p-fluorophenyl 4-piperidyl ketone hydrochloride

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

12 December 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 guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

other: ISO 13320-1

Deviations:

no

Test guideline 2

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 distribution:

volumetric distribution

Test material

Test material information

Constituent 1

Reference substance name:

p-fluorophenyl 4-piperidyl ketone hydrochloride

EC Number:

247-070-0

EC Name:

p-fluorophenyl 4-piperidyl ketone hydrochloride

Cas Number:

25519-78-2

Molecular formula:

C12H14FNO.ClH

IUPAC Name:

4-(4-fluorobenzoyl)piperidine hydrochloride

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

- Name of test material (as cited in study report): JNJ-398099-AAC (T001047)
- Physical state: solid
- Analytical purity: 97.2%
- Batch N°: I15DB1484
- Expiry date: 19 April 2017
- Storage condition: at room temperature

Results and discussion

Mass median aerodynamic diameter:

12.04 µm

Geometric standard deviation:

>= 3.204 - <= 3.216

Particle size

Particle size 1

Percentile:

D10

Mean:

2.086 µm

St. dev.:

0.015

Particle size 2

Key result

Percentile:

D50

Mean:

10.52 µm

St. dev.:

0.088

Particle size 3

Percentile:

D90

Mean:

47.274 µm

St. dev.:

0.962

Any other information on results incl. tables

Visual Microscope Analysis

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

(2) 100x magnification: particles appeared to be irregular shaped crystals (smallest +/- 3 µm and largest +/- 304 µm)

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

Manual Sieve Analysis

The manual sieve analysis indicated that 93.5% by weight of the sample had a particle size of < 500 µm.

Laser Diffraction Particle Size Analysis

Average volume weighted mean was determined to be 20.511 µm.

Average mode was determined to be 10.040 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 3 µm and 304 µm.
The particle size distribution of T001047 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 20.511 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 12.040 µm with a standard deviation (of the population) of 0.10 µm, whereas the average D10, D50 and the D90 were determined to be 2.086 µm, 10.520 µm and 47.274 µm, respectively.