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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:
07 December 2017 to 04 January 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
2009
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: IPAC MT 187 “Particle Size Analysis by Laser Diffraction”
Version / remarks:
Handbook K, 2007.
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Mass median aerodynamic diameter:
45.396 µm
Geometric standard deviation:
0.007
Key result
Percentile:
D10
Mean:
3.27 µm
St. dev.:
0.025
Key result
Percentile:
D50
Mean:
17.486 µm
St. dev.:
0.213
Key result
Percentile:
D90
Mean:
47.431 µm
St. dev.:
1.059

- During the method development phase of the analysis trials were conducted using the small volume (wet) module (SVM) only. The SVM trials were conducted using water as the dispersant. The results of these trials indicated that the most appropriate test and material parameters to obtain the optimum measurements were.

Module: SVM

Dispersant: Water

Dispersion speed: 1500 rpm

Refractive index (sample): 0.000 n

Absorption: 0 AU

Analysis Model: General Purpose (Normal)

- Using the identified parameters, the particle size was analysed over the range 0.02 μm to 2000 μm. The results of the formal analysis are presented in Table 1.

- 30.79 % by volume of sample was seen to be < 10.00 μm.

- Coefficient of variation for d50 is less than 3 %; d10 and d90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the ISO 13320-1 test standard.

Table 1: Full Test Results

 

Run 1

Run 2

Run 3

Run 4

Run 5

Average **

Volume weighted mean

23.243

23.401

23.227

22.013

22.473

22.872

Median

17.671

17.724

17.570

17.272

17.199

17.486

Mode

23.629

23.574

23.580

23.636

23.281

23.539

MMAD

45.877

46.015

45.615

44.839

44.652

45.396

d10- 10 % of material is <

3.290

3.300

3.279

3.245

3.237

3.270

d50- 50 % of material is <

17.671

17.724

17.570

17.272

17.199

17.486

d90- 90 % of material is <

49.171

49.603

48.673

46.795

47.431

48.313

All results are in μm

* Mass median aerodynamic diameter

** Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

 

Table 2: Standard Deviation Results

 

Run 1

Run 2

Run 3

Run 4

Run 5

STDVP

% STDVP

d10 - 10 % of material is <

3.290

3.300

3.279

3.245

3.237

0.025

0.8

d50 - 50 % of material is <

17.671

17.724

17.570

17.272

17.199

0.213

1.2

d90 - 90 % of material is <

49.171

49.603

48.673

46.795

47.431

1.059

2.2

d15.78 - 15.78 % of material is <

4.922

4.931

4.888

4.825

4.808

0.050

1.0

GSD

3.590

3.594

3.595

3.580

3.577

0.007

0.2

MMAD

45.877

46.015

45.615

44.839

44.652

0.552

1.2

GSD = Geometric standard deviation of the lognormal particle size distribution (calculated from d50/d15.78)

STDVP = standard deviation of the population

% STDVP = percentage standard deviation of the population

Conclusions:
Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.
Executive summary:

The particle size distribution of the test material was determined in accordance with the standardised guidelines ISO 13320:2009 and CIPAC MT 187 under GLP conditions using particle size apparatus based on laser diffraction.

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.

Description of key information

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.

Additional information

The particle size distribution of the test material was determined in accordance with the standardised guidelines ISO 13320:2009 and CIPAC MT 187 under GLP conditions using particle size apparatus based on laser diffraction. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.