Reaction product of 3,9-dibromobenzanthrone condensed with 2 equivalents of 1-aminoanthraquinone, subsequently further condensed under oxidative conditions

Oxidising properties

Link to relevant study record(s)

Reference

Endpoint:

oxidising solids

Type of information:

experimental study

Adequacy of study:

key study

Study period:

July 20, 2015 - August 05, 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

EU Method A.17 (Oxidising Properties (Solids))

Deviations:

not specified

GLP compliance:

no

Contact with:

powdered cellulose

Key result

Sample tested:

test mixture as specified

Parameter:

maximum burning rate

Result:

1.01 mm/s

Results

Grinding, sieving and drying of the test item, barium nitrate and cellulose.

The cellulose was dried by treating the sample at 105 °C ± 5 °C until the weight was constant. Due to the particle size of the cellulose grinding and sieving was not necessary. The barium nitrate was grounded with a mill, sieved< 0.12 mmand dried by treating the sample at 105 °C ± 5 °C until the weight was constant. The test item was grounded with a mortar, sieved <125 µm and dried by treating the sample at 50 °C ± 5 °C under vacuum until the weight was constant.

Preliminary test

Three test mixtures with the test item and cellulose 2:1 showed a short flame with discoloring of the surface of the mixture. The mixtures burned for 5 s, 7 s and 7 s, respectively. The flames extinguished before the pile was completely consumed. Three test mixtures with barium nitrate/cellulose 2:1 burned down completely in 57 s, 57 s and 58 s, respectively. Due to the results of the preliminary test the main test had to be performed.

 

 Main test

Four tests were performed for the reference mixture (barium nitrate and cellulose) with 50, 55, 60 and 70 wt. %oxidizer (barium nitrate). The results are shown in Table1.

Table1: Burning times and rates of reference mixtures

Barium nitrate [wt.%]	Burning time over 200 mm [s]	Burning rate [mm/s]
50	144	1.39
55	137	1.46
60	144	1.39
70	167	1.20

The highest burning rate of 1.46 mm/s was found for the mixture with 55 wt. % oxidizer.

Mixtures of the test item with cellulose were prepared in between 10 and 90 wt. % of the test item and tested. An additional test with 15 % was performed. Table2 shows the results.

Table2: Burning times and rates of test item mixtures

Test item[%]	Burning time over 200 mm [s]	Burning rate [mm/s]
10	213	0.94
15	238	0.84
20	260	0.77
30	336 (¼ of zone with burning, ¾ of zone with flame shortly before extinguishing)	-
40	Flame extinguished in starting zone	-
60	The test item could not be ignited	-
90	The test item could not be ignited	-

Due to the fact that the maximum burning rate of the mixtures of the test item with cellulose is lower than the maximum burning rate of the reference mixture, six tests were performed only with the three mixtures with the highest burning rates of 10, 15 and 20 wt.% of test item to verify these values (seeTable3) 

Table3: Burning times and rates of the fastest test item mixtures

Test:	t [s]	V[mm/s]	t [s]	V[mm/s]	t [s]	V[mm/s]	t [s]	V[mm/s]	t [s]	V[mm/s]	t [s]	V[mm/s]
10 %	231	0.94	206	0.97	208	0.96	199	1.01	203	0.99	199	1.01
15 %	238	0.84	228	0.88	226	0.89	230	0.87	223	0.90	232	0.86
20 %	260	0.77	250	0.80	255	0.78	245	0.82	258	0.78	250	0.80

The maximum burning rate of the mixtures of the test item and cellulose (1.01 mm/s) was less than the maximum burning rate of the reference mixture of cellulose and barium nitrate (1.20 mm/s). Due to the fact that the mixture of the test item with cellulose burned slower compared to the reference mixtureit was concluded that the test item has no oxidizing properties.

Interpretation of results:

GHS criteria not met

Conclusions:

The maximum burning rate of the mixtures of the test item and cellulose (1.01 mm/s) was less than the maximum burning rate of the reference mixture of cellulose and barium nitrate (1.20 mm/s). Due to the fact that the mixture of the test item with cellulose burned slower compared to the reference mixture it was concluded that the test item has no oxidizing properties.The test item had no oxidizing properties in the sense of the European Commission Regulation (EC) No. 440/2008, Method A.17.

Executive summary:

Study performed in accordance with EU Method A.17 (Oxidising Properties (Solids)).

 

A preliminary test is carried out in the interest of safety. The preliminary test will be sufficient when it clearly indicates that the test item or the preparation has oxidizing properties. If this is not the case, the substance or preparation is subject to the full main test.

In the main test, the test item and a defined combustible substance (both sieved to < 0.125 mm and dried) will be mixed in various ratios. Each mixture is then formed into a pile and the pile is ignited at one end. The maximum burning rate determined is compared with the maximum burning rate of the reference mixture.

Mixtures of oxidizers with cellulose must be treated as potentially explosive and handled with care.

