O-(ethoxycarbonyl)-N-(1-methyl-2-oxo-2-phenylethylidene)hydroxylamine

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

28 July 2017 to 05 October 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: European Commission Guidance Document EUR 20268 ‘Determination of Particle Size Distribution, Fibre Length and Diameter Distribution of Chemical Substances’

Version / remarks:

2002

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

cascade impaction

Remarks on result:

other: Too few particles were of a size less than 10.0 µm to allow accurate assessment of the mass median aerodynamic diameter.

No.:

#1

Size:

< 100 µm

Distribution:

58.4 %

No.:

#2

Size:

< 10 µm

Distribution:

1.28 %

No.:

#3

Size:

< 5.5 µm

Distribution:

0.443 %

Sieving Screening Test

Table 2: Results of the Sieving Screening Test

Measurement	Result
Mass of test material transferred to sieve	15.01 g
Mass of test material passed through sieve	8.77 g
Proportion of test material <100 µm	58.4 %

 

Cascade Impactor Method

Table 3: Cascade Impactor Method Determination 1

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	≥10.0	86.0025	88.8318	2.8293
Cup 2	≥5.5 to <10.0	85.4564	85.4867	0.0303
Cup 3	≥2.4 to <5.5	85.8388	85.8461	0.0073
Cup 4	≥1.61 to <2.4	85.6099	85.6130	0.0031
Cup 5	≥0.307 to <1.61	85.7117	85.7128	0.0011
Filter	<0.307	75.6023	75.6108	0.0085

- Mass of test material found in artificial throat: 0.0600 g.

- Total mass of test material recovered from artificial throat, sample cups and filter: 2.9396 g.

 

Table 4: Cascade Impactor Method Determination 2

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	≥10.0	86.0033	88.8698	2.8665
Cup 2	≥5.5 to <10.0	85.4571	85.4809	0.0238
Cup 3	≥2.4 to <5.5	85.8395	85.8451	0.0056
Cup 4	≥1.61 to <2.4	85.6113	85.6128	0.0015
Cup 5	≥0.307 to <1.61	85.7139	85.7166	0.0027
Filter	<0.307	75.6020	75.6023	0.0003

- Mass of test material found in artificial throat: 0.0500 g.

- Total mass of test material recovered from artificial throat, sample cups and filter: 2.9504 g.

 

Table 5: Cascade Impactor Method Determination 3

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	≥10.0	86.0036	88.8501	2.8465
Cup 2	≥5.5 to <10.0	85.4573	85.4770	0.0197
Cup 3	≥2.4 to <5.5	85.8397	85.8447	0.0050
Cup 4	≥1.61 to <2.4	85.6105	85.6121	0.0016
Cup 5	≥0.307 to <1.61	85.7151	85.7163	0.0012
Filter	<0.307	75.6041	75.6054	0.0013

- Mass of test material found in artificial throat: 0.1000 g.

- Total mass of test material recovered from artificial throat, sample cups and filter: 2.9753 g.

 

Table 6: The cumulative amounts of test material found in the three determinations for the individual particle size cut-points

Particle Size Cut-point (µm)	Cumulative Mass (g)			Cumulative Percentage (%)
	Det. 1	Det. 2	Det. 3	Det. 1	Det. 2	Det. 3
10.0	0.0503	0.0339	0.0288	1.71	1.15	0.968
5.5	0.0200	0.0101	0.0091	0.680	0.342	0.306
2.4	0.0127	0.0045	0.0041	0.432	0.153	0.138
1.61	0.0096	0.0030	0.0025	0.327	0.102	8.4 x 10^-2
0.307	0.0085	0.0003	0.0013	0.289	1.0 x 10^-2	4.4 x 10^-2

 

Table 7: The overall cumulative percentage (%) of test material with a particle size less than 10.0 µm and 5.5 µm

Particle Size	Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Mean
<10.0 µm	1.71	1.15	0.968	1.28
<5.5 µm	0.680	0.342	0.306	0.443

 

Discussion

- Too few particles were of a size less than 10.0 µm to allow accurate assessment of the mass median aerodynamic diameter.

- Sampling for the cascade impactor determinations was performed by rolling the test material container for approximately 10 minutes and then sampling from the top (determination 1), middle (determination 2) and bottom (determination 3).

Conclusions:

Under the conditions of this study the proportion of test item having an inhalable particle size <100 µm determined by sieving was 58.4 %. The proportion of test item having a thoracic particle size <10.0 µm, determined by the cascade impactor was 1.28. % and the proportion of test item having a respirable particle size <5.5 µm, also determined by the cascade impactor was 0.443 %.

Executive summary:

The particle size distribution of the test material was investigated in accordance with the European Commission Guidance Document EUR 20268 ‘Determination of Particle Size Distribution, Fibre Length and Diameter Distribution of Chemical Substances. The test was performed under GLP conditions.

The test material was first evaluated using a sieving screening test and then using the cascade impactor method.

Too few particles were of a size less than 10.0 µm to allow accurate assessment of the mass median aerodynamic diameter.

Sampling for the cascade impactor determinations was performed by rolling the test material container for approximately 10 minutes and then sampling from the top (determination 1), middle (determination 2) and bottom (determination 3).

Under the conditions of this study the proportion of test material having an inhalable particle size <100 µm determined by sieving was 58.4 %. The proportion of test material having a thoracic particle size <10.0 µm, determined by the cascade impactor was 1.28. % and the proportion of test material having a respirable particle size <5.5 µm, also determined by the cascade impactor was 0.443 %.

Description of key information

Under the conditions of this study the proportion of test material having an inhalable particle size <100 µm determined by sieving was 58.4 %. The proportion of test material having a thoracic particle size <10.0 µm, determined by the cascade impactor was 1.28. % and the proportion of test material having a respirable particle size <5.5 µm, also determined by the cascade impactor was 0.443 %.

Additional information

The particle size distribution of the test material was investigated in accordance with the European Commission Guidance Document EUR 20268 ‘Determination of Particle Size Distribution, Fibre Length and Diameter Distribution of Chemical Substances. The test was performed under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The test material was first evaluated using a sieving screening test and then using the cascade impactor method.

Too few particles were of a size less than 10.0 µm to allow accurate assessment of the mass median aerodynamic diameter.

Sampling for the cascade impactor determinations was performed by rolling the test material container for approximately 10 minutes and then sampling from the top (determination 1), middle (determination 2) and bottom (determination 3).

Under the conditions of this study the proportion of test material having an inhalable particle size <100 µm determined by sieving was 58.4 %. The proportion of test material having a thoracic particle size <10.0 µm, determined by the cascade impactor was 1.28. % and the proportion of test material having a respirable particle size <5.5 µm, also determined by the cascade impactor was 0.443 %.