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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:
25 June 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
Qualifier:
according to guideline
Guideline:
other: Chilworth Technology Limited Standard Operating Procedures (CTL SOP No. 417)
Deviations:
no
Qualifier:
according to guideline
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Deviations:
no
Qualifier:
according to guideline
Guideline:
other: CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”, Handbook K
Version / remarks:
2007
GLP compliance:
yes (incl. QA statement)
Type of method:
Laser scattering/diffraction
Remarks:
and optical microscope analysis
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Mass median aerodynamic diameter:
166 µm
Geometric standard deviation:
0.03
Percentile:
D10
Mean:
3.95 µm
St. dev.:
0.072
Percentile:
D50
Mean:
129 µm
St. dev.:
2.26
Percentile:
D90
Mean:
373 µm
St. dev.:
8.9

Optical Microscope Analysis

- Standard visual observation: Sample observed to be a fine to medium, yellowish powder with clusters.

- Observation using 3.2 objective lens: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 μm and the largest individual size was approximately 96 μm.

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

Solubility and Dispersability Test

 Solvent used  Soluble  Comments
 Water  No  Floats on surface
 2 -propanol  Yes  Soluble
 Methanol  No

 Well dispersed

The sample was well dispersed in two of the three solvents tested. For the full solubility and dispersability test methanol and water were selected.

In the full solubility test the sample proved to be insoluble and well dispersed in both methanol and water. Both solvents were therefore trialled as the dispersant.

Laser Diffraction

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 ISO 13320-1 test standard.

Conclusions:
Under the conditions of the study the MMAD was determined to be 166 µm while the D10, D50 and D90 were determined to be 3.95, 129 and 373 µm, respectively. 16.57 % of the particles were < 10 µm.
Executive summary:

A particle size analysis of the substance was conducted under GLP conditions and in accordance with the Standard Operating Procedures of the test laboratory and in accordance with ISO 13320:2009 “Particle Size Analysis – Laser Diffraction Methods”, 2009 and CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”, Handbook K, 2007.

Under the conditions of the study the MMAD was determined to be 166 µm while the D10, D50 and D90 were determined to be 3.95, 129 and 373 µm, respectively. 16.57 % of the particles were < 10 µm.

Description of key information

Under the conditions of the study the MMAD was determined to be 166 µm while the D10, D50 and D90 were determined to be 3.95, 129 and 373 µm, respectively. 16.57 % of the particles were < 10 µm.

Additional information

A particle size analysis of the substance was conducted under GLP conditions and in accordance with the Standard Operating Procedures of the test laboratory and in accordance with ISO 13320:2009 “Particle Size Analysis – Laser Diffraction Methods”, 2009 and CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”, Handbook K, 2007. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Under the conditions of the study the MMAD was determined to be 166 µm while the D10, D50 and D90 were determined to be 3.95, 129 and 373 µm, respectively. 16.57 % of the particles were < 10 µm.