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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:
October 2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
other: UN Manual of Tests and Criteria, ST/SG/AC. 10/11/Rev.5
Version / remarks:
2009
Deviations:
no
GLP compliance:
no
Remarks on result:
other: Detonation (Test Series A): BAM 50/60 Steel Tube Test (Test A.1)
Remarks:
No detonation - Fragmentation length shorter than 1.5 times comparative length, i.e. < 18.75 cm.
Remarks on result:
other: Deflagration (Test Series C): Time / Pressure Test (Test C.1).
Remarks:
“No” (Gauge pressure 2070 kPa not achieved).
Remarks on result:
other: Deflagration Test (Test C.2).
Remarks:
“No deflagration” was detected.
Remarks on result:
other: Heating Under Defined Confinement: Koenen Test (E.1)
Remarks:
Tubes unchanged: Concluding result “no”.
Remarks on result:
other: Heating Under Defined Confinement: Dutch Pressure Vessel Test (E.2)
Remarks:
The limiting diameter is < 1.0 mm.
Remarks on result:
other: Test on Explosion Power, BAM Trauzl Test (Test F.3)
Remarks:
The sample has no explosive power.
Remarks on result:
other: Performance of the SADT Test
Remarks:
The SADT of the test material is ≥ 60 °C.

Detonation (Test Series A): BAM 50/60 Steel Tube Test (Test A.1).

Sample conditions: Ambient temperature (12 – 14 °C)

Fragmentation length: 12.3 cm / 12.7 cm

Comparative fragmentation length with an inert substance (water) 12.5 cm.

Result: No detonation - Fragmentation length shorter than 1.5 times comparative length, i.e. < 18.75 cm.

Deflagration (Test Series C): Time / Pressure Test (Test C.1).

Sample conditions: Ambient temperature (16 – 18 °C).

The sample was investigated at ambient temperature.

Trial 1: Maximum pressure 560 kPa.

Trial 2: Maximum pressure 452 kPa.

Trial 3: Maximum pressure 473 kPa.

In none of the three trials a pressure rise to 2070 kPa above atmospheric pressure was achieved.

Evaluation: “No” (Gauge pressure 2070 kPa not achieved).

Deflagration Method 2: Deflagration Test (Test C.2).

Sample masses: 254 g / 256 g.

Sample conditions: 50 °C

The substance could not be ignited within 5 minutes during application of a gas burner flame.

Thus, “no deflagration” was detected.

 

Conclusion on Propagation of Deflagration

According to the results of the tests C1 and C2 the test material is not able to propagate a deflagration. The answer is “no” if the deflagration test (C.2) result is “no” and the time/pressure test (C.1) result is not “yes rapidly” according to the UN Manual of Tests and Criteria, Section 23, point 23.2.2.

Heating Under Defined Confinement: Koenen Test (E.1)

Sample mass: 27.3 g

Orifice diameter 20.0 mm: Tube unchanged / No explosion.

Orifice diameter 12.0 mm: Tube unchanged / No explosion.

Orifice diameter 8.0 mm: Tube unchanged / No explosion.

Orifice diameter 5.0 mm: Tube unchanged / No explosion.

Orifice diameter 3.0 mm: Tube unchanged / No explosion.

Orifice diameter 2.0 mm: Tube unchanged / No explosion.

Orifice diameter 1.5.0 mm: Tube unchanged / No explosion.

Orifice diameter 1.0 mm: Tube unchanged / No explosion.

Orifice diameter 1.0 mm: Tube unchanged / No explosion.

Orifice diameter 1.0 mm: Tube unchanged / No explosion.

Limiting diameter: < 1.0 mm

It was found that the limiting diameter is less than 1.0 mm and the effect in all tests was type “O” (tubes unchanged).

Concluding result: “No”.

