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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:
8 September 2017 to 22 November 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
2009
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
Laser scattering/diffraction
Type of distribution:
volumetric distribution
Key result
Percentile:
D10
Mean:
117.782 µm
St. dev.:
2.307
Key result
Percentile:
D50
Mean:
565.432 µm
St. dev.:
6.223
Key result
Percentile:
D90
Mean:
1 241.385 µm
St. dev.:
5.055

VISUAL OBSERVATIONS

- Standard visual observation: Sample observed to be a polydispersed, brown solid with clusters.

- Observation using a 3.2 objective lens: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 19 µm and the largest individual size approximately 2640 µm.

- Observation using a 40 objective lens: The sample was observed to be made up of single crystalline particles.

 

MANUAL SIEVE ANALYSIS

- 94.1% of the test material by weight was < 2000 µm

- Results can be seen in Table 1.

Table 1: Results of the Manual Sieve Analysis

Sieve Size (µm)

Sieve Weight (g)

Sieve + Powder Weight (g)

Powder Weight (g)

% by Weight

< 2000

352.4

446.5

94.1

94.1

> 2000

326

331.9

5.9

5.9

TOTALS

100.0

100.0

 

LASER DIFFRACTION

- Results can be seen in Tables 2 and 3.

0.28 % by volume of the 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 test guideline.

 

Table 2: Laser Diffraction Full Test Results

 

Run 1

Run 2

Run 3

Run 4

Run 5

Average*

Volume Weighted Mean

625.425

631.510

639.382

625.533

628.887

630.148

Median

560.036

567.089

576.622

559.745

563.377

565.432

Mode

785.801

756.215

760.814

759.382

758.984

758.847

d10: 10 % of the material is <

116.625

118.923

121.753

115.048

116.914

117.782

d50: 50 % of the material is <

560.036

567.089

576.622

559.745

563.377

565.432

d90: 90 % of the material is <

1235.891

1240.976

1250.320

1237.303

1242.339

1241.385

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

 All results are in µm.

Table 3: Laser Diffraction Standard Deviation Results

 

Run 1

Run 2

Run 3

Run 4

Run 5

STDVP

%STDVP

d10: 10 % of the material is <

116.625

118.923

121.753

115.048

116.914

2.307

2.0

d50: 50 % of the material is <

560.036

567.089

576.622

559.745

563.377

6.223

1.1

d90: 90 % of the material is <

1235.891

1240.976

1250.320

1237.303

1242.339

5.055

0.4

d15.78: 15.78 % of the material is <

176.749

182.953

188.303

176.357

178.236

4.544

2.5

GSD

3.169

3.100

3.062

3.174

3.161

0.0440

1.4

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 this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.
Executive summary:

The particle size distribution of the test material was investigated in accordance with the standardised guideline ISO 13320, under GLP conditions.

The particle size was investigated using microscope analysis, manual sieving and laser diffraction.

0.28% by volume of the sample was seen to be < 10.00 µm. The coefficient of variation for d50 was 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 test guideline.

Under the conditions of this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.

Description of key information

Under the conditions of this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.

Additional information

The particle size distribution of the test material was investigated in accordance with the standardised guideline ISO 13320, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The particle size was investigated using microscope analysis, manual sieving and laser diffraction.

0.28% by volume of the sample was seen to be < 10.00 µm. The coefficient of variation for d50 was 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 test guideline.

Under the conditions of this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.