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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:
10 June 2016 - 15 June 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-17299412-AAA (T001599)
- Physical state: solid (powder)
- Appearance: white powder
Specific details on test material used for the study:
- Batch n°: I15HB2951
- Analytical purity: 100.2% (based on base assay titration)
- Expiration date: 09 August 2017
- Storage condition: at room temperature

Results and discussion

Mass median aerodynamic diameter:
33.505 µm
Geometric standard deviation:
>= 2.575 - <= 2.594
Particle sizeopen allclose all
Percentile:
D10
Mean:
8.225 µm
St. dev.:
0.093
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:
29.968 µm
St. dev.:
0.321
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:
75.801 µm
St. dev.:
0.838
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 medium to fine white powder with lumps and clusters. Some particles had formed into clumps.

(2) 100x magnification: particles appeared to be crystalline with needles and fibres (smallest +/- 3 µm and largest +/- 128 µm)

(3) 400x magnification: sample was observed to be made up of single crystalline particles which were transparent with rough surfaces. Some aggregations were present.

Solubility and Dispersability Test

The sample proved to be insoluble and well dispersed in Silicone oil. Therefore, Silicone oil was used as the suspension fluid.

 

Laser Diffraction Particle Size Analysis

Using the identified parameters, the particle size was analysed over the range 0.2 μm to 2000 μm.

The average Volume weighted Mean was 36.908 µm and the mode was 39.990 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 crystalline with needles and fibres between approximately 3 µm and 128 µm.
The particle size distribution of T001599 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 36.908 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 33.505 µm, whereas the average D10, D50 and the D90 were determined to be 8.225 µm, 29.968 µm and 75.801 µm, respectively.