Reaction product of the mixture p-phenylenediamine and 4-(2-naphthalenylamino)phenol with sodium polysulfide

Explosiveness

Administrative data

Endpoint:

explosive properties of explosives

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-10-25 - 2018-05-07

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference 1

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Reference 2

Reference Type:

study report

Title:

Unnamed

Year:

2018

Report date:

2018

Materials and methods

Test guideline

Test guideline 1

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:

Rev. 6, 2015

Deviations:

no

Test guideline 2

Qualifier:

according to guideline

Guideline:

other: OECD Test Guideline 113: Thermal Stability

Version / remarks:

1981

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Test material

Test material information

Constituent 1

Reference substance name:

Reaction product of the mixture p-phenylenediamine and 4-​(2-​naphthalenylamino)​phenol with sodium polysulfide

EC Number:

947-876-9

Molecular formula:

not applicable

IUPAC Name:

Reaction product of the mixture p-phenylenediamine and 4-​(2-​naphthalenylamino)​phenol with sodium polysulfide

Test material form:

solid: particulate/powder

Details on test material:

Test item: Black DB
Appearance: black powder

Results and discussion

Small-scale preliminary tests

Key result

Parameter:

other: Thermal stability

Remarks on result:

other: Due to the decomposition energy being above the threshold of -500 J/g, explosive properties cannot be excluded and further tests on explosive properties were carried in study CSL-17-1663.05.

Results of test series for explosives

Results of test series for explosives 1

Key result

Test series:

UN Test series 1

Method:

UN Test 1 (b): Koenen test

Parameter:

limiting diameter (mm)

Value:

1

Result:

result is considered "-" (negative)

Remarks on result:

other: "D": Wall of tube split

Results of test series for explosives 2

Key result

Test series:

UN Test series 2

Method:

UN Test 2 (b): Koenen test

Parameter:

limiting diameter (mm)

Value:

1

Result:

result is considered "-" (negative)

Remarks on result:

other: "D": Wall of tube split

Results of test series for explosives 3

Key result

Test series:

UN Test series 1

Method:

UN Test 1 (c) (i): Time/pressure test

Parameter:

other: time for a pressure rise from 690 to 2070 kPa

Result:

result is considered "-" (negative)

Remarks on result:

p < 2070 kPa

Remarks:

Pressure of 690 kPa not reached

Results of test series for explosives 4

Key result

Test series:

UN Test series 2

Method:

UN Test 2 (c) (i): Time/pressure test

Parameter:

other: time for a pressure rise from 690 to 2070 kPa

Result:

result is considered "-" (negative)

Remarks on result:

p < 2070 kPa

Remarks:

Pressure of 690 kPa not reached

Results of test series for explosives 5

Key result

Test series:

other: UN Test F.3: Trauzl test

Remarks:

The UN Test Series F.3 can be used as screening tests for assessing the ability to propagate a detonation.

Method:

UN Test 1 (a): UN gap test

Parameter:

other: Volume of the enlarged cavity per 10 g (mL)

Value:

8.7

Result:

result is considered "-" (negative)

Remarks on result:

other:

Remarks:

Based on this result also the UN-Transport Regulation Test 1(a) (UN gap test) deemed to be “-“.

Results of test series for explosives 6

Key result

Test series:

other: UN test F.3

Remarks:

The UN Test Series F.3 can be used as screening tests for assessing the ability to propagate a detonation.

Method:

UN Test 2 (a): UN gap test

Parameter:

other: Volume of the enlarged cavity per 10 g (mL)

Value:

8.7

Result:

result is considered "-" (negative)

Remarks on result:

other:

Remarks:

Based on this result also the UN-Transport Regulation Test 2(a) (UN gap test) deemed to be “-“.

Any other information on results incl. tables

Thermal stability (DSC)

In DSC run PN14838 the test item showed an exothermic effect in the temperature range of 110 – 330 °C with a decomposition energy of approx. -140 J/g. In DSC run PN14846 two exothermic effects can be observed in the temperature ranges of 100 – 290 °C and 290 – 370 °C with an overall decomposition energy of approx. -280 J/g.

Due to the fact that the DSC signal got noisy starting at a temperature of approx. 380 °C, which may be caused by a pressure rise inside the crucible, two further measurements in closed gold plated stainless steel crucibles were carried out.

In DSC run PN14615 the test item showed two exothermic effects in the temperature ranges of 100 – 350 °C and 360 – 500 °C. Due to the fact that the second exothermic effect was not finished at the maximum test temperature of 500 °C and could not be recorded completely, the overall decomposition energy is greater than -1160 J/g. In DSC run PN14950 three exothermic effects could be observed in the temperature ranges of 100 – 350 °C, 260 – 310 °C and 370 – 500 °C. Due to the fact that the third exothermic effect was not finished at the maximum test temperature of 500 °C and could not be recorded completely, the overall decomposition energy is greater than -430 J/g.

