 2, 8 and 11 droplets but no ignition occurred.

 

H-A2 program was then used from 231°C using 5 droplets and the test were continued, in varying the amount of droplets and decreasing the temperature in 2°C steps.

The last ignition occurred at 231°C using 8 droplets and correspond to the first auto-ignition temperature (LASTIP on raw data).

 

For the second determination, temperature was then increased to the value obtained with VORB program (243°C) and H-A1 program was performed using 8 droplets. The same operatory mode as for the first determination was performed and the lowest auto-ignition was found at 231°C using 8 droplets.

 

A third determination was performed but the sample did not dropped into the Erlenmeyer and therefore measurement was stopped.

As the trial stopped before the end, a new trial was performed.

 

Second trial:

 

The preselected auto-ignition temperature was set to 243°C (VORB value from the previous trial).

Results of this trial are reported on Appendix I: Apparatus Data, Second trial at 243°C.

 

Firstly,VORBprogram was used with an amount of 5 droplets for each test.

Ignition occurred for a sample temperature of 250.1°C.

 

Then H-A1 program and H-A2 program were conducted.

For the first determination, H-A1 program was performed from 245°C using 5 droplets by decreasing temperature in 5°C steps as ignition occurred.

At 230°C, ignition did not occur so the amount of test item that is injected was modified. Tests were performed with 2 and 8 droplets.

Ignition occurred using 8 droplets and so the temperature was decreased to 225°C but no ignition occurred whatever the amount of droplets.

 

H-A2 program was then used from 228°C but no ignition occurred whatever the amount of droplets.

The last ignition occurred at 230°C using 8 droplets and correspond to the first auto-ignition temperature (LASTIP on raw data).

 

For the second determination, temperature was then increased to the value obtained with VORB program (250°C) and H-A1 program was performed using 8 droplets. The same operatory mode as forthe first determination was performed and the lowest auto-ignition was found at 230°C using 8 droplets.

 

A third determination was performed as for the second one and a lowest auto-ignition temperature of 230°C with 5 droplets was found.

 

The lowest value (230°C) wasreduced by the absolute deviation calculated using the reproducibility value (1.5% relative) and rounded up to the next 1 °C.

 

A final auto-ignition temperature (END IP VALUE in raw data) of 227°C was obtained.

 

The atmospheric pressure was 976hPaat the beginning of the test and 978hPaat the end of the test.

 

The following table summarised the protocol and the results obtained from the second trial:

 

Determination

Program

Temperature

Droplets

2

5

8

11

/

VORB

164.1

 

-

 

 

184.30

 

-

 

 

205.6

 

-

 

 

227.2

 

-

 

 

249.6

 

-

 

 

250.1

 

X

 

 

1

H-A1

245

 

X

 

 

240

 

X

 

 

235

 

X

 

 

230

-

-

X

 

225

-

-

-

-

H-A2

228

-

-

-

-

2

H-A1

250

 

X

-

 

245

 

X

 

 

240

 

X

 

 

235

 

X

 

 

230

-

-

X

 

225

-

-

-

-

H-A2

228

-

-

-

-

3

H-A1

250

 

X

-

 

245

 

X

 

 

240

 

X

 

 

235

 

X

 

 

230

 

X

 

 

225

-

-

-

-

H-A2

228

-

-

-

-

With    X : auto-ignition

- : no auto-ignition

 

Finally, three determinations were performed and then, three lowest auto-ignition temperatures were recorded as 230°C, 230°C and 230°C respectively using 8, 8 and 5 droplets.

 

As these temperatures did not differ by more than 2%, these results were considered as valid and the lowest value (230°C) wasretained. As described in DIN EN 14522:2005, the final auto-ignition temperature was obtained in reducing the retained value by the absolute deviation calculated using the reproducibility value (1.5% relative).

 

This value was rounded up to the next 1 °C and a final auto-ignition temperature (END IP VALUE in raw data) of 227°C was obtained.

 

Moreover, the apparatus control was performed less than 6 months before the test (controlon 27 April 2018 and measurements dated on 07 to 17 May 2018). The lowest auto-ignition temperature measured for each reference substance did not differ by more than 1.5% from the reference value.

 

Therefore, the results of this study were considered as valid.

 

Applicant's summary and conclusion

Conclusions:
Finally, three determinations were performed and then, three lowest auto-ignition temperatures were recorded as 230°C, 230°C and 230°C respectively using 8, 8 and 5 droplets.

As these temperatures did not differ by more than 2%, these results were considered as valid and the lowest value (230°C) was retained. As described in DIN EN 14522:2005, the final auto-ignition temperature was obtained in reducing the retained value by the absolute deviation calculated using the reproducibility value (1.5% relative).

This value was rounded up to the next 1 °C and a final auto-ignition temperature (END IP VALUE in raw data) of 227°C was obtained.
Executive summary:

A study was performed to determine the auto-ignition Temperature of the test item Tri-n-hexylamine under GLP. The method followed was designed to be compliant with the Council Regulation (EC) No 440/2008, Method A.15: “Auto-ignition Temperature (Liquids and gases)”. In this method, the auto-ignition temperature of the test item was determined by varying the temperature of the test vessel and the amount of test substance.

The lowest temperature where ignition occurs was retained and, in order to take into account all uncertainties (calibration, temperature measuring system, amount of substance etc.), this lowest value was reduced by the absolute deviation calculated using the reproducibility value (1.5% relative) as described in DIN EN 14522:2005.

Two trials were conducted. In the first one, the preselected auto-ignition temperature was set to 150°C and ignition occurred at 243°C (VORB program) but the test stopped automatically before the end because the substance did not dropped into the Erlenmeyer during a measurement. In the second one, the preselected auto-ignition temperature was set to 243°C and three auto-ignition temperature were recorded (recorded as LASTIP on raw data): 230°C, 230°C and 230°C.

As these three auto-ignition temperature obtained with the determination program did not differ by more than 2%, the results were validated and the lowest value (230°C) was reduced by the absolute deviation calculated using the reproducibility value (1.5% relative) as described in DIN EN 14522:2005.

This value was rounded up to the next 1 °C and a final auto-ignition temperature of 227°C was obtained.

The atmospheric pressure was 976 hPa at the beginning of the test and 978 hPa at the end of the test.