Registration Dossier

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:
08 January 2009 to 07 February 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 relevant results.

Data source

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

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
GLP compliance:
yes (incl. certificate)
Remarks:
Date of inspection: 19 August 2008; Date of signature: 04 March 2009
Type of distribution:
volumetric distribution

Test material

Reference
Name:
Unnamed
Type:
Constituent
Details on test material:
Sponsor's identification : H-CB sodium salt
Description : blue solid
Purity : 94.8%
Lot number : MB-2
Date received : 04 December 2008
Storage conditions : room temperature in the dark


Results and discussion

Particle size
Percentile:
D50
Remarks on result:
other: Too few particles were of a size less than 10.0 µm to allow accurate assessment of mass median aerodynamic diameter.(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:
41.6 %
Remarks on result:
other: Proportion of test material having an inhalable particle size less than 100 µm using the sieve method.
No.:
#2
Size:
> 10 µm
Distribution:
0.417 %
Remarks on result:
other: Proportion of test material having a thoracic particle size less than 10.0 µm using the Cascade Impactor method.
No.:
#3
Size:
> 5.5 µm
Distribution:
0.365 %
Remarks on result:
other: Proportion of test material having a respirable particle size less than 5.5 µm using the Cascade Impactor method.

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)

10.05

Mass of test material passed through sieve (g)

4.18

Test material less than sieve aperture size (%)

41.6

 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

Particle Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.1181

88.8044

2.6863

2

5.5 - 10.0

85.4806

85.4804

-0.0002*

3

2.4 - 5.5

85.8954

85.8961

0.0007

4

1.61 - 2.4

85.5740

85.5762

0.0022

5

0.307 - 1.61

85.7355

85.7351

-0.0004*

Filter

<0.307

0.1209

0.1210

0.0001

*value of 0.000 g used in further calculations. Negative value within uncertainty of the balance.

Amount of test material found in artificial throat: 0.3 g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 2.9893 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

0.0030

0.100

3

5.5

0.0030

0.100

4

2.4

0.0023

7.69 x 10-2

5

1.61

0.0001

3.35 x 10-3

Filter

0.307

0.0001

3.35 x 10-3

 


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

86.1046

89.1365

3.0319

2

5.5 - 10.0

85.4728

85.4747

0.0019

3

2.4 - 5.5

85.8832

85.8855

0.0023

4

1.61 - 2.4

85.5642

85.5691

0.0049

5

0.307 - 1.61

85.7241

85.7301

0.0060

Filter

<0.307

0.1164

0.1164

0.0000

Amount of test material found in artificial throat: 0.0 g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 3.0470 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

0.0151

0.496

3

5.5

0.0132

0.433

4

2.4

0.0109

0.358

5

1.61

0.0060

0.197

Filter

0.307

0.0000

0.000

 


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

86.1020

89.1582

3.0562

2

5.5 - 10.0

85.4714

85.4743

0.0029

3

2.4 - 5.5

85.8775

85.8834

0.0059

4

1.61 - 2.4

85.5613

85.5685

0.0072

5

0.307 - 1.61

85.7230

85.7278

0.0048

Filter

<0.307

0.1164

0.1164

0.0000

Amount of test material found in artificial throat: 0.1 g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 3.1770 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

0.0208

0.655

3

5.5

0.0179

0.563

4

2.4

0.0120

0.378

5

1.61

0.0048

0.151

Filter

0.307

0.0000

0.000


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

0.100

0.417

2

0.496

3

0.655

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

0.100

0.365

2

0.433

3

0.563


Applicant's summary and conclusion

Conclusions:
Particle size data acquired for the test material are shown as follows:

Proportion of test material having an inhalable particle size less than 100 µm 41.6%
Proportion of test material having a thoracic particle size less than 10.0 µm 0.417%
Proportion of test material having a respirable particle size less than 5.5 µm 0.365%

Executive summary:

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 Diameter Distribution' (June 1996), which satisfies the requirents 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

41.6%

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

Cascade Impactor

0.417%

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

Cascade Impactor

0.365%