Table 1:    Results of the DSC-measurements

No.	Crucible material	Sample weight / mg	Start of effect / °C	Energy / J/g	Remark
PN14838	Glass	9.03	110	-140 (exothermic)
PN14846	Glass	5.36	100 290	-260 (exothermic) -30 (exothermic)
PN14615	Gold plated stainless steel	6.54	100 360	-410 (exothermic) >-750 (exothermic)
PN14950	Gold plated stainless steel	7.27	100 260 370	-120 (exothermic) -20 (exothermic) >-290 (exothermic)

Due to the decomposition energy being above the threshold of -500 J/g, explosive properties cannot be excluded and further tests on explosive properties were carried in study
CSL-17-1663.05.

Explosive Properties UN Class 1

In the DSC-measurements in closed crucibles of study CSL-17-1663.01 the test item showed a decomposition with an overall decomposition energy of greater than -1160 J/g, meaning the decomposition energy is above the threshold of -500 J/g to exclude explosive properties.

Due to the fact that the decomposition energy is above the threshold of -500 J/g the Koenen- and the Time-Pressure-Test had to be performed.

Due to the fact that the decomposition energy is above the threshold of -800 J/g also the Trauzl test had to be performed.

Explosive Properties; Thermal Sensitivity: Koenen-Test

Three tests witha 1.0 mm diameter orifice plate were performed.

Table 2:    Results of the Koenen-Test

No.	Sample weight / g	Diameter orifice plate / mm	Reaction time t1 / s	Reaction time t2 / s	Reaction time t3 / s	Reaction	Appearance of tube
1	12.8	1	90	155	> 300	t1: ejection of test item t2: bang, wall of tube split	Wall of tube split
2	13.0	1	80	130	> 300	t1: ejection of test item t2: bang, wall of tube split	Wall of tube split
3	12.9	1	90	130	> 300	t1: ejection of test item t2: bang, wall of tube split	Wall of tube split

t1: time to first reaction: test item gets blown out of the orifice
t2: time to second reaction: bang and wall of tube split
t3: time to main reaction: no reaction

Due to the fact that the test series with a 1.0 mm diameter orifice plate showed no explosionthe UN-Transport Regulation Test 1(b) and Test 2(b) deemed to be “-“.

 

Explosive Properties; Time-Pressure Test

Table 3 summarizes the results of the three tests.

Table 3:    Results of the Time-Pressure-Test

	Test 1	Test 2	Test 3
Time [s] at 690 kPa	Pressure not reached	Pressure not reached	Pressure not reached
Time [s] at 2,070 kPa	Pressure not reached	Pressure not reached	Pressure not reached
Time for pressure rise [s]	---	---	---

 

Due to the fact that the test item did not reach a pressure of 2070 kPa,the UN-Transport Regulation Test 1(c) and 2(c) deemed to be “-“.

Explosive Properties; Trauzl Test

Two tests with a test item mass of approx. 3.45 g were carried out. Thevolume of the enlarged cavity is 3.0 mL. Normalization to 10 g of the test item results in an expansion of 8.7 mL per 10 g, therefore theUN-Transport Regulation Test F.3 results to be “No”.Based on the UN Recommendations on the TRANSPORT OF DANGEROUS GOODS: Manual of Tests and Criteria, the UN Test Series F.3 can be used as screening tests for assessing the ability to propagate a detonation.Based on this the UN-Transport Regulation Test 1(a) and 2(a) (UN gap test) deemed to be “-“.

Applicant's summary and conclusion

Interpretation of results:

GHS criteria not met

Conclusions:

In the test on explosive properties according to UN Transport Regulation, Test series 1 and 2, the test item Black DB showed no explosive properties.

According to the results of the test on thermal stability and explosive properties, the test item is classified as following:
UN Transport Regulation: The test item does not have to be classified as explosive substance in class 1 according to the UN Transport Regulation.
GHS (CLP Regulation EC 1272/2008: Annex 1: 2.1): The test item does not have to be classified as explosive substance according to GHS or CLP Regulation EC 1272/2008 Annex 1: 2.1, respectively.

Executive summary:

Summary

In the test on explosive properties accordingto UN Transport Regulation, Test series 1 and 2,the test itemBlack DB showed no explosive properties.

According to the results of the test on thermal stability and explosive properties, the test item is classified as following:

UN Transport Regulation: The test item does not have to be classified as explosive substance in class 1 according to the UN Transport Regulation.

GHS (CLP Regulation EC 1272/2008: Annex 1: 2.1): The test item does not have to be classified as explosive substance according to GHS or CLP Regulation EC 1272/2008 Annex 1: 2.1, respectively.