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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:
19 November 2015 - 26 January 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
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
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

Test material

Constituent 1
Chemical structure
Reference substance name:
3-(2-CHLOROETHYL)-9-HYDROXY-2-METHYL-4H-PYRIDO[1,2-A]PYRIMIDIN-4-ONE HYDROCHLORIDE (1:1)
EC Number:
617-648-0
Cas Number:
849727-62-4
Molecular formula:
C11H11ClN2O2.HCl
IUPAC Name:
3-(2-CHLOROETHYL)-9-HYDROXY-2-METHYL-4H-PYRIDO[1,2-A]PYRIMIDIN-4-ONE HYDROCHLORIDE (1:1)
Test material form:
solid: particulate/powder
Remarks:
migrated information: powder
Details on test material:
- Name of test material (as cited in study report): JNJ-1692405-AAC (T002006)
- Physical state: solid
- Analytical purity: 97.5%
- Batch N°: I15BB0722
- Expiry date: 21 February 2017
- Storage condition: at room temperature

Results and discussion

Mass median aerodynamic diameter:
150.128 µm
Geometric standard deviation:
>= 1.74 - <= 1.744
Particle sizeopen allclose all
Key result
Percentile:
D10
Mean:
54.805 µm
St. dev.:
0.772
Key result
Percentile:
D50
Mean:
118.686 µm
St. dev.:
1.359
Key result
Percentile:
D90
Mean:
210.468 µm
St. dev.:
2.32

Any other information on results incl. tables

Visual Microscope Analysis

(1) Standard visual observation: sample observed to be a medium to coarse, free flowing almost white to ochre powder.

(2) 100x magnification: particles appeared to be irregular shaped crystals (smallest +/- 16 µm and largest +/- 112 µm).

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

Laser Diffraction Particle Size Analysis

Average volume weighted mean was determined to be 125.612 µm

Average mode was determined to be 126.875 µm

The Coefficient of Variation (CV) for d50 wass <3%. For d10 and d90 it was <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 16 µm and 112 µm.
The particle size distribution of T002006 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 125.612 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 150.128 µm with a standard deviation (of the population) of 1.72 µm, whereas the average D10, D50 and the D90 were determined to be 54.805 µm, 118.686 µm and 210.468 µm, respectively.