4-bromo-2,2-diphenylbutanenitrile

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:

11 Aug 2016 - 04 Jan 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

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

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°: I16AB0081
- Analytical purity: >99.3% (based on chromatographic purity GC, the sum of impurities was 0.7%)
- Expiration date: 11 January 2018
- Storage condition: at room temperature

Mass median aerodynamic diameter:

25.402 µm

Geometric standard deviation:

>= 2.866 - <= 2.912

Percentile:

D10

Mean:

5.073 µm

St. dev.:

0.04

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:

21.242 µm

St. dev.:

0.224

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:

107.438 µm

St. dev.:

3.074

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 +/- 205 µm)

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

 

Manual Sieve Analysis

It was noted that 39.5 % of the test material by weight was < 850 µm.

 

Laser Diffraction Particle Size Analysis

Using the identified parameters, the particle size was analysed over the range 0.02μm to 2000μm.

The average Volume weighted Mean was 39.830 µm and the mode was 18.665 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 205 µm.
The particle size distribution of T000625 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 39.830 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 25.402 µm, whereas the average D10, D50 and the D90 were determined to be 5.073 µm, 21.242 µm and 107.438 µm, respectively.

Description of key information

The particle size distribution of T000625 was determined by the laser diffraction method in a GLP study according to Chilworth Technology Ltd SOP n°417, ISO 13320:2009 and CIPAC MT 187 (Livingston, 2017). The visual examination at 100x magnification showed irregular shaped crystals between approximately 3µm and 205µm. The MMAD was determined to be 25.402 µm, whereas the average D10, D50 and the D90 were determined to be 5.073 µm, 21.242 µm and 107.438 µm, respectively.