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:
Testing was conducted between 16 May 2008 and 13 June 2008.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Study conducted to GLP and in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not effect the quality of the relevant results.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2008
Report date:
2008

Materials and methods

Test guideline
Qualifier:
according to guideline
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Remarks:
The work described was performed in compliance with UK GLP standards (Schedule 1, Good Laboratory Practice Regulations 1999 (SI 1999/3106 as amended by SI 2004/0994)).

Test material

Reference
Name:
Unnamed
Type:
Constituent

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.
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:
33 %
No.:
#2
Size:
< 10 µm
Distribution:
1.76 %
No.:
#3
Size:
< 5.5 µm
Distribution:
0.372 %

Any other information on results incl. tables

Screening test (sieve method)

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

Sieve aperture size (µm)

100

Mass of test material transferred to sieve (g)

14.98

Mass of test material passed through sieve (g)

4.94

Test material less than sieve aperture size (%)

33.0


Definitive test (cascade impactor method)

Determination 1

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

    Determination 1

Cup Number

Particle Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.1066

88.9407

2.8341

2

5.5 - 10.0

85.4348

85.4790

0.0442

3

2.4 - 5.5

85.8883

85.8940

0.0057

4

1.61 - 2.4

85.5811

85.5835

0.0024

5

0.307 - 1.61

85.7488

85.7504

0.0016

Filter

0.307

75.0908

75.0923

0.0015

Amount of test material found in artificial throat: 0.09g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 2.98g.

The cumulative amounts found for the individual particle size cut-points (µm) are shown in the following table:       Determination 1

Cup Number

Particle Size Cut-points (µm)

Cumulative Mass of Test Material (g)

Cumulative Amount of Test Material (%)

2

10.0

0.0554

1.86

3

5.5

0.0112

0.376

4

2.4

0.0055

0.185

5

1.61

0.0031

0.104

Filter

0.307

0.0015

5.03 x 10-2


Determination 2

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

      Determination 2

Cup Number

Particle Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.1076

88.9085

2.8009

2

5.5 - 10.0

85.4354

85.4728

0.0374

3

2.4 - 5.5

85.8895

85.8955

0.0060

4

1.61 - 2.4

85.5817

85.5848

0.0031

5

0.307 - 1.61

85.7495

85.7517

0.0022

Filter

0.307

75.0936

75.0951

0.0015

Amount of test material found in artificial throat: 0.15g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 3.00g.

The cumulative amounts found for the individual particle size cut-points (µm) are shown in the following table:     Determination 2

Cup Number

Particle Size Cut-points (µm)

Cumulative Mass of Test Material (g)

Cumulative Amount of Test Material (%)

2

10.0

0.0502

1.67

3

5.5

0.0128

0.427

4

2.4

0.0068

0.227

5

1.61

0.0037

0.123

Filter

0.307

0.0015

5.00 x 10-2


Determination 3

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

      Determination 3

Cup Number

Particle Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.0

86.1083

88.9796

2.8713

2

5.5 - 10.0

85.4362

85.4793

0.0431

3

2.4 - 5.5

85.8900

85.8948

0.0048

4

1.61 - 2.4

85.5824

85.5843

0.0019

5

0.307 - 1.61

85.7501

85.7510

0.0009

Filter

<0.307

75.0916

75.0934

0.0018

Amount of test material found in artificial throat: 0.07g.
Total amount of test material recovered from impactor cups, filter and artificial throat: 2.99g.

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

     Determination 3

Cup Number

Particle Size Cut-points (µm)

Cumulative Mass of Test Material (g)

Cumulative Amount of Test Material (%)

2

10.0

0.0525

1.75

3

5.5

0.0094

0.314

4

2.4

0.0046

0.154

5

1.61

0.0027

9.02 x 10-2

Filter

0.307

0.0018

6.01 x 10-2


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:

Determination

Cumulative Amount of Test Material

Less Than 10.0 µm (%)

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

1

1.86

1.76

2

1.67

3

1.75

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:

Determination

Cumulative Amount of Test Material

Less Than 5.5 µm (%)

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

1

0.376

0.372

2

0.427

3

0.314

Discussion

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

Representative sampling was ensured by rolling the sample container for approximately 10 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.

Conclusion

Particle size data acquired for the test material are shown in the following table:

Measurement

Method

Result

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

Sieve

33.0%

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

Cascade Impactor

1.76%

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

Cascade Impactor

0.372%

Applicant's summary and conclusion

Conclusions:
Particle size data acquired for the test material are shown in the following table:

Measurement Method Result
Proportion of test material having an inhalable particle size less than 100 µm Sieve 33.0%
Proportion of test material having a thoracic particle size less than 10.0 µm Cascade Impactor 1.76%
Proportion of test material having a respirable particle size less than 5.5 µm Cascade Impactor 0.372%
Executive summary:

For substance Na-Na in project number 1307 -0436 the method used is designed to comply with that given in ‘Particle Size Distribution, Fibre Length and Diameter Distribution’, June 1996 European Commission technical guidance document, which satisfies the requirements of OECD Guideline 110.