p-nitrophenyl dihydrogen phosphate, compound with 2-amino-2-(hydroxymethyl)propane-1,3-diol (1:2)

Explosiveness

Administrative data

Endpoint:

explosive properties of explosives

Type of information:

experimental study

Adequacy of study:

key study

Study period:

13 August - 23 October 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Cross-reference

Reason / purpose for cross-reference:

reference to other study

Reference

Endpoint:

melting point/freezing point

Type of information:

experimental study

Adequacy of study:

key study

Study period:

13-26 August 2020

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EPA OPPTS 830.7200 (Melting Point / Melting Range)

Version / remarks:

1998

Deviations:

no

Qualifier:

according to guideline

Guideline:

EU Method A.1 (Melting / Freezing Temperature)

Version / remarks:

EC No. 440/2008

Deviations:

no

Qualifier:

according to guideline

Guideline:

OECD Guideline 102 (Melting point / Melting Range)

Version / remarks:

1995

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

differential scanning calorimetry

Specific details on test material used for the study:

Batch No.: 46587100
Storage: Refrigerator (approx. 2-8°C)

Key result

Melting / freezing pt.:

>= 162 - <= 163 °C

Atm. press.:

>= 1 002 - <= 1 004 hPa

Decomposition:

yes

Decomp. temp.:

ca. 210 °C

During the heating phase a distinct endothermic effect was observed in the temperature range of 150-180°C, which can be assigned to the melting of the test item. The endothermic effect was directly followed by a small exothermic effect starting at a temperature of approx. 180°C with an average energy release of -20 J/g.

As the onset temperatures in both tests deviate by more than 0.5 K from their mean value of 162.51 °C, the test item has a melting range of 162-163°C.

A second exothermic effect was observed starting at a temperature of approx. 220°C with an average energy release of -290 J/g.

Measurement No.	Sample weight / mg	Onset of Effect / °C	Range of effect / °C	Weight loss / mg	Atmospheric pressure / hPa
PN20063	7.72	163.23 --- ---	150 – 180 (endo) 180 – 190 (exo) 220 – 340 (exo)	3.86	1001.8
PN20065	9.53	161.78 --- ---	150 – 180 (endo) 180 – 190 (exo) 220 – 330 (exo)	4.57	1003.6

Optical verification using the capillary method

To verify the results of the DSC measurement, an additional measurement in a melting capillary was performed in the temperature range of 27°C to 225°C with a heating rate of 10 K/min. The test item started to melt at a temperature of approx. 140°C. At a temperature of 165°C the test item was completely molten (dark yellow liquid). At a temperature of 210°C the colour of the test item changed to orange. At a temperature of 225 °C the test item turned brown and rose inside the capillary. The test was terminated at a maximum temperature of 225 °C.

According to the observations during the test in the capillary method, the endothermic effect in the DSC measurements with open crucibles can be assigned to the melting of the test item.

Conclusions:

The test item 4-NPP, di-TRIS (CAS no. 68189-42-4) has a melting range of 162-163°C at atmospheric pressure (1002-1004 hPa) as determined by Differential Scanning Calorimetry and capillary method according to Regulation (EC) No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Executive summary:

The test item 4-NPP, di-TRIS (CAS no. 68189-42-4) has a melting range of 162-163°C at atmospheric pressure (1002-1004 hPa) as determined by Differential Scanning Calorimetry and capillary method according to Regulation (EC) No. 440/2008 Method A.1. and OECD Test Guideline 102 (1995).

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2020

Report date:

2020

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

other: OECD 113 (1981) Screening Test for Thermal Stability and Stability in Air

Deviations:

no

Test guideline 2

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:

Class 1 Test series 1 / 2, Test 1(b) / 2(b): Koenen Test
Class 1 Test series 1 / 2, Test 1(c) (i) / 2(c) (i): Time Pressure Test

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Test material

Test material information

impurity 1

Reference substance name:

Methanol

EC Number:

200-659-6

EC Name:

Methanol

Cas Number:

67-56-1

Molecular formula:

CH4O

IUPAC Name:

methanol

impurity 2

Reference substance name:

Acetone

EC Number:

200-662-2

EC Name:

Acetone

Cas Number:

67-64-1

Molecular formula:

C3H6O

IUPAC Name:

acetone

impurity 3

Reference substance name:

Water

EC Number:

231-791-2

EC Name:

Water

Cas Number:

7732-18-5

Molecular formula:

H2O

IUPAC Name:

Oxidane

Constituent 1

Reference substance name:

p-nitrophenyl dihydrogen phosphate, compound with 2-amino-2-(hydroxymethyl)propane-1,3-diol (1:2)

EC Number:

269-198-6

EC Name:

p-nitrophenyl dihydrogen phosphate, compound with 2-amino-2-(hydroxymethyl)propane-1,3-diol (1:2)

