Benzonitrile, 4-[(1,6-dihydro-4-hydroxy-6-oxo-2-pyrimidinyl)amino]-

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:

17 August 2015 - 2 September 2015

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 distribution:

volumetric distribution

Mass median aerodynamic diameter:

18.995 µm

Geometric standard deviation:

>= 2.429 - <= 2.436

Percentile:

D10

Mean:

4.753 µm

St. dev.:

0.009

Percentile:

D50

Mean:

15.407 µm

St. dev.:

0.035

Percentile:

D90

Mean:

39.042 µm

St. dev.:

0.186

Visual Microscope Analysis

(1) Standard visual observation: sample observed to be a fine/medium slight beige powder with lumps and clusters

(2) 100x magnification: particles appeared to be crystalline needles/fibres (smallest +/- 3 µm and largest +/- 70 µm)

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

Solubility 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 19.024 µm and the mode was 17.451 µm. The Coefficient of Variation for d50 was <3%; d10 and d90 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 crystalline fibres/needles between approximately 3 µm and 70 µm.
The particle size distribution of T002326 determined by the laser diffraction method led to the conclusion that the average Volume weighted Mean based on 5 runs was 19.024 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 18.995 µm, whereas the average D10, D50 and the D90 were determined to be 4.753 µm, 15.407 µm and 39.042 µm, respectively.

Description of key information

The particle size distribution of T002326 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, 2015). The visual examination at 100x magnification showed crystalline fibres/needles between approximately 3 µm and 70 µm. The MMAD (mass median aerodynamic diameter) was determined to be 18.995 µm, whereas the average D10, D50 and the D90 were determined to be 4.753 µm, 15.407 µm and 39.042 µm, respectively.