Heating Under Defined Confinement: Dutch Pressure Vessel Test (E.2)

Sample Mass

Orifice Diameter

Effect / Assessment

(+ Rupture, - No rupture)

10 g

16.0 mm

No rupture / -

10 g

6.0 mm

No rupture / -

10 g

2.0 mm

No rupture / -

10 g

1.0 mm

No rupture / -

50 g

1.0 mm

No rupture / -

50 g

1.0 mm

No rupture / -

50 g

1.0 mm

No rupture / -

 

The limiting diameter is < 1.0 mm.

Concluding result: “No”.

 

Concluding Result of the Effect of Heating Under Defined Confinement

According to the results of the tests E.1 and E.2 the concluding assessment of the effect under defined confinement is: “No”.

Test on Explosion Power, BAM Trauzl Test (Test F.3)

The results of two trials (sample masses: 10.7 g test 1 and 10.6 g test 2) are:

Test 1: 6.4 cm^3 expansion per 10 g sample.

Test 2: 6.4 cm^3 expansion per 10 g sample.

In both cases the volume of expansion of the lead block was less than 10 cm^3 per 10 g sample. Therefore it can be stated that the sample has no explosive power.

The assessment result: “No”.

The question “what is the effect of heating it under confinement” led to the answer “No”. Therefore Exit G had to be selected.

 

Concluding Result of the Flow Chart Testing.

With reference to all test results “Exit G” (should be considered for exemption) was reached in the flow-chart scheme. According to the classification procedure for self-reactive substances (point 20.4.2 “g”) the sample should be exempted from classification as a self-reactive substance of Division 4.1 provided that the formulation in thermally stable (self-accelerating decomposition temperature 60 °C to 75 °C for a 50 kg package) and any diluent meets the requirements of paragraph 2.4.2.3.5 of the Model Regulations (defined as self-reactive substance type G ,exit box G of figure 20.1).

Therefore the last and final step was the executing of an UN H.4 SADT-test.

 

SADT Test for Organic Peroxides of Div. 5.2 and self-reactive substances of Div. 4.1 (UN Recommendations on the Transport of Dangerous Goods, Manual of Tests and Criteria, ST/SG/AC.10/11/Rev. 5, New York and Geneva, 2009, Section 28.4.4, Test H4, Heat Accumulation Storage Test).

At the ambient temperature of 55 °C, the sample showed stability in the Dewar Vessel. Within the testing time period of Seven days (noted from the point when the sample reaches a temperature 2 K below the ambient temperature, i.e. 53 °C), the sample temperature did not exceed a temperature 6 K above the test chamber temperature, i.e. 61 °C (maximum temperature 58.2 °C).

According to the UN Test Manual, the H.4 SADT test is performed in steps of 5 °C. As the SADT is defined as the lowest ambient temperature at which instability is detected, the SADT of the sample tested is at least 5 K higher than 55 °C (which means 60 °C).

Therefore the SADT of the test material is ≥ 60 °C.

 

Concluding Assessment of all Test Results

The measurements according to the flow scheme (UN Manual of Tests and Criteria figure 20.1 a/b) led to “Exit G” (material should be considered for exemption).

The SADT test (representing a 50 kg transport package) was ≥ 60 °C.

Therefore it can be stated that the sample of the test material has not to be considered as a material of the transport class 4.1 “self-reactive substances".

Conclusions:
Under the conditions of the study, the test material is not considered as a self-reactive substance of transport class 4.1.
Executive summary:

In order to check whether the test material fulfils the criteria to be classified in Division 4.1 (self-reactive substances) the prescribed tests according to the flow-chart scheme for self-reactive substances (UN Recommendations on the Transport of Dangerous Goods, Manual of Tests and Criteria, CT/SG/AC.10/11/Rev. 5, 2009, section 20, fig. 20.1 a/b) were performed.

The BAM 50/60 steel tube test (Test A.1) resulted in no detonation - Fragmentation length was shorter than 1.5 times comparative length, i.e. < 18.75 cm.

