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:
2004-07-02 to 2004-11-25
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
comparable to guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2005
Report Date:
2005

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions) - Method B: Fibre Length and Diameter Distributions
Version / remarks:
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.
Deviations:
yes
Remarks:
a preliminary sieve test was followed by a determination with the cascade impactor method
GLP compliance:
yes (incl. certificate)
Type of method:
cascade impaction
Remarks:
Screening test: sieve method; Definitive test: cascade impactor method
Type of distribution:
mass based distribution

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder
Specific details on test material used for the study:
STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: approximately 4°C, in the dark

Results and discussion

Remarks on result:
other:
Remarks:
A significant proportion (21.1%) of particles were found to be in the thoracic range (< 10.2 µm). However, there were too few to allow accurate assessment of mass median aerodynamic diameter.
Particle size
Key result
Percentile:
other: Mean Proportion of particles in the thoracic range
Mean:
21.1 other: %
Remarks on result:
other: Stadard deviation is not applicable
Remarks:
A significant proportion (21.1%) of particles were found to be in the thoracic range (<10.2 µm). However, there were too few to allow accurate assessment of mass median aerodynamic diameter.
Particle size distribution at different passagesopen allclose all
No.:
#2
Size:
10.2 µm
Distribution:
15.2 %
Remarks on result:
other: Number given for No. specifies Cup Number
No.:
#3
Size:
5.4 µm
Distribution:
3.61 %
Remarks on result:
other: Number given for No. specifies Cup Number
No.:
#4
Size:
2.5 µm
Distribution:
1.51 %
Remarks on result:
other: Number given for No. specifies Cup Number
No.:
#5
Size:
1.67 µm
Distribution:
0.964 %
Remarks on result:
other: Number given for No. specifies Cup Number
No.:
#6
Size:
0.393 µm
Distribution:
0.62 %
Remarks on result:
other: results for Filter

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)

 12.0

 Mass of test material passed through sieve (g)

 1.9

 Test material less than sieve aperture size (%)

 15.8

Definitive test (cascade impactor method)

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

Determination 1

Cup Number

Particle Size Range
Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.2

86.8605

88.7111

1.8506

2

5.4 - 10.2

86.0529

86.5346

0.4817

3

2.5 - 5.4

86.3154

86.4053

0.0899

4

1.67 - 2.5

86.1372

86.1607

0.0235

5

0.393 - 1.67

86.1918

86.2025

0.0107

Filter

<0.393

75.5593

75.6026

0.0433

 

Amount of test material found in artificial throat: 0.0 g.

Total amount of test material recovered from impactor cups, filter and artificial throat: 2.50 g.

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

10.2

0.6491

26.0

3

5.4

0.1674

6.70

4

2.5

0.0775

3.10

5

1.67

0.0540

2.16

Filter

0.393

0.0433

1.73

Determination 2

Cup Number

Particle Size Range
Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.2

86.8614

88.1852

1.3238

2

5.4 - 10.2

86.0517

86.2963

0.2446

3

2.5 - 5.4

86.3153

86.3580

0.0427

4

1.67 - 2.5

86.1375

86.1472

0.0097

5

0.393 - 1.67

86.1915

86.1971

0.0056

Filter

<0.393

75.5648

75.5794

0.0146

 

Amount of test material found in artificial throat: 0.0 g.

Total amount of test material recovered from impactor cups, filter and artificial throat: 1.64 g.

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

10.2

0.3172

19.3

3

5.4

0.0726

4.42

4

2.5

0.0299

1.82

5

1.67

0.0202

1.23

Filter

0.393

0.0146

0.890

Determination 3

Cup Number

Particle Size Range
Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.2

86.8591

88.7070

1.8479

2

5.4 - 10.2

86.0509

86.3130

0.2621

3

2.5 - 5.4

86.3139

86.3929

0.0790

4

1.67 - 2.5

86.1361

86.1546

0.0185

5

0.393 - 1.67

86.1894

86.2023

0.0129

Filter

<0.393

75.5673

75.5962

0.0289

 

Amount of test material found in artificial throat = 0.0 g.

