cis-2-(bromomethyl)-2-(2,4-dichlorophenyl)-1,3-dioxolane-4-ylmethyl benzoate

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

14 November 2016 - 02 December 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: ISO 13320-1

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: Chilworth Technology Ltd SOP n°417

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of distribution:

volumetric distribution

Specific details on test material used for the study:

- Batch n°: I15DB1648
- Expiration date: 19 April 2020
- Purity: 96.70% (based on chromatographic purity)
- Storage condition of test material: at room temperature

Mass median aerodynamic diameter:

12.525 µm

Geometric standard deviation:

>= 3.147 - <= 3.216

Percentile:

D10

Mean:

1.795 µm

St. dev.:

0.033

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:

9.902 µm

St. dev.:

0.212

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:

34.303 µm

St. dev.:

1.284

Remarks on result:

other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

Visual Microscope Analysis

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

(2) 100x magnification: particles appeared to be irregular shaped crystals (smallest +/- 3 µm and largest +/- 80 µm)

(3) 400x magnification: sample was observed to be made up of single crystalline particles and agglomerated 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 14.621 µm and the mode was 10.143 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.

Conclusions:

Visual examination at 100x magnification showed irregular shaped crystals between approximately 3 µm and 80 µm.
The particle size distribution of T001095 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 14.621 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 12.525 µm, whereas the average D10, D50 and the D90 were determined to be 1.795 µm, 9.902 µm and 34.303 µm, respectively.

Description of key information

In the guideline study (Livingston, 2016) the test item, JNJ-16479671AAA (T001095) on visual examination at 100x magnification showed irregular shaped crystals between approximately 3 µm and 80 µm. The particle size distribution of T001095 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 14.621 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 12.525µm, whereas the average D10, D50 and the D90 were determined to be 1.795µm, 9.902µm and  34.303µm, respectively. Results of this study are reliable without restrictions.