D-Glucitol, 1,5-anhydro-1-C-[3-[[5-(4-fluorophenyl)-2-thienyl]methyl]-4-methylphenyl]-, 2,3,4,6-tetraacetate, (1S)-

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:

25 January 2017 - 26 January 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°: I16CB1581
- Analytical purity: >99.9% (based on HPLC with impurities of 0.1%)
- Expiration date: 04 April 2019
- Storage condition: at room temperature

Mass median aerodynamic diameter:

7.638 µm

Geometric standard deviation:

>= 2.435 - <= 2.446

Percentile:

D10

Mean:

2.111 µm

St. dev.:

0.02

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:

6.599 µm

St. dev.:

0.06

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:

22.205 µm

St. dev.:

0.213

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 medium to fine white powder with lumps and 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 and agglomerated particles

 

Solubility and Dispersability Test

The sample proved to be insoluble and well dispersed in Kerosene. Therefore, Kerosene 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 10.569 µm and the mode was 6.250 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 3µm and 26µm.
The particle size distribution of T003066 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 10.569 µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 7.638 µm, whereas the average D10, D50 and the D90 were determined to be 2.111 µm, 6.599 µm and 22.205 µm, respectively.

Description of key information

The particle size distribution of T003066 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 26µm. The MMAD was determined to be 7.638 µm, whereas the average D10, D50 and the D90 were determined to be 2.111 µm, 6.599 µm and 22.205 µm, respectively.