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Reference
Endpoint:
explosive properties of explosives
Type of information:
experimental study
Adequacy of study:
key study
Study period:
09 January - 23 May 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
The study was conducted according to an internationally recognised method, and under GLP. The substance is considered to be adequately characterised. Therefore full validation applies.
Qualifier:
according to
Guideline:
UN Manual of Tests and Criteria: Part I: Classification procedures, test methods and criteria relating to explosives of Class 1
Version / remarks:
United Nations, Recommendations on the transport of dangerous goods, Manual of tests and criteria, Sixth revised edition, 2015: Appendix 6
Deviations:
no
Qualifier:
according to
Guideline:
other:
Version / remarks:
OECD Guidelines for the Testing of Chemicals, Method No. 113, adopted 12. May 1981: “Screening Test for Thermal Stability and Stability in Air”
Deviations:
no
Principles of method if other than guideline:
Not applicable
GLP compliance:
yes (incl. certificate)
Remarks:
inspected on 20 and 21 June 2017 / signed on 04 September 2017
Test series:
other: Thermal stability DSC measurements
Method:
other: DSC measurements / closed crucible
Parameter:
other: heat of decomposition
Value:
658
Result:
other: Units J/g
Remarks on result:
neither a test for propagation of detonation nor a test for sensitivity to detonative shock is required because the exothermic decomposition energy of the organic substance is less than 800 J/g
Key result
Test series:
UN Test series 1
Method:
UN Test 1 (b): Koenen test
Parameter:
limiting diameter (mm)
Remarks:
<1 mm
Result:
result is considered "-" (negative)
Remarks on result:
other: no effect if heating under confinement
Key result
Test series:
UN Test series 1
Method:
UN Test 2 (b): Koenen test
Parameter:
limiting diameter (mm)
Remarks:
<1 mm
Result:
result is considered "-" (negative)
Remarks on result:
other: no effect if heating under confinement
Key result
Test series:
UN Test series 1
Method:
UN Test 8 (c): Koenen test
Parameter:
limiting diameter (mm)
Remarks:
<1 mm
Result:
negative, no violent effect on heating under confinement
Remarks on result:
other: no effect of heating under confinement
Key result
Test series:
UN Test series 1
Method:
UN Test 1 (c) (i): Time/pressure test
Parameter:
other: pressure and time
Result:
result is considered "-" (negative)
Remarks on result:
p < 2070 kPa
Key result
Test series:
UN Test series 1
Method:
UN Test 2 (c) (i): Time/pressure test
Parameter:
other: pressure and time
Result:
result is considered "-" (negative)
Remarks on result:
p < 2070 kPa
Key result
Test series:
UN Test series 1
Method:
other: Serie C. Test C.1: Time/pressure test
Parameter:
other: pressure and time
Result:
negative, no or slow deflagration
Remarks:
No ability of the substance under confinement to propagate a deflagration.
Remarks on result:
p < 2070 kPa

Thermal stability

Two DSC-measurements in closed glass crucibles with the test item showed an exothermal effect in the temperature range of 140 – 470 °C with a maximum energy release of 658 J/g. Above 470 °C the course of the baseline indicated a pressure rise.

Graphical presentation of the DSC runs is given on the experimental report. The results are summarised in the table below.

Table 4.14/1.-Thermal stability (DSC measurements)

Ident-No.

Weight / mg

Final temperature / °C

Temperature range / °C

Type of effect

Energy

/ J/g

36799

12.29

500

140 – 470

Exothermal

658

36803

14.36

500

140 – 270

280 – 470

Exothermal

Exothermal

105

481

Explosive properties

The explosive properties of the test item could not be excluded with DSC-measurements due to an energy release above 500 J/g. Due to an energy release above 500 J/g but below 800 J/g the next tests which would have to be performed according to test series 1 are time pressure test and Koenen test.

Koenen-Test:

Tests were performed with a circular nozzle plate with a hole of varying diameters. Table 2 shows the results of the thermal sensitivity.

10 tests were performed. The results are shown in Table 4.14/1.

