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Physical & Chemical properties

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:
24-06-2019
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:
ISO 13320:2009 “Particle Size Analysis – Laser Diffraction Methods”, 2009
Deviations:
no
GLP compliance:
yes
Type of method:
Laser scattering/diffraction
Type of particle tested:
agglomerate
Type of distribution:
volumetric distribution
Specific details on test material used for the study:
No further details specified in the study report
Mass median aerodynamic diameter:
21.231 µm
Geometric standard deviation:
2.275
Key result
Percentile:
D10
Mean:
8.33 µm
St. dev.:
0.008
Key result
Percentile:
D50
Mean:
18.7 µm
St. dev.:
0.024
Key result
Percentile:
D90
Mean:
37.2 µm
St. dev.:
0.118
No.:
#1
Size:
< 10 µm
Distribution:
14.71 %

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 kerosene 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: Kerosene

Dispersion speed: 1700 rpm

Refractive index (sample): 0.000n

Absorption: 0.000 AU

Analysis Model: General Purpose

 

Using the identified parameters, the particle size was analysed over the range 0.01 μm to 3500 μm.

 

Full Test Results

 

Run 1

Run 2

Run 3

Run 4

Run 5

Average

STDVP

% STDVP

VWM

23.8

23.8

23.6

23.9

24.4

23.9

N/A

N/A

Mode

19.7

19.6

19.6

19.6

19.6

19.6

N/A

N/A

d10

8.34

8.33

8.32

8.33

8.34

8.33

0.00778

0.0934

d50 (Median)

18.8

18.8

18.7

18.7

18.7

18.7

0.0241

0.129

d90

37.1

37.2

37.0

37.1

37.3

37.2

0.118

0.318

MMAD

21.262

21.255

21.196

21.216

21.227

21.231

0.025

0.1

GSD

2.269

2.272

2.264

2.276

2.297

2.275

0.011

0.5

All particle size results are in µm

 

14.71% by volume of sample was seen to be <10.00 µm

 

Definitions

VWM: volume weighted mean

d10: 10% of the test item is less than this particle size

d50: 50% of the test item is less than this particle size

d90: 90% of the test item in less than this particle size

GSD: geometric standard deviation of the lognormal particle size distribution

MMAD: mass median aerodynamic diameter

Average: calculated from the entirety of the data captured in each run and not a simple arithmetic mean

STDVP: standard deviation of the population

% STDVP: percentage standard deviation of the population

 

The 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 is within the acceptable limits as per the ISO 13320-1 test standard.

Conclusions:
14.71% by volume of sample was seen to be <10.00 µm
Executive summary:

 

Particle Size Analysis using small volume (wet) module (SVM)

Average (µm)

Volume weighted mean

23.9

Median (d50)

18.7

Mode

19.6

MMAD (Mass Median Aerodynamic Diameter)

21.231

10% of material is <

8.33

50% of material is <

18.7

90% of material is <

37.2

By volume of sample was seen to be < 10.00 µm

14.71%

 

Description of key information

 

Particle Size Analysis using small volume (wet) module (SVM)

Average (µm)

Volume weighted mean

23.9

Median (d50)

18.7

Mode

19.6

MMAD (Mass Median Aerodynamic Diameter)

21.231

10% of material is <

8.33

50% of material is <

18.7

90% of material is <

37.2

By volume of sample was seen to be < 10.00 µm

14.71%

 

Additional information