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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:
21 June 2016 to 23 June 2016
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)
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Type of method:
Laser scattering/diffraction
Key result
Percentile:
D10
Mean:
26.22 µm
St. dev.:
0.366
Key result
Percentile:
D50
Mean:
197.131 µm
St. dev.:
2.287
Key result
Percentile:
D90
Mean:
534.74 µm
St. dev.:
5.764

Visual Observations

- Standard visual observation: Sample observed to be a coarse, gritty free flowing red to brown solid. Most of the sample

particles appear to be > 2 000 μm, therefore sieve analysis was employed.

- Observation at 100 x magnification: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 μm and the largest individual size was >2 000 μm.

- Observation at 400 x magnification: The sample was observed to be made up of single crystalline particles.

 

Manula Sieve Analysis

- 13.7 % of the test material by weight was < 2 000 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

241.6

295.8

54.2

13.7

>2000

325.8

667.4

341.6

86.3

TOTALS

395.8

100.0

 

Solubility Test

- The sample proved to be insoluble, and well dispersed in silicone oil. Therefore silicone oil was used as a dispersant for the analysis.

LASER DIFFRACTION

- Results can be seen in Tables 2 and 3.

4.58 % 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

245.696

248.554

252.004

243.708

247.208

247.434

Median (d.50)

199.867

198.637

198.288

195.050

193.856

197.131

Mode (μm)

298.621

293.195

290.881

292.856

285.551

292.154

*MMAD

223.904

222.526

222.136

218.508

217.171

220.84

10 % of material is <

26.698

26.469

26.339

25.915

25.700

26.220

50 % of material is <

199.867

198.637

198.288

195.050

193.856

197.131

90 % of material is <

530.283

540.910

542.311

527.894

532.738

534.740

* Mass Median Aerodynamic Diameter

**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

26.698

26.469

26.339

25.915

25.700

0.366

1.4

d50

199.867

198.637

198.288

195.050

193.856

2.287

1.2

d90

530.283

540.910

542.311

527.894

532.738

5.764

1.1

d15.78

47.201

46.737

46.520

45.798

45.330

0.670

1.4

GSD

4.234

4.250

4.262

4.259

4.277

0.014

0.3

MMAD

223.90

222.53

222.14

218.51

217.17

2.56

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 this study the d10, d50 and d90 of the test material were 26.220, 197.131 and 534.740 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.

4.58 % 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 26.220, 197.131 and 534.740 µm, respectively.

Description of key information

Under the conditions of this study the d10, d50 and d90 of the test material were 26.220, 197.131 and 534.740 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.

4.58 % 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 26.220, 197.131 and 534.740 µm, respectively.

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