Cas Number:

68189-42-4

Molecular formula:

C6H6NO6P.2C4H11NO3

IUPAC Name:

4-nitrophenyl dihydrogen phosphate - 2-amino-2-(hydroxymethyl)propane-1,3-diol (1:2)

Test material form:

solid

Details on test material:

Batch / Lot No. 46587100

Specific details on test material used for the study:

Batch No.: 46587100
Storage: Refrigerator (approx. 2-8°C)

Results and discussion

Small-scale preliminary tests

Parameter:

other: Exothermic decomposition energy (J/g)

Value:

-750

Remarks on result:

other: Explosivity could not be excluded as the DSC measurement was above the threshold of -500 J/g.

Results of test series for explosives

Results of test series for explosives 1

Key result

Test series:

other: UN Test series 1 and 2

Method:

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

Parameter:

other: time (s) for pressure rise from 690 kPa to 2,070 kPa

Result:

result is considered "-" (negative)

Remarks on result:

p < 2070 kPa

Results of test series for explosives 2

Key result

Test series:

other: UN Test series 1 and 2

Method:

UN Test 1 (b): Koenen test

Parameter:

limiting diameter (mm)

Result:

negative, no explosion

Remarks on result:

other: Appearance of the tube: unchanged

Any other information on results incl. tables

Thermal Stability OECD 113

The test item showed an endothermic effect starting at a temperature of approx. 140 °C, which can be assigned to the melting of the test item (see cross-reference). The endothermic effect was directly followed by a small exothermic effect starting at a temperature of 160 °C, with an average energy release of -10 J/g. A second exothermic effect was observed starting at a temperature of approx. 210 °C with an average energy release of -750 J/g. No further thermal effects could be observed up to the maximum test temperature of 500 °C. The results of the DSC measurements are summarized in the table below.

Measurement No.	Crucible material / Atmosphere	Sample weight / mg	Start of effect / °C	Energy / J/g
PN20064	Glass / Air	5.03	140 160 210	+100 (endothermic) -10 (exothermic) -750 (exothermic)
PN20066	Glass / Air	5.56	140 160 210	+80 (endothermic) -10 (exothermic) -740 (exothermic)

Energies of exothermic effects are presented in the table as negative values and energies of endothermic effects as positive values.

Explosive Properties UN Class 1

The DSC measurements in closed crucibles showed a decomposition of the test item with an maximum overall decomposition energy of -760 J/g, meaning the decomposition energy goes beyond 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.

Explosive Properties; Thermal Sensitivity: Koenen Test

One series of three tests with a 1.0 mm diameter orifice plate were performed. Results of the Koenen Test are presented in the table below:

 

No.	Sample weight / g	Diameter orifice plate / mm	Reaction time t /s	Main Reaction	Appearance of tube
1	8.00	1	30 – 150	flame with emission of solid test item	“O”: unchanged
2	8.00	1	30 – 150	flame with emission of solid test item	“O”: unchanged
3	8.00	1	30 – 150	flame with emission of solid test item	“O”: unchanged

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

Explosive Properties; Time-Pressure Test

The results of the three tests conducted for the Time-Pressure test are summarised in the table below.

 

	Test 1	Test 2	Test 3
Time [s] at 690 kPa	Not reached	Not reached	Not reached
Time [s] at 2,070 kPa	Not reached	Not reached	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) (i) and 2 (c) (i) deemed to be “-”.

 

Applicant's summary and conclusion

Interpretation of results:

GHS criteria not met

Conclusions:

According to the results of the tests on explosive properties (UN Transport Regulation, Test series 1 and 2), the test item does not have to be classified as explosive substance in class 1 according to the UN Transport Regulation nor as explosive substance according to GHS or CLP Regulation EC 1272/2008 Annex I: 2.1.

Executive summary:

Thermal Stability (OECD 113)

The test item 4-NPP, di-TRIS (CAS no. 68189-42-4) showed an endothermic effect starting at a temperature of approx. 140 °C, which can be assigned to the melting of the test item (see cross-reference). The endothermic effect was directly followed by a small exothermic effect starting at a temperature of 160 °C, with an average energy release of -10 J/g. A second exothermic effect was observed starting at a temperature of approx. 210 °C with an average energy release of -750 J/g.

Explosive Properties UN Class 1

In the DSC measurements the energy of the exothermic decomposition of the test item 4-NPP, di-TRIS (CAS no. 68189-42-4) was > -500 J/g. Therefore, further tests on explosive properties had to be performed.

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

According to the results of the tests on explosive properties, the test item is classified as follows:

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) No. 1272/2008: Annex I: 2.1): The test item does not have to be classified as explosive substance according to GHS or CLP Regulation (EC) No. 1272/2008 Annex I: 2.1, respectively.