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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:
17 August 2016 to 19 December 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)
Version / remarks:
2009
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: CIPAC MT 187
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:
45.275 µm
Geometric standard deviation:
0.003
Key result
Percentile:
D50
Mean:
< 60.367 µm
St. dev.:
0.186

Optical Microscope Analysis

Standard visual observation: Sample observed to contain fine, medium and coarse, particles of white powder with clusters and agglomerations.

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 approximately 144 μm.

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

 

Manual Sieve Analysis

Manual sieve analysis indicated that 82.5 % by weight of the sample had a particle size of < 500 μm.

 

Laser Diffraction Analysis

Using the identified parameters, the particle size was analysed over the range 0.02 μm to 2000 μm.

Results can be seen in Tables 1 and 2.

Table 1: Summary of Test Results

Result

Average result (µm) of 5 runs

Volume weighted mean

93.473

Median

60.367

Mode

58.894

Mass median aerodynamic diameter (MMAD)

45.275

d10 - 10 % of material is <

20.858

d50 - 50 % of material is <

60.367

d90 - 90 % of material is <

202.378

 2.67 % by volume of sample was see to be < 10.0 µm.

Table 2: Summary of standard deviation results

Result

Standard deviation of the population (STDVP)

%STDVP

d10 - 10 % of material is <

0.053

0.3

d50 - 50 % of material is <

0.186

0.3

d90 - 90 % of material is <

3.376

1.7

d15.78 - 15.78 % of material is <

0.062

0.2

Geometric standard deviation (GSD)

0.003

0.1

Mass median aerodynamic diameter (MMAD)

0.14

0.3

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.

Conclusions:
Under the conditions of this study the MMAD of the test material was 45.275 µm and the D50 was < 60.367 µm.
Executive summary:

The particle size of the test material was investigated in accordance with the standardised guideline ISO 13320:2009 and CIPAC MT 187 under GLP conditions.

Following from optical microscope analysis and manual sieve analysis, laser diffraction was performed.

Under the conditions of this study the MMAD of the test material was 45.275 µm and the D50 was < 60.367 µm.

Description of key information

Under the conditions of this study the MMAD of the test material was 45.275 µm and the D50 was < 60.367 µm.

Additional information

The particle size of the test material was investigated in accordance with the standardised guideline ISO 13320:2009 and CIPAC MT 187 under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Following from optical microscope analysis and manual sieve analysis, laser diffraction was performed.

Under the conditions of this study the MMAD of the test material was 45.275 µm and the D50 was < 60.367 µm.