Total amount of test material recovered from impactor cups, filter and artificial throat = 2.25 g.

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

10.2

0.4014

17.8

3

5.4

0.1393

6.19

4

2.5

0.0603

2.68

5

1.67

0.0418

1.86

Filter

0.393

0.0289

1.29

Determination 4

Cup Number

Particle Size Range
Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.2

86.8557

88.5836

1.7279

2

5.4 - 10.2

86.0469

86.5248

0.4779

3

2.5 - 5.4

86.3116

86.3983

0.0867

4

1.67 - 2.5

86.1342

86.1542

0.0200

5

0.393 - 1.67

86.1889

86.1979

0.0090

Filter

<0.393

75.5533

75.5967

0.0434

 

Amount of test material found in artificial throat = 0.0 g.

Total amount of test material recovered from impactor cups, filter and artificial throat = 2.36 g.

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

Determination 4

Cup Number

Particle Size Cut-points
(µm)

Cumulative Mass of Test
Material (g)

Cumulative Amount of
Test Material (%)

2

10.2

0.6370

26.9

3

5.4

0.1591

6.73

4

2.5

0.0724

3.06

5

1.67

0.0524

2.22

Filter

0.393

0.0434

1.84

Determination 5

Cup Number

Particle Size Range
Collected (µm)

Cup Masses (g)

Pre-sampling

Post-sampling

Difference

1

>10.2

86.8521

89.0211

2.1690

2

5.4 - 10.2

86.0459

86.3566

0.3107

3

2.5 - 5.4

86.3101

86.3665

0.0564

4

1.67 - 2.5

86.1342

86.1487

0.0145

5

0.393 - 1.67

86.1856

86.1948

0.0092

Filter

<0.393

75.5610

75.5776

0.0166

 

Amount of test material found in artificial throat = 0.1 g.

Total amount of test material recovered from impactor cups, filter and artificial throat = 2.68 g.

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

Determination 5

Cup Number

Particle Size Cut-points
(µm)

Cumulative Mass of Test
Material (g)

Cumulative Amount of
Test Material (%)

2

10.2

0.4074

15.2

3

5.4

0.0967

3.61

4

2.5

0.0403

1.51

5

1.67

0.0258

0.964

Filter

0.393

0.0166

0.620

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

following table:

 Cup Number

 Particle Size Cut-points (µm)

 Cumulative Mass of Test Material (g)

 Cumulative Amount of

Test Material (%)

 2

10.2

 0.4074

15.2 

 3

5.4 

 0.0967

 3.61

 4

 2.5

 0.0403

 1.51

 5

 1.67

 0.0258

 0.964

 Filter

 0.393

 0.0166

 0.620

The overall cumulative amounts of test material with a particle size less than 10.2 µm (%) from Determinations 1 to 5 are shown in the following table:

 Determination

 Cumulative Amount of Test Material Less Than 10 µm (%)

 Mean Cumulative Amount of Test Material Less Than 10 µm (%)

 1

 26.0

 

 2

 19.3

 

 3

 17.8

 21.1

 4  26.9  
 5  15.2  

Discussion

Due to the slight variation between the results of the first three determinations, an extra two were performed.  As no definite trend was observed, all five were included in the mean result.

A significant proportion (21.1%) of particles were found to be in the thoracic range (<10.2 µm). However, there were too few 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 inhalation fraction is defined as the mass fraction of particles which can be inhaled by nose or mouth and the thoracic fraction is defined as the mass fraction of particles that passes the larynx.

It was noted that a greater proportion of test material was found to be <10.2 µm than went through the 100 µm sieve.  This probably due to partial blocking of the sieve with test material.

Applicant's summary and conclusion

Conclusions:
Particle size data acquired for the test material showed:
The proportion of test material having a particle size less than 100 µm , as determined by the sieve method, is 15.8%.
The proportion of test material having a particle size less than 10.2 µm, as determined by the Cascade Impactor method, is 21.1%.