4-[(4-HYDROXYPYRIMIDIN-2-YL)AMINO]BENZONITRILE

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 April - 20 May 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

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of particle tested:

primary particle

Type of distribution:

volumetric distribution

Specific details on test material used for the study:

- Batch n°: M15GC2731
- Analytical purity: 99.8%
- Expiration date: 23 July 2016
- Storage condition: at room temperature protected from light

Mass median aerodynamic diameter:

13.369 µm

Geometric standard deviation:

>= 1.859 - <= 1.864

Percentile:

D10

Mean:

4.797 µm

St. dev.:

0.007

Percentile:

D50

Mean:

11.064 µm

St. dev.:

0.027

Percentile:

D90

Mean:

21.352 µm

St. dev.:

0.055

Visual Microscope Analysis

(1) Standard visual observation: sample observed to be a fine, off-white powder with clusters.

(2) 100x magnification: particles appeared to be irregular shaped crystals (smallest +/- 3 µm and largest +/- 26 µm).

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

Laser Diffraction Particle Size Analysis

The average volume weighted mean was determined to be 12.125 µm.

The average mode was determined to be 11.929 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.

Conclusions:

Visual examination at 100x magnification showed irregular shaped crystals between approximately 3 µm and 26 µm.
The particle size distribution of T002487 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 12.125 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 13.369 µm, whereas the average D10, D50 and the D90 were determined to be 4.797 µm, 11.064 µm and 21.352 µm, respectively.

Description of key information

The particle size distribution of T002487 was determined by the laser diffraction method in a Klimisch 1 GLP study according to the ISO 13320:2009 and CIPAC MT 187 method (Chilworth Technology Limited, 2016).

Visual examination at 100x magnification showed irregular shaped crystals between approximately 3 and 26 µm.

The Mass Median Aerodynamic Diameter (MMAD) was determined to be 13.369 µm. The average D10, D50 and the D90 were determined to be 4.797 µm, 11.064 µm and 21.352 µm, respectively.