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Particle size distribution (Granulometry)

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Reference
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
Between 15 February and 03 March 2012.
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
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 method:
sieving
Type of distribution:
other: Sieving Screening Test, Cascade Impactor
Remarks on result:
not determinable because of methodological limitations
Percentile:
D50
Remarks on result:
not determinable
No.:
#1
Size:
< 100 other: µm
Distribution:
13.8 %
No.:
#2
Size:
< 10 µm
Distribution:
<= 5.58 %
No.:
#3
Size:
< 5.5 µm
Distribution:
<= 0.83 %

Results

Screening test (sieve method)

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

 

Table 3.16

 

Measurement

Result

Mass of test item transferred to sieve

15.18 g

Mass of test item passed through sieve

2.10 g

Proportion of test item <100 µm

13.8 %

 

 

  

Definitive test

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

 

Determination 1

 

Table 3.17

 

Collection Stage

Particle Size Range Collected (µm)

Mass (g)

Pre-sampling

Post-sampling

Difference

Cup 1

>10.0

86.1543

88.7816

2.6273

Cup 2

5.5 to 10.0

85.6025

85.6433

0.0408

Cup 3

2.4 to 5.5

85.9395

85.9548

0.0153

Cup 4

1.61 to 2.4

85.7216

85.7288

0.0072

Cup 5

0.307 to 1.61

85.8571

85.8573

0.0002

Filter

<0.307

75.5386

75.5404

0.0018

 

Mass of test item found in artificial throat: 0.26 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 2.95 g.


Determination 2

 

Table 3.18

 

Collection Stage

Particle Size Range Collected (µm)

Mass (g)

Pre-sampling

Post-sampling

Difference

Cup 1

>10.0

86.1168

88.6874

2.5706

Cup 2

5.5 to 10.0

85.5581

85.6647

0.1066

Cup 3

2.4 to 5.5

85.9077

85.9158

0.0081

Cup 4

1.61 to 2.4

85.6864

85.6876

0.0012

Cup 5

0.307 to 1.61

85.8565

85.8578

0.0013

Filter

<0.307

75.5343

75.5369

0.0026

 

Mass of test item found in artificial throat: 0.28 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 2.97 g.

 

Determination 3

 

Table 3.19

 

Collection Stage

Particle Size Range Collected (µm)

Mass (g)

Pre-sampling

Post-sampling

Difference

Cup 1

>10.0

86.1163

88.8757

2.7594

Cup 2

5.5 to 10.0

85.5566

85.7113

0.1547

Cup 3

2.4 to 5.5

85.9078

85.9201

0.0123

Cup 4

1.61 to 2.4

85.6859

85.6877

0.0018

Cup 5

0.307 to 1.61

85.8575

85.8579

0.0004

Filter

<0.307

75.5385

75.5419

0.0034

 

Mass of test item found in artificial throat: 0.16 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.09 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 3.20

 

Particle Size Cut-point (µm)

Cumulative Mass (g)

Cumulative Percentage (%)

Determination 1

Determination 2

Determination 3

Determination 1

Determination 2

Determination 3

10.0

0.0653

0.1198

0.1726

2.21

4.03

5.58

5.5

0.0245

0.0132

0.0179

0.830

0.444

0.579

2.4

0.0092

0.0051

0.0056

0.312

0.172

0.181

1.61

0.0020

0.0039

0.0038

6.8 x 10-2

0.131

0.123

0.307

0.0018

0.0026

0.0034

6.1 x 10-2

8.8 x 10-2

0.110

 

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 3.21

 

Particle size

Cumulative Percentage (%)

Determination 1

Determination 2

Determination 3

Overall

<10.0 µm

2.21

4.03

5.58

5.58

<5.5 µm

0.830

0.444

0.579

0.830

Particle size data acquired for the test item is shown in the following table:

 

Table 3.22

 

Measurement

Method

Result

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

Sieve

13.8 %

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

Cascade Impactor

5.58 %

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

Cascade Impactor

0.830 %

Conclusions:
Conclusion
Particle size data acquired for the test item is shown in the following table:

Table 3.22
Measurement Method Result
Proportion of test item having an Sieve 13.8 %
inhalable particle size <100 µm


Proportion of test item having a Cascade Impactor ≤5.58 %
thoracic particle size <10.0 µm


Proportion of test item having a Cascade Impactor ≤0.830 %
respirable particle size <5.5 µm
Executive summary:

Performance of the Test

Sieving Screening Test

The proportion of test item passing through a 100 µm sieve was determined using an Inclyno sieve shaker. A known mass (15.18 g) of test item was added to a 100 µm sieve fitted above a receiver pan of known mass. A lid was then secured onto the sieve and the assembled apparatus placed on the sieve shaker for a period of approximately 30 minutes. Following the shaking period, the mass of the receiver pan and collected test item was recorded and the percentage test item with a particle size <100 µm calculated as detailed in the data handling section.

Cascade Impactor

Test item (approximately 3 g) was passed into the artificial throat of a Marple Miller Cascade Impactor (MSP Corporation, Minneapolis, Minnesota, USA – Figure 3.4 - Attachment 1). During cascade impactor analysis, air was pulled through the impactor, by a vacuum pump, at a flow rate of approximately 60 L/min. The flow enters the impactor through a throat and inlet tube and accelerates through the stages. At each stage one or more nozzles direct the particle-laden airstream into a collection cup.

 

Particles larger than the cut size of that stage, impact onto the collection plate and stay in the collection cup. Smaller particles follow the airstream and are carried to the next stage. In succeeding stages the nozzles are smaller, the air velocity is higher and finer particles are collected. In the final stage the smallest particles are collected on a glass fibre filter. The mass of the collection cups and filter were recorded before and after each determination.

       

Conclusion

Particle size data acquired for the test item is shown in the following table:

 

Table 3.22

 

Measurement

Method

Result

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

Sieve

13.8 %

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

Cascade Impactor

5.58 %

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

Cascade Impactor

0.830 %

Description of key information

Following measurement of particle size according to OECD Guideline 110, the following fractions were determined:

Proportion of test item having an inhalable particle size <100 µm:  13.8 %; proportion of test item having a thoracic particle size <10.0 µm: ≤5.58 %;

proportion of test item having a respirable particle size <5.5 µm: ≤0.830 %.

      

Additional information