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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:
Between 07 February and 15 March 2012.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: see 'Remark'
Remarks:
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. The study report was conclusive, done to a valid guideline and the study was conducted under GLP conditions.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2012

Materials and methods

Test guideline
Qualifier:
equivalent or similar to guideline
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
Version / remarks:
The method used is based on a procedure 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 Guideli
Deviations:
no
Principles of method if other than guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
GLP compliance:
yes
Type of distribution:
other:

Test material

Reference
Name:
Unnamed
Type:
Constituent
Details on test material:
Identification: BMS-528235-01
Description: Off white powder
Batch: 1L63487N
Purity: 98.6 %
Expiry Date: 27 November 2014
Storage Conditions: Room temperature in the dark

Results and discussion

Particle sizeopen allclose all
Percentile:
D50
Remarks on result:
other: Not applicable(migrated from fields under 'Mass median diameter' as D50 percentile. No source field for Standard deviation.)
Mean:
other: Not Applicable
Particle size distribution at different passagesopen allclose all
No.:
#1
Size:
< 100 µm
Distribution:
27.9 %
No.:
#2
Size:
< 10 µm
Distribution:
0.233 %
No.:
#3
Size:
< 5.5 µm
Distribution:
0.156 %

Any other information on results incl. tables

Results

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

 

Table 3.18

 

Measurement

Result

Mass of test item transferred to sieve

19.93 g

Mass of test item passed through sieve

5.56 g

Proportion of test item <100 µm

27.9 %

 

 

 

Definitive test (cascade impactor method)

The results of the cascade impactor method determinations are shown as follows:

 

Determination 1

 

Table 3.19

 

Collection Stage

Particle Size Range Collected (µm)

Mass (g)

Pre-sampling

Post-sampling

Difference

Cup 1

>10.0

86.1153

88.5606

2.4453

Cup 2

5.5 to 10.0

85.5530

85.5553

0.0023

Cup 3

2.4 to 5.5

85.9031

85.9065

0.0034

Cup 4

1.61 to 2.4

85.6836

85.6839

0.0003

Cup 5

0.307 to 1.61

85.8546

85.8561

0.0015

Filter

<0.307

75.5387

75.5402

0.0015

 

Mass of test item found in artificial throat: 0.69 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.14 g.


Determination 2

 

Table 3.20

 

Collection Stage

Particle Size Range Collected (µm)

Mass (g)

Pre-sampling

Post-sampling

Difference

Cup 1

>10.0

86.1145

88.5350

2.4205

Cup 2

5.5 to 10.0

85.5557

85.5582

0.0025

Cup 3

2.4 to 5.5

85.9035

85.9040

0.0005

Cup 4

1.61 to 2.4

85.6831

85.6841

0.0010

Cup 5

0.307 to 1.61

85.8552

85.8552

0

Filter

<0.307

75.5371

75.5393

0.0022

 

Mass of test item found in artificial throat: 0.62 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.05 g

 

Determination 3

 

Table 3.21

 

Collection Stage

Particle Size Range Collected (µm)

Mass (g)

Pre-sampling

Post-sampling

Difference

Cup 1

>10.0

86.1172

87.9666

1.8494

Cup 2

5.5 to 10.0

85.5543

85.5566

0.0023

Cup 3

2.4 to 5.5

85.9041

85.9048

0.0007

Cup 4

1.61 to 2.4

85.6829

85.6845

0.0016

Cup 5

0.307 to 1.61

85.8552

85.8561

0.0009

Filter

<0.307

75.5353

75.5361

0.0008

 

Mass of test item found in artificial throat: 1.15 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.01 g.

 


 

Cumulative amounts

The cumulative amounts of test item found in the three determinations for the individual particle size cut-points are shown in the following table:

 

Table 3.22

 

Particle Size Cut-point (µm)

Cumulative Mass (g)

Cumulative Percentage (%)

Determination 1

Determination 2

Determination 3

Determination 1

Determination 2

Determination 3

10.0

0.0090

0.0062

0.0063

0.286

0.203

0.210

5.5

0.0067

0.0037

0.0040

0.213

0.121

0.133

2.4

0.0033

0.0032

0.0033

0.105

0.105

0.110

1.61

0.0030

0.0022

0.0017

9.5 x 10-2

7.2 x 10-2

5.7 x 10-2

0.307

0.0015

0.0022

0.0008

4.8 x 10-2

7.2 x 10-2

2.7 x 10-2

 

The overall cumulative percentage (%) of test item with a particle size less than 10.0 µm and 5.5 µm are shown in the following table:

 

Table 3.23

 

Particle size

Cumulative Percentage (%)

Determination 1

Determination 2

Determination 3

Mean

<10.0 µm

0.286

0.203

0.210

0.233

<5.5 µm

0.213

0.121

0.133

0.156

 

Applicant's summary and conclusion

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

The method used is based on a procedure 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, 12 May 1981.

Conclusion

Table 3.24

 

Measurement

Method

Result

Proportion of test item having an inhalable particle size <100 µm

Sieve

27.9 %

Proportion of test item having a thoracic particle size <10.0 µm

Cascade Impactor

0.233 %

Proportion of test item having a respirable particle size <5.5 µm

Cascade Impactor

0.156 %

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