Table 4.14/1.- Koenen-test

Amount

Diameter of orifice

t1

t2

Reaction

Effect

g

mm

s

s

26.8

20.0

20

>300

Flame

O

26.8

12.0

20

>300

Flame

O

26.8

8.0

22

>300

Flame

O

26.8

5.0

21

>300

Flame

O

26.8

3.0

21

>300

Flame

O

26.8

2.0

20

>300

Flame

O

26.8

1.5

19

>300

Flame

O

26.8

1.0

19

>300

Flame

O

26.8

1.0

19

>300

Flame

O

26.8

1.0

19

>300

Flame

O

t1: Time to the first reaction                 t2: Time to the main reaction        O: Tube unchanged

The results have to be evaluated as negative according to UN-tests 1(b), 2(b) and E.1:

UN-Tests 1(b) and 2(b): "-“

UN-Test E.1:"no“

Time-Pressure-Test:

Table 4.14/2 shows the used amounts of sample and the results from the Time-Pressure-Test. Figure 2, in the experimental report shows the time/pressure profiles of the Time-Pressure-Test. In order to protect the ignition source from the liquid sample it was put into a thin foil of polyethylene.

Table 4.14/2.-Amount for and times of the Time-Pressure-Tests

 

Test 1

Test 2

Test 3

Amount in g

5.0

5.0

5.0

Time to 690 kPagin s

1.0

2.2

1.7

Time to 2070 kPagin s

---

---

---

Pressure rise time in s

---

---

---

 

None of the three tests reached a pressure of 2070 kPa. Therefore the result had to be evaluated as negative according to UN-tests 1(c), 2(c) and C.1:

UN-Tests 1(c) and 2(c): “-“

UN-Test C.1: “no“

Final results

Due to the results presented in this report from the UN-tests 1(b) (effect of heating under confinement) and 1(c) (effect of ignition under confinement) the question “Is it an explosive substance?” can be answered in the negative. Therefore the test item can be excluded from classification in class 1 (explosives) according to series 1 of the ”UN Recommendations on Transport of Dangerous Goods - Manual of Test and Criteria“.

 

Interpretation of results:
GHS criteria not met
Conclusions:
Therefore the test item can be excluded from classification in class 1 (explosives) according to series 1 of the ”UN Recommendations on Transport of Dangerous Goods - Manual of Test and Criteria“.
Executive summary:

The thermal stability of the test substance is tested with Differential Scanning Calorimetry, in accordance with conditions recommended in UN MTC screening procedure/OECD guideline. Two DSC-measurements in closed glass crucibles with the test item showed an exothermal effect in the temperature range of 140 – 470 °C with a maximum energy release of 658 J/g. The heat of decomposition was above 500 J/g. Therefore further tests had to be performed. Due to a heat of decomposition below 800 J/g the appropriate tests were Koenen-Test and Time-Pressure-Test.

Due to the results presented from the UN-tests 1(b) (effect of heating under confinement) and 1(c) (effect of ignition under confinement) the question “Is it an explosive substance?” can be answered in the negative. Therefore the test item can be excluded from classification in class 1 (explosives) according to series 1 of the ”UN Recommendations on Transport of Dangerous Goods - Manual of Test and Criteria“.

Description of key information

Therman stability-> energy released in DSC screening 658 J/g (>500J/g and < 800J/g)

Koenen-Test and Time-Pressure-Test were performed -> the results from the UN-tests 1(b) (effect of heating under confinement) and 1(c) (effect of ignition under confinement) were negatives and excluded from classification in class 1 (explosives) according to series 1 of the ”UN Recommendations on Transport of Dangerous Goods - Manual of Test and Criteria“.

Key value for chemical safety assessment

Explosiveness:
non explosive

Additional information

A GLP fully reliable experimental study was conducted according to United Nations, Recommendations on the transport of dangerous goods, Manual of tests and criteria, Sixth revised edition, 2015: Appendix 6 as well as Guideline OECD 113 (1981). Therefore, it is considered as a key study. The result is retained as key data.

Justification for classification or non-classification

The thermal stability of the test substance is tested with Differential Scanning Calorimetry, in accordance with conditions recommended in UN MTC screening procedure/OECD guideline.Two DSC-measurements in closed glass crucibles with the test item showed an exothermal effect in the temperature range of 140 – 470 °C with a maximum energy release of 658 J/g.The heat of decomposition was above 500 J/g. Therefore further tests had to be performed. Due to a heat of decomposition below 800 J/g the appropriate tests were Koenen-Test and Time-Pressure-Test.

Due to the results presented from the UN-tests 1(b) (effect of heating under confinement) and 1(c) (effect of ignition under confinement) the question “Is it an explosive substance?” can be answered in the negative. Therefore the test item can be excluded from classification in class 1 (explosives) according to series 1 of the ”UN Recommendations on Transport of Dangerous Goods - Manual of Test and Criteria“.