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Reference
Endpoint:
relative self-ignition temperature (solids)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-07-12 - 2018-03-06
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, 6th edition, New York and Geneva, 2015, Class 4, Division 4.2
Version / remarks:
Rev. 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)
Specific details on test material used for the study:
Reagents: Kieselguhr
Batch No.: TA2082010
Identity and content: Conforms
Certificate of analysis: Certificate of Analysis dated 2016-10-20; Merck KGaA, Frankfurter Straße 250, 64293 Darmstadt
Expiry date: 2021-10-31
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-heating in the Grewer Oven for the pure test item, an endothermic effect was detected in the temperature range of 40 – 150 °C, which may be caused by the drying of the test item. Starting at a temperature of approx. 160 °C the test item showed a self-heating, which leaded to a maximum temperature of 180 °C. After the measurement a black residue remained in the basket.

For the test item in mixture with Kieselguhr no endothermic or exothermic effects were detected.

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

160

180

Test item in mixture
with Kieselguhr (1:1)

--

--

On the basis of the results of the screening test on theself-heating in the Grewer Oven a classification of the test item as self-heating substance cannot be excluded. Further tests have to be performed for the classification.

Bowes-Cameron-Cage Test (UN Test N.4)

140 °C, 100 mm cube sample

The temperature in the centre of the sample did not exceed the oven temperature of 140°C over a time period of 24 h.

Due to the negative result in the 100 mm cube sample at an oven temperature of 140 °C no further tests had to be performed.

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.

In the Grewer oven the pure test item CI Solubilised Sulphur Black 1 indicated a self-heating at atmospheric pressure starting at a temperature of approx. 160 °C, which leaded to a maximum temperature of 180 °C.

The Bowes-Cameron-Cage test in the 1 L wire basket at 140 °C showed no self-heating of the test itemCI Solubilised Sulphur Black 1within 24 hours.

According to the result of the test on the self-ignition in the Bowes-Cameron-Cage Test (UN-Test N.4) the test item CI Solubilised Sulphur Black 1 is classified as follows:
UN Transport Regulation: On the basis of this result 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 and EC 1272/2008 (CLP Regulation) Annex 1: 2.11: On the basis of this result the test item has not to be classified as self-heating substance according to EC 1272/2008 (CLP Regulation) Annex 1: 2.11.
Executive summary:

Summary

In the Grewer oven the pure test item CI Solubilised Sulphur Black 1 indicated a self-heating at atmospheric pressure starting at a temperature of approx. 160 °C, which leaded to a maximum temperature of 180 °C.

The Bowes-Cameron-Cage test in the 1 L wire basket at 140 °C showed no self-heating of the test item CI Solubilised Sulphur Black 1 within 24 hours.

According to the result of the test on theself-ignition in the Bowes-Cameron-Cage Test (UN-Test N.4) the test item CI Solubilised Sulphur Black 1 is classified as follows:

UN Transport Regulation:On the basis of this result the test item has not to be classified asself-heating substancein Class 4 Division 4.2 according to the UN Transport Regulation.

GHS and EC 1272/2008 (CLP Regulation) Annex 1: 2.11:On the basis of this result the test item has not to be classified asself-heating substanceaccording to EC 1272/2008 (CLP Regulation) Annex 1: 2.11.

Description of key 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.

The Bowes-Cameron-Cage test in the 1 L wire basket at 140 °C showed no self-heating of the test item Solubilised Sulphur Black 1 within 24 hours.

According to the result of the test on the self-ignition in the Bowes-Cameron-Cage Test (UN-Test N.4) the test item Solubilised Sulphur Black 1 is not classified as self-heating substance in Class 4 Division 4.2 according to the UN Transport Regulation. It 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