3-acetoxymethylen-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

Oxidising properties

Administrative data

Endpoint:

oxidising solids

Type of information:

experimental study

Adequacy of study:

key study

Study period:

September 25, 2012 to November 02, 2012

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Comparable to guideline study (Regulation EC No. 440/2008 Method A.17.) with acceptable restrictions

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Report date:

2012

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

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

Deviations:

no

GLP compliance:

no

Test material

Test material information

Constituent 1

Reference substance name:

3-acetoxymethylen-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

EC Number:

213-485-0

EC Name:

3-acetoxymethylen-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

Cas Number:

957-68-6

Molecular formula:

C10H12N2O5S

IUPAC Name:

(6R,7R)-3-[(acetyloxy)methyl]-7-amino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid

Test material form:

solid: particulate/powder

Remarks:

migrated information: powder

Details on test material:

Name: 7-Aminocefalosporansäure (7-ACA)
Lot no.: B146988

Results and discussion

Test results (Oxidising solids)

Test results (Oxidising solids) 1

Sample tested:

reference mixture (not specified)

Remarks:

migrated information

Parameter:

maximum burning rate

Result:

1.18 other: mm/s (migrated information)

Test results (Oxidising solids) 2

Sample tested:

test mixture (not specified)

Remarks:

migrated information

Parameter:

maximum burning rate

Result:

0.96 other: mm/s (migrated information)

Any other information on results incl. tables

The burning rates for the mixtures of barium nitrate with cellulose are shown inTable1.

Table1: Burning rates for the mixtures of barium nitrate with cellulose

Mixtures of barium nitrate : cellulose	Burning time	Burning rate
50 : 50 % (w/w)	207 s	0.97 mm/s
55 : 45 % (w/w)	172 s	1.16 mm/s
60 : 40 % (w/w)	169 s	1.18 mm/s
65 : 35 % (w/w)	190 s	1.05 mm/s
70 : 30 % (w/w)	273 s	0.73 mm/s

The reference mixture (60 : 40 % (w/w); mixture of the reference item barium nitrate with cellulose having the maximum burning rate) had a burning rate of 1.18 mm/s.

The burning rates for the mixtures of the test item with cellulose are shown inTable2.

Table2: Burning rates for the mixtures of test item with cellulose

Mixture of test item : cellulose	Burning time	Burning rate
0 : 100 % (w/w)	276 s	0.72 mm/s
5 : 95 % (w/w)	208 s	0.96 mm/s
10 : 90 % (w/w)	268 s	0.75 mm/s
15 : 85 % (w/w)	284 s	0.70 mm/s
20 : 80 % (w/w)	326 s	0.61 mm/s
30 : 70 % (w/w)	158 s for 25 mm (Flame extinguished after a few cm)	0.16 mm/s
40 : 60 % (w/w)	193 s for 40 mm (Flame extinguished after a few cm)	0.21 mm/s
50 : 50 % (w/w)	Flame extinguished after a few sec, no propagation of combustion)	--

The three highest burning rates for mixtures of test item and cellulose were observed for the ratios 5 : 95 % (w/w), 10 : 90 % (w/w) and 15 : 85 % (w/w). The main tests for these ratios were repeated five times.

The burning rates for the mixtures of the test item with cellulose with the three highest burning rates are shown inTable3.

Table3: Burning rates for the mixtures of test item with cellulose

Mixture test item : cellulose	Test 1	Test 2	Test 3	Test 4	Test 5	Test 6	Min. time	Maximum rate
5 : 95 % (w/w)	208 s	232 s	225 s	211 s	231 s	224 s	208 s	0.96 mm/s
10 : 90 % (w/w)	268 s	255 s	266 s	253 s	257 s	266 s	253 s	0.79 mm/s
15 : 85 % (w/w)	284 s	312 s	282 s	291 s	294 s	289 s	282 s	0.71 mm/s

The highest burning rate of a mixture of test item with cellulose was 0.96 mm/s.

