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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:
22/03/2018 to 11/04/2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reason / purpose:
reference to same study
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
ISO 13320:2009 “Particle Size Analysis – Laser Diffraction Methods”, 2009
Deviations:
no
Qualifier:
according to
Guideline:
other: CIPAC MT 187
Version / remarks:
CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”, Handbook K, 2007.
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
Laser scattering/diffraction
Type of particle tested:
aggregate
Type of distribution:
mass based distribution
Specific details on test material used for the study:
No further details specified.
Mass median aerodynamic diameter:
496.146 µm
Geometric standard deviation:
> 1.47 - < 1.559
Key result
Percentile:
D10
Mean:
236.133 µm
St. dev.:
5.539
Key result
Percentile:
D50
Mean:
395.654 µm
St. dev.:
7.782
Key result
Percentile:
D90
Mean:
653.894 µm
St. dev.:
30.812

Solubility and Dispersability Test for Particle Size Analysis

Table of solubility results

 

Dispersant used: Sunflower oil

 

Series 1

Series 2

Time elapsed

1

(1.5 mg)

2

(1.5 mg)

3

(1.5 mg)

1

(5.1 mg)

2

(5.0 mg)

3

(5.0 mg)

10 seconds

Well dispersed

Well dispersed

30 minutes

Well dispersed

Well dispersed

60 minutes

Well dispersed

Well dispersed

90 minutes

Well dispersed

Well dispersed

120 minutes

Well dispersed

Well dispersed

 

Dispersant used: Silicone oil

 

Series 1

Series 2

Time elapsed

1

(1.5 mg)

2

(1.5 mg)

3

(1.5 mg)

1

(4.9 mg)

2

(5.0 mg)

3

(5.0 mg)

10 seconds

Well dispersed

Well dispersed

30 minutes

Well dispersed

Well dispersed

60 minutes

Well dispersed

Well dispersed

90 minutes

Well dispersed

Well dispersed

120 minutes

Well dispersed

Well dispersed

 

Comments: Sunflower oil was initially selected for the test but showed poor reproducibility. The sample was well dispersed in silicone oil. Therefore, silicone oil was used as the dispersant.

 

Laser Diffraction Particle Size Analysis

Test Results

During the method development phase of the analysis trials were conducted using the small volume (wet) module (SVM). The SVM trials were conducted using silicone oil 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: Silicone oil

Dispersion speed: 2600 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.

 

Full Test Results

 

RUN 1

RUN 2

RUN 3

RUN 4

RUN 5

Average**

Volume weighted mean

421.122

421.130

434.047

405.720

440.820

424.568

Median

396.058

395.986

405.836

382.148

399.767

395.654

Mode

399.495

406.593

408.362

386.131

399.194

399.324

MMAD*

469.626

469.54

481.219

453.132

474.023

469.146

d10 (10% of material is <)

242.044

232.257

243.006

235.089

228.705

236.133

d50 (50% of material is <)

396.058

395.986

405.836

382.148

399.767

395.654

d90 (90% of material is <)

639.242

650.062

669.361

612.078

704.251

653.894

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.

0.00% by volume of sample was seen to be <10.00 µm.

 

Standard Deviation results

Run No.

1

2

3

4

5

STDVP

% STDVP

d10 (10% of material is <)

242.044

232.257

243.006

235.089

228.705

5.539

2.3

d50 (50% of material is <)

396.058

395.986

405.836

382.148

399.767

7.782

2.0

d90 (90% of material is <)

639.242

650.062

669.361

612.078

704.251

30.812

4.7

d15.78

268.077

259.523

270.268

259.922

256.437

5.350

2.0

GSD

1.477

1.526

1.502

1.470

1.559

0.033

2.2

MMAD

469.626

469.540

481.219

453.132

474.023

9.227

2.0

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

Executive summary:

To characterise the particle size distribution of the powder. The analysis is conducted initially using a visual microscope and is then undertaken more formally using a Laser Diffraction Particle Size Analyser.

 

Summary of Results

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

Average (µm)

Volume weighted mean

424.568

Median (d.50)

395.654

Mode

399.324

MMAD (Mass Median Aerodynamic Diameter)

469.146

10% of material is <

236.133

50% of material is <

395.654

90% of material is <

653.894

By volume of sample was seen to be <10.00 µm

0.00%

 

Description of key information

To characterise the particle size distribution of the powder. The analysis is conducted initially using a visual microscope and is then undertaken more formally using a Laser Diffraction Particle Size Analyser.

 

Summary of Results

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

Average (µm)

Volume weighted mean

424.568

Median (d.50)

395.654

Mode

399.324

MMAD (Mass Median Aerodynamic Diameter)

469.146

10% of material is <

236.133

50% of material is <

395.654

90% of material is <

653.894

By volume of sample was seen to be <10.00 µm

0.00%

 

Additional information