6-fluoro-3-(piperidin-4-yl)-1,2-benzoxazole hydrochloride

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

17 August 2017 - 22 August 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2017

Report date:

2017

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

Test guideline 3

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

Test material

Test material information

Constituent 1

Reference substance name:

6-FLUORO-3-(PIPERIDIN-4-YL)-1,2-BENZOXAZOLE HYDROCHLORIDE

EC Number:

700-303-4

Cas Number:

84163-13-3

Molecular formula:

C12H13FN2O.HCl

IUPAC Name:

6-FLUORO-3-(PIPERIDIN-4-YL)-1,2-BENZOXAZOLE HYDROCHLORIDE

Test material form:

solid: particulate/powder

Specific details on test material used for the study:

- Batch n°: I16EC2452
- Expiration date: 22 November 2020 (retest date)
- Purity: 100.2% (based on assay for the test item)
- Storage condition of test material: At room temperature

Results and discussion

Mass median aerodynamic diameter:

225.6 µm

Geometric standard deviation:

>= 19.226 - <= 22.277

Particle size

Particle size 1

Percentile:

D10

Mean:

5.394 µm

St. dev.:

0.229

Remarks on result:

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

Particle size 2

Key result

Percentile:

D50

Mean:

189.32 µm

St. dev.:

2.862

Remarks on result:

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

Particle size 3

Percentile:

D90

Mean:

473.002 µm

St. dev.:

9.56

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 fine and medium gritty particles of white powder with clusters.

(2) 100x magnification: particles appeared to be irregular shaped crystals (smallest +/- 3 µm and largest +/- 272 µm)

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

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 0.02 µm to 2000 µm.

The average Volume weighted Mean was 214.928 µm and the mode was 288.624 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 272 µm.
The particle size distribution of T001492 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 214.928 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 225.6 µm, whereas the average D10, D50 and the D90 were determined to be 5.394 µm, 189.320 µm and 473.002 µm, respectively.