The highest burning rate of a mixture of test item with cellulose (0.96 mm/s) is lower compared to the highest burning rate of a mixture of barium nitrate with cellulose (1.18 mm/s). Due to this result, the test item7-Aminocephalosporanic acidhas no oxidizing properties according to Directive EC 440/2008 A.17..

Applicant's summary and conclusion

Interpretation of results:

other: no oxidising properties

Remarks:

Migrated information

Conclusions:

The test item 7-Aminocephalosporanic acid has no oxidizing properties according to Directive EC 440/2008 A.17..

Executive summary:

A preliminary test was carried out in the interests of safety. No further testing would have been required if the preliminary test clearly indicated that the test substance has oxidizing properties. In this case, the substance would be regarded as oxidizing according toDirective EC 440/2008 Method A.17. Oxidizing properties of solids.

If this would not be the case, the substance should then be subject to the full test.

In the full test, the test item (< 125 µm) and a defined combustible substance (here cellulose) were mixed in various ratios. Each mixture was then formed into a pile and the pile was ignited at one end. The maximum burning rate determined was compared with the maximum burning rate of the mixture between barium nitrate (the reference item) and cellulose.

Preliminary Test

The dried test item was thoroughly mixed with the dried cellulose in the proportions 2 of test item to 1 of cellulose by weight. The mixture was shaped into a small cone pile of 3.5 cm (diameter of base) × 2.5 cm (height) by filling, without tamping, a cone-shaped former (e.g. a laboratory glass funnel with the stem plugged).

The pile was placed on a cool, non-combustible, non-porous and low heat-conducting base plate. The test was carried out in a fume cupboard.

The ignition source (flame) was put in contact with the cone. The vigor and duration of the resultant reaction were observed and recorded.

The substance is to be considered as oxidizing if the reaction is vigorous.

In any case where the result is open to doubt, it is then necessary to complete the full main test described below.

Main Test

Oxidizer-cellulose mixtures containing 10 to 90 % weight of oxidizer in 10 % increments were prepared for both, the test item and reference material. In this case, also mixtures with intermediate oxidizer-cellulose ratios (e.g. in 5% increments) were used to obtain the maximum burning rate more precisely.

The pile was 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 the longitudinal direction, two metal plates were mounted as sidewalls which project 2 mm beyond the upper edge of the triangular cross-section. This arrangement was loosely filled with a slight excess of mixture. After dropping the mould once from a height of 2 cm onto a solid surface, the remaining excess substance was scraped off with an obliquely positioned sheet. The sidewalls were removed and the remaining powder was smoothed, using a roller. A non-combustible, non-porous and low heat-conducting base plate was then placed on the top of the mould, the apparatus inverted and the mould removed.

The pile was arranged across the draught in a fume cupboard. The air-speed should be sufficient to prevent fumes escaping into the laboratory and should not be varied during the test.

Due to hygroscopicity of cellulose, the test should be carried out as quickly as possible.

One end of the pile was ignited by touching with the flame. Then, the time of reaction over a distance of 200 mm after the reaction zone was propagated an initial distance of 30 mm was measured.

The test was performed with the reference (barium nitrate – cellulose) mixture and, at least once, with each one of the test item - cellulose mixtures (samples). If the maximum burning rate of the samples is found to be much greater than that of the reference mixtures, the test can be stopped and the test item shall be regarded as oxidizing. Otherwise the test should be repeated five times for each of the three mixtures of test item and cellulose giving the fastest burning rate.

If the result is suspected of being a false positive, then the test should be repeated using an inert substance with a similar particle size, such as Kieselguhr, in place of cellulose. Alternatively, the test substance cellulose mixture, having the fastest burning rate, should be retested in an inert atmosphere (< 2 % v/v oxygen content).

In conclusion, a test item is to be considered as an oxidizing substance when:

(a)      in the preliminary test, there is a vigorous reaction;

(b)      in the full test, the maximum burning rate of the mixtures tested is higher than or equal to the maximum burning rate of the reference mixture of cellulose and barium nitrate.