The deflagration (Test Series C) time / pressure test (Test C.1) showed that in none of the three trials a pressure rise to 2070 kPa above atmospheric pressure was achieved. The evaluation was “No” (Gauge pressure 2070 kPa not achieved).

Deflagration test (Test C.2) showed the substance could not be ignited within 5 minutes during application of a gas burner flame. Thus, “no deflagration” was detected.

In the heating under defined confinement: Koenen Test (E.1) it was found that the limiting diameter is less than 1.0 mm and the effect in all tests was type “O” tubes unchanged”. Concluding result: “No”.

In the heating under defined confinement test using the Dutch Pressure Vessel Test (E.2) the limiting diameter is < 1.0 mm. Concluding result: “No”.

Test on explosion power using the BAM Trauzl Test (Test F.3) showed that in both cases the volume of expansion of the lead block was less than 10 cm^3 per 10 g sample. Therefore it can be stated that the sample has no explosive power.

These measurements led to “Exit G” (material should be considered for exemption).

The SADT test (representing a 50 kg transport package) was ≥ 60 °C.

Under the conditions of the study, the test material is not considered as a self-reactive substance of the transport class 4.1.

Description of key information

Autoflammabilty testing on 4-Oxo Tempo results in negative results for all tests (Habrich, J. 2014, report A140003711).

Key value for chemical safety assessment

Autoflammability / Self-ignition temperature at 101 325 Pa:
60 °C

Additional information

To identify whether the test material fulfils the criteria to be classified in Division 4.1 (self-reactive substances) the prescribed tests according to the flow-chart scheme for self-reactive substances (UN Recommendations on the Transport of Dangerous Goods, Manual of Tests and Criteria, CT/SG/AC.10/11/Rev. 5, 2009, section 20, fig. 20.1 a/b) were performed (Habrich, J. 2014).

The BAM 50/60 steel tube test (Test A.1) resulted in no detonation - Fragmentation length was shorter than 1.5 times comparative length, i.e. < 18.75 cm.

The deflagration (Test Series C) time / pressure test (Test C.1) showed that in none of the three trials a pressure rise to 2070 kPa above atmospheric pressure was achieved. The evaluation wasNo(Gauge pressure 2070 kPa not achieved).

Deflagration test (Test C.2) showed the substance could not be ignited within 5 minutes during

application of a gas burner flame. Thus,no deflagrationwas detected.

In the heating under defined confinement: Koenen Test (E.1) it was found that the limiting diameter is less than 1.0 mm and the effect in all tests was typeOtubes unchanged. Concluding result:No.

In the heating under defined confinement test using the Dutch Pressure Vessel Test (E.2) the limiting

diameter is < 1.0 mm. Concluding result:No.

Test on explosion power using the BAM Trauzl Test (Test F.3) showed that in both cases the volume

of expansion of the lead block was less than 10 cm^3 per 10 g sample. Therefore, it can be stated that the sample has no explosive power.

These measurements led toExit G(material should be considered for exemption).

The SADT test (representing a 50 kg transport package) was60°C.

Under the conditions of the study, the test material is not considered as a self-reactive substance of the transport class 4.1.

 

Additional supporting data is available in the form of adiabatic calorimetry on the Oxo Tempo concentrate (Tee, Waldram, 1999), tests for determination of transport classification of the formulated product (Brown, Fletcher, 1999) and Differential Scanning Calorimetry on formulated Oxo Tempo (McIntosh, Tee, 1999). Althou8gh providing useful information regarding the safe handling of the substance, the Habrich 2014 study is the only available guideline study. As a result, this study was taken as the key study and classification of the substance is based solely on the outcome of this study. 

According to the flow scheme (UN Manual of Tests and Criteria figure 20.1 a/b) the Habrich study results lead toExit G(material should be considered for exemption). Oxo Tempo is not considered as a self-reactive substance of transport class 4.1.