 

Preliminary test

The dried test item is mixed with the dried cellulose in the proportions 2 of the test item to 1 of cellulose by weight and the mixture is formed into a small cone shaped pile of dimensions 3.5 cm (diameter of base) x 2.5 cm (height) by filling, without tamping, a cone-shaped glass. The pile is placed on a non-combustible and non-porous plate. As ignition source a flame is used to ignite the pile. The vigour and duration of the resultant reaction is observed and recorded.

The test result is compared with this of a mixture of barium nitrate/cellulose 2:1.

The test item is to be considered as oxidizing if the reaction is vigorous. In this case no further testing is required. When this is not the case, the substance should then be subject to the main test.

 

Main test

Mixtures of oxidizer/cellulose are prepared in 10 wt. % increments. For borderline cases, intermediate oxidizer/cellulose-mixtures are used to obtain the maximum burning rate more precisely. The pile is formed by means of a mould. The mould is made of metal, has a length of 250 mm and a triangular cross-section with an inner height of 10 mm and an inner width of 20 mm. On both sides of the mould, in longitudinal direction, two metal sheets are mounted as lateral limitations which overlook 2 mm the upper edge of the triangular cross-section. This arrangement is loosely filled with mixture in a slight excess. After dropping the mould from a height of 2 cm on to a solid surface, the remaining excess test item is scraped off with an oblique positioned sheet. Then the lateral limitations are removed and the remaining powder is smoothed. A non-combustible plate is then placed on the top of the mould, the apparatus is inverted and the mould removed. The flame of a gas burner is used as ignition source. The time of reaction over 200 mm after the reaction zone has propagated an initial distance of 30 mm is measured. First the test is performed with the reference substance. The test is then carried out at least once with each one of the range of mixtures of the test item with cellulose. If the burning rate of a given mixture is found significantly greater than that of the reference mixture, the test can be stopped. Otherwise, the test has to be repeated five times more with the three mixtures having shown the highest burning rate. In case of a positive result additional tests of the reference substance and of the test item in mixture with kieselguhr are performed as well as experiments under an inert atmosphere (Argon). For safety reasons the maximum burning rate - not the mean value - shall be considered to be the characteristic oxidizing property of the test item.

 

Results

Grinding, sieving and drying f the test item, barium nitrate and cellulose.

The cellulose was dried by treating the sample at 105 °C ± 5 °C until the weight was constant. Due to the particle size of the cellulose grinding and sieving was not necessary. The barium nitrate was grounded with a mill, sieved< 0.12 mm and dried by treating the sample at 105 °C ± 5 °C until the weight was constant. The test item was grounded with a mortar, sieved <125 µm and dried by treating the sample at 50 °C ± 5 °C under vacuum until the weight was constant.

 

Preliminary test

Three test mixtures with the test item and cellulose 2:1 showed a short flame with discolouring of the surface of the mixture. The mixtures burned for 5 s, 7 s and 7 s, respectively. The flames extinguished before the pile was completely consumed. Three test mixtures with barium nitrate/cellulose 2:1 burned down completely in 57 s, 57 s and 58 s, respectively. Due to the results of the preliminary test the main test had to be performed.

 

Main test

Four tests were performed for the reference mixture (barium nitrate and cellulose) with 50, 55, 60 and 70 wt. %oxidizer (barium nitrate).

The highest burning rate of 1.46 mm/s was found for the mixture with 55 wt. % oxidizer.

Mixtures of the test item with cellulose were prepared in between 10 and 90 wt. % of the test item and tested. An additional test with 15 % was performed.

Due to the fact that the maximum burning rate of the mixtures of the test item with cellulose is lower than the maximum burning rate of the reference mixture, six tests were performed only with the three mixtures with the highest burning rates of 10, 15 and 20 wt.% of test item to verify these values.

The maximum burning rate of the mixtures of the test item and cellulose (1.01 mm/s) was less than the maximum burning rate of the reference mixture of cellulose and barium nitrate (1.20 mm/s). Due to the fact that the mixture of the test item with cellulose burned slower compared to the reference mixture it was concluded that the test item has no oxidizing properties.

 

The test item had no oxidizing properties in the sense of the European Commission Regulation (EC) No. 440/2008, Method A.17.

Description of key information

Key value determined in a laboratory study performed in accordance with EU Method A.17 (Oxidising Properties (Solids)).

According to this study, the test item has no oxidising properties.

Key value for chemical safety assessment

Oxidising properties:

non oxidising

Additional information

Study performed in accordance with EU Method A.17 (Oxidising Properties (Solids)).

 

The maximum burning rate of the mixtures of the test item and cellulose (1.01 mm/s) was less than the maximum burning rate of the reference mixture of cellulose and barium nitrate (1.20 mm/s). Due to the fact that the mixture of the test item with cellulose burned slower compared to the reference mixture it was concluded that the test item has no oxidising properties.

Justification for classification or non-classification

The test substance is not classified as oxidising in accordance with the CLP regulation.