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Physical & Chemical properties

Particle size distribution (Granulometry)

Administrative data

Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Testing was conducted between 29 April 2009 and 17 June 2009.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affect the quality of the relevant results.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2009

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
Deviations:
no
GLP compliance:
yes (incl. certificate)
Remarks:
Date of Signature: 04/03/09 Date of Inspection: 19/08/08
Type of distribution:
other:

Test material

Reference
Name:
Unnamed
Type:
Constituent
Type:
Constituent
Details on test material:
Sponsor's identification : PDE-28
Description : red powder
Purity : 97%
Batch number : 1RF-8017
Date received : 23 March 2009
Storage conditions : room temperature, in the dark

Results and discussion

Particle size
Percentile:
D50
Mean:
other: Too few particles were of a size less than 10.0 µm to allow accurate assessment of mass median aerodynamic diameter. EXAMPLE
Remarks on result:
other: Migrated from fields under 'Mass median diameter' as D50 percentile. No source field for Standard deviation.
Particle size distribution at different passagesopen allclose all
No.:
#1
Size:
< 100 µm
Distribution:
93.7 %
No.:
#2
Size:
< 10 µm
Distribution:
<= 0.15 %
No.:
#3
Size:
< 5.5 µm
Distribution:
<= 0.07 %

Any other information on results incl. tables

 Screening test (sieve method)

The results of the sieving procedure are shown in the following table:

Table 2:

Sieve aperture size (µm)

100

Mass of test material transferred to sieve (g)

10.07

Mass of test material passed through sieve (g)

9.44

Test material less than sieve aperture size (%)

93.7

Definitive test (cascade impactor method):

Determination 1:

The results of the cascade impactor method are shown in the following table:

Table 3 - Determination 1:

Cup Number

ParticleCollected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.1216

88.7792

2.6576

2

5.5 - 10.0

85.4438

85.4475

0.0037

3

2.4 - 5.5

85.9145

85.9140

-0.0005[1]

4

1.61 - 2.4

85.6294

85.6292

-0.0002*

5

0.307 - 1.61

85.7944

85.7943

-0.0001*

Filter

<0.307

75.0847

75.0849

0.0002

Amount of test material found in artificial throat: 0.33 g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 2.9907 g.

The cumulative amounts found for the individual particle size cut-points (µm) are shown in the following table:

Table 4 - Determination 1

Cup Number

Particle Size Cut-points (µm)

Cumulative Mass of Test Material (g)

Cumulative Amount of Test Material (%)

2

10.0

0.0039

0.13

3

5.5

0.0002

<0.01

4

2.4

0.0002

<0.01

5

1.61

0.0002

<0.01

Filter

0.307

0.0002

<0.01

 

[1]Insignificant weight loss noted, within anticipated balance tolerance. Value of 0.0000 g used in further calculations.

Determination 2:

The results of the cascade impactor method are shown in the following table:

Table 5 - Determination 2

Cup Number

ParticleCollected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.1279

88.9110

2.7831

2

5.5 - 10.0

85.4436

85.4456

0.0020

3

2.4 - 5.5

85.9142

85.9146

0.0004

4

1.61 - 2.4

85.6286

85.6289

0.0003

5

0.307 - 1.61

85.7936

85.7941

0.0005

Filter

<0.307

75.0774

75.0776

0.0002

Amount of test material found in artificial throat: 0.17 g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 2.9565 g.

The cumulative amounts found for the individual particle size cut-points (µm) are shown in the following table:

Table 6  - Determination 2

Cup Number

Particle Size Cut-points (µm)

Cumulative Mass of Test Material (g)

Cumulative Amount of Test Material (%)

2

10.0

0.0034

0.12

3

5.5

0.0014

0.05

4

2.4

0.0010

0.03

5

1.61

0.0007

0.02

Filter

0.307

0.0002

<0.01

 

Determination 3:

The results of the cascade impactor method are shown in the following table:

Table 7 -  Determination 3:

Cup Number

ParticleCollected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.13

89.0296

2.8996

2

5.5 - 10.0

85.4441

85.4466

0.0025

3

2.4 - 5.5

85.9143

85.9151

0.0008

4

1.61 - 2.4

85.6293

85.6298

0.0005

5

0.307 - 1.61

85.7945

85.7952

0.0007

Filter

<0.307

75.0827

75.0827

0.0000

Amount of test material found in artificial throat: 0.11 g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 3.0141 g.

The cumulative amounts found for the individual particle size cut-points (µm) are shown in the following table:

Table 8 -  Determination 3

Cup Number

Particle Size Cut-points (µm)

Cumulative Mass of Test Material (g)

Cumulative Amount of Test Material (%)

2

10.0

0.0045

0.15

3

5.5

0.0020

0.07

4

2.4

0.0012

0.04

5

1.61

0.0007

0.02

Filter

0.307

0.0000

0.00

The overall cumulative amounts (%) of test material with a particle size less than 10.0 µm from Determinations 1 to 3 are shown in the following table:

Table 9:

Determination

Cumulative Amount of Test Material

Less Than 10.0 µm (%)

Mean Cumulative Amount of Test Material Less Than 10.0 µm (%)

1

0.13

≤0.15

2

0.12

3

0.15

The overall cumulative amounts (%) of test material with a particle size less than 5.5 µm from Determinations 1 to 3 are shown in the following table:

Table 10:

Determination

Cumulative Amount of Test Material

Less Than 5.5 µm (%)

Mean Cumulative Amount of Test Material Less Than 5.5 µm (%)

1

<0.01

≤0.07

2

0.05

3

0.07

Discussion:

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

Due to a high degree of variance for the less than 5.5 µm particle size data, an overall limit value has been reported. For consistency, a limit value has been reported for the less than 10.0 µm data also.

Representative sampling was ensured by rolling the sample container for approximately ten minutes and sampling from the top, middle and bottom prior to definitive testing.

The inhalable fraction is defined as the mass fraction of particles which can be inhaled by nose or mouth, the thoracic fraction is defined as the mass fraction of particles that passes the larynx and the respirable fraction is defined as the mass fraction of particles that reaches the alveoli.

Applicant's summary and conclusion

Conclusions:
Measurement Method Result
Proportion of test material having an inhalable particle size less than 100 µm Sieve 93.7%
Proportion of test material having a thoracic particle size less than 10.0 µm Cascade Impactor ≤0.15%
Proportion of test material having a respirable particle size less than 5.5 µm Cascade Impactor ≤0.07%
Executive summary:

Particle Size Distribution:

 Particle size data have been acquired using a procedure designed to comply with the European Commission technical guidance docunt 'Particle Size Distribution, Fibre Length and Diater Distribution' (June 1996), which satisfies the requirements of OECD Guideline 110. The results are as follows:

Measurent

Method

Result

Proportion of test material having an inhalable particle size less than 100 µm

Sieve

93.7%

Proportion of test material having a thoracic particle size less than 10.0  µm

Cascade Impactor

≤0.15%

Proportion of test material having a respirable particle size less than 5.5 µm

Cascade Impactor

≤0.07%