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Physical & Chemical properties

Particle size distribution (Granulometry)

Administrative data

Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
13 June 2016 - 11 October 2016
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2016
Report Date:
2016

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
other: ISO 13320-1
Deviations:
no
Qualifier:
according to
Guideline:
other: CIPAC MT 187
Deviations:
no
Qualifier:
according to
Guideline:
other: Chilworth Technology Ltd SOP n°417
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
Laser scattering/diffraction
Type of distribution:
volumetric distribution

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder
Details on test material:
- Name of test material (as cited in study reports): JNJ-40064973-AAA (Isonicotinezuur)
- Physical state: solid (powder)
- Appearance: white powder
Specific details on test material used for the study:
- Batch n°: M15HB3488
- Expiration date: 30 July 2020
- Purity: 98.9% (based on assay acid titration)
- Storage condition of test material: at room temperature

Results and discussion

Mass median aerodynamic diameter:
21.525 µm
Geometric standard deviation:
>= 2.2 - <= 2.234
Particle sizeopen allclose all
Percentile:
D10
Mean:
6.285 µm
St. dev.:
0.04
Remarks on result:
other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.
Key result
Percentile:
D50
Mean:
17.575 µm
St. dev.:
0.258
Remarks on result:
other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.
Percentile:
D90
Mean:
40.598 µm
St. dev.:
0.596
Remarks on result:
other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

Any other information on results incl. tables

Visual Microscope Analysis

(1) Standard visual observation: sample observed to be a fine, white powder with clusters.

(2) 100x magnification: particles appeared to be irregular shaped crystals (smallest +/- 3 µm and largest +/- 45 µm)

(3) 400x magnification: sample was observed to be made up of single crystalline particles.

Laser Diffraction Particle Size Analysis

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

The average Volume weighted Mean was 20.856 µm and the mode was 20.027 µm. The Coefficient of Variation for d50 was <3%; d10 and d90 were <5%. Thus the repeatability of the characteristic particles in the size distribution was within the acceptable limits according to the ISO 13320-1 test standard.

Applicant's summary and conclusion

Conclusions:
Visual examination at 100x magnification showed irregular shaped crystals between approximately 3 µm and 45 µm.
The particle size distribution of Isonicotinezuur determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 20.856 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 21.525 µm, whereas the average D10, D50 and the D90 were determined to be 6.285 µm, 17.575 µm and 40.598 µm, respectively.