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Diss Factsheets

Administrative data

Endpoint:
explosive properties of explosives
Type of information:
experimental study
Adequacy of study:
key study
Study period:
13 Jul - 13 Aug 2020
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2020
Report date:
2020

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to guideline
Guideline:
UN Manual of Tests and Criteria: Part I: Classification procedures, test methods and criteria relating to explosives of Class 1
Version / remarks:
UN Manual of Tests and Criteria, rev. 7 (2019), Appendix 6 - Koenen test: UN-tests 1(b), 2(b) - Time / pressure test 1(c), 2(c)
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: OECD 113 Screening test for thermal stability and stability in air
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
Hess. Ministerium für Umwelt, Klimaschutz, Landwirtschaft und Verbraucherschutz, Wiesbaden, Germany

Test material

Constituent 1
Chemical structure
Reference substance name:
1-(2,2,4-trimethyl-1,2-dihydroquinolin-1-yl)ethan-1-one
EC Number:
665-911-3
Cas Number:
5855-23-2
Molecular formula:
C14 H17 N O
IUPAC Name:
1-(2,2,4-trimethyl-1,2-dihydroquinolin-1-yl)ethan-1-one

Results and discussion

Small-scale preliminary tests
Parameter:
other: decomposition energy from DSC measurement
Value:
532
Remarks on result:
other: Two exothermal effects in the temperature range of 100 - 180 °C and 270 - 440 °C with a maximum energy release of 532 J/g.
Results of test series for explosivesopen allclose all
Test series:
UN Test series 1
Method:
UN Test 1 (b): Koenen test
Parameter:
limiting diameter (mm)
Result:
negative, no explosion
Remarks on result:
other: No explosion was observed, the limiting diameter was less than 1 mm.
Test series:
UN Test series 1
Method:
UN Test 1 (c) (i): Time/pressure test
Parameter:
other: Pressure rise time
Result:
negative, no or slow deflagration
Remarks on result:
p = 2070 kPa: no
Remarks:
None of the three tests reached a pressure of 2070 kPa.
Test series:
UN Test series 2
Method:
UN Test 2 (b): Koenen test
Parameter:
limiting diameter (mm)
Result:
negative, no explosion
Remarks on result:
other: No explosion was observed, the limiting diameter was less than 1 mm.
Test series:
UN Test series 2
Method:
UN Test 2 (c) (i): Time/pressure test
Parameter:
other: Pressure rise time
Result:
negative, no or slow deflagration
Remarks on result:
p = 2070 kPa: no
Remarks:
None of the three tests reached a pressure of 2070 kPa.
Test series:
UN Test series 2
Method:
UN Test 2 (a): UN gap test
Parameter:
other: fragmentation
Result:
other: see remarks
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

Any other information on results incl. tables

Thermal stability
Two DSC measurement in closed glass crucibles showed two exothermal effects in the temperature range of 100 - 180 °C and 270 - 440 °C with a maximum energy release of 532 J/g. The course of the baseline above the second exothermal effect was ambiguous, this could have been caused by a pressure rise. The results are summarized in the Table below:

Ident-No. Weight / mg Final temperature / °C Temperature range / °C Type of effect Energy / J/g
39139 10.28 500

120 - 180

270 - 435

Exothermal

Exothermal

23

509

39142 10.62 500

100 - 180

275 - 440

Exothermal

Exothermal

26

432

The heat of decomposition was above 500 J/g. Therefore, further tests on explosive properties had to be performed. As the heat of decomposition was below 800 J/g and the test item is an organic substance the appropriate tests were Koenen-test according to UN 1 (b)/2 (b) and Time-Pressure test according to UN 1 (c)/2 (c).

Koenen test
The Koenen test was started with a diameter of 20 mm and subsequently continued with 1 2 mm, 8 mm, 5 mm, 3 mm, 2.5 mm, 2 mm, 1.5 mm and 1 mm. 11 tests were performed. The results are shown in Table below.

Amount / g Diameter of orifice / mm t1 / s t2 / s Reaction Effect
28.1 20 52 > 300 Flame o
28.1 12 53 > 300 Flame o
28.1 8 53 > 300 Flame o
28.1 5 52 > 300 Flame o
28.1 3 50 > 300 Flame o
28.1 2.5 49 > 300 Flame o
28.1 2 49 > 300 Flame o
28.1 1.5 48 > 300 Flame o
28.1 1.0 46 > 300 Flame o
28.1 1.0 47 > 300 Flame o
28.1 1.0 47 > 300 Flame o

t1: time to any reaction, e.g. whistle or flame
t2: time to main reaction, e.g. rupture of tube or flashing
o: tube unchanged

No explosion was observed. The limiting diameter was less than 1 mm. Therefore, the results had to be evaluated as negative according to UN tests 1(b) and 2(b): negative "-". 

 

Time / pressure test
Table below shows the used amounts of sample and the results from the Time / pressure test. 

  Test 1 Test 2 Test 3
Amount in g 4.9 5.0 5.0
Time to 690 kPag in s 2.34 4.20 3.31
Time to 2070 kPag in 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) and 2(c): negative "-".  These evaluations indicate no (or slow) deflagration according to the UN tests 1(c) and 2(c).

 

Applicant's summary and conclusion

Interpretation of results:
GHS criteria not met
Remarks:
Due to a decomposition energy <800 J/g and due to the fact that the test item consisted mainly of organic components a serie 1 type (a) test (propagation of a detonation) was not necessary (see appendix 6 of UN Manual of Tests and Criteria, revision 7 (2019)). Also due to negative results presented above from the UN tests 1(b) (effect of heating under confinement) and 1 (c) (effect of ignition under confinement), the test item can be excluded from classification in class 1 (explosives) according to series 1 of the UN Manual of Tests and Criteria, revision 7 (2019).