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Reference
Endpoint:
relative self-ignition temperature (solids)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-03-01 - 2017-06-22
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
other: Recommendations on the TRANSPORT OF DANGEROUS GOODS: Manual of Tests and Criteria
Version / remarks:
Revision 6 (2015)
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: VDI 2263, sheet 1, Grewer Oven
Version / remarks:
1990
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Key result
Remarks on result:
not measured/tested
Remarks:
see endpoint 4.13 self-heating substances

Self-ignition in the Grewer Oven

In the investigation of self-ignition in the Grewer Oven for the pure test item, a small endothermic effect was detected in the temperature range of 40 – 90 °C, which may be caused by the drying of the test item. Starting at a temperature of approx. 170 °C the test item showed a slight self-heating, which did not led to a significant temperature increase in relation to the corresponding oven temperature. Due to this result the exothermic effect cannot be considered as a self-ignition of the test item. After the measurement a black residue remained in the basket.

For the test item in mixture with Kieselguhr an exothermic effect was detected, in the temperature range of 220 – 340 °C that led to a maximum temperature of approx. 710 °C (corresponding oven temperature 340 °C).

Table 1summarizes the results of the Grewer Oven experiment.

Table1: Results of the screening test for self-ignition in the Grewer Oven

Experiment

Onset self-
ignition / °C

Maximum temperature / °C

Remarks

Pure test item

---

---

Figure 4,Figure 5

Test item in mixture
with Kieselguhr (1:1)

220

710

Bowes-Cameron-Cage Test (UN Test N.4) -140 °C, 100 mm cube sample

The wire basket was only filled up to four fifths of the volume, due to a lack of test item. Nevertheless the filling level was considered as sufficient to verify the result of the Grewer oven test. The temperature in the centre of the sample exceeded the oven temperature by about 10 K within approximately 11 hours test time. Since the temperature increase is below threshold of 60 °C within 24 hours the result of the test is negative.

Conclusions:
Instead of the test on the relative self-ignition temperature according EC A.16. the test for self-heating substances according to Recommendations on the TRANSPORT OF DANGEROUS GOODS: Manual of Tests and Criteria: UN Test N.4 and the screening test in the Grewer oven according to VDI 2263, sheet 1 were performed, since these are now recommended for evaluation and classification.

Final Results / Classification:
In the Grewer oven the pure test item Leuco Sulfur Blue 20 indicated a slight self-heating at atmospheric pressure starting at a temperature of approx. 170 °C, which cannot be considered as a self-ignition of the test item.
In the Bowes-Cameron-Cage test with a 1 L wire basket at 140 °C the test showed a self-heating of the test item with a temperature increase of < 60 °C within 24 hours.

On the basis of the results of the tests on the self-ignition in the Grewer Oven test and the Bowes-Cameron-Cage test with a 1 L wire basket at 140 °C the item is classified as follows:
UN Transport Regulation: The test item has not to be classified as self-heating substance in class 4, division 4.2 according to the UN Transport Regulation.
GHS / CLP Regulation EC 1272/2008 Annex 1: 2.11: The test item has not to be classified as self-heating substance according to GHS/CLP Regulation EC 1272/2008 Annex 1: 2.11.
Executive summary:

Summary

In the Grewer oven the pure test item Leuco Sulfur Blue 20 indicated a slight self-heating at atmospheric pressure starting at a temperature of approx. 170 °C, which cannot be considered as a self-ignition of the test item.

In the Bowes-Cameron-Cagetest with a 1 L wire basket at 140 °C the test showed a self-heating of the test item with a temperature increase of < 60 °C within 24 hours.

According to the results of the tests on the self-ignition in the Bowes-Cameron-Cage Test (UN-Test N.4) the test item is classifiedas follows:

On the basis of the results of the tests on the self-ignition in the Grewer Oven test and the Bowes-Cameron-Cage test with a 1 L wire basket at 140 °C the item is classified as follows:

UN Transport Regulation: The test item has not to be classified asself-heating substancein class 4, division 4.2 according to the UN Transport Regulation.

GHS / CLP RegulationEC 1272/2008 Annex 1: 2.11: The test item has not to be classified as self-heating substance according to GHS/CLP Regulation EC 1272/2008 Annex 1: 2.11.

Description of key information

According to the results of the tests on the self-ignition in the Grewer Oven test and the Bowes-Cameron-Cage test with a 1 L wire basket at 140 °C the item Leuco Sulfur Blue 20 has not to be classified as self-heating substance according to EC 1272/2008 (CLP Regulation) Annex 1: 2.11.

Key value for chemical safety assessment

Additional information

Instead of the test on the relative self-ignition temperature according EC A.16. the test for self-heating substances according to Recommendations on the TRANSPORT OF DANGEROUS GOODS: Manual of Tests and Criteria: UN Test N.4 and the screening test in the Grewer oven according to VDI 2263, sheet 1 were performed, since these are now recommended for evaluation and classification.

Final Results / Classification:

In the Grewer oven the pure test item Leuco Sulfur Blue 20 indicated a slight self-heating at atmospheric pressure starting at a temperature of approx. 170 °C, which cannot be considered as a self-ignition of the test item.

In the Bowes-Cameron-Cage test with a 1 L wire basket at 140 °C the test showed a self-heating of the test item with a temperature increase of < 60 °C within 24 hours.

On the basis of the results of the tests on the self-ignition in the Grewer Oven test and the Bowes-Cameron-Cage test with a 1 L wire basket at 140 °C the item is classified as follows:

UN Transport Regulation: The test item has not to be classified as self-heating substance in class 4, division 4.2 according to the UN Transport Regulation.

GHS / CLP Regulation EC 1272/2008 Annex 1: 2.11: The test item has not to be classified as self-heating substance according to GHS/CLP Regulation EC 1272/2008 Annex 1: 2.11.