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

7 July - 12 September 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 distribution:

volumetric distribution

Specific details on test material used for the study:

- Batch n°: I15AB0305
- Analytical purity: 99.7% (based on LC)
- Expiration date: 23 January 2017
- Storage condition: at room temperature

Mass median aerodynamic diameter:

22.131 µm

Geometric standard deviation:

>= 2.665 - <= 2.759

Percentile:

D10

Mean:

5.061 µm

St. dev.:

0.105

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:

20.287 µm

St. dev.:

0.17

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:

57.824 µm

St. dev.:

0.269

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. Some of the clusters were found to be > 2000μm

(2) 100x magnification: particles appeared to be irregular shaped crystals with needles and fibres. Some agglomerations were observed. The smallest individual particle size was approximately 3μm and the largest individual size was approximately 192μm.

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

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 27.283µm and the mode was 22.610µm. 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 with needles and fibres between approximately 3µm and 192µm.
The particle size distribution of T003422 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 27.283µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 22.131µm, whereas the average D10, D50 and the D90 were determined to be 5.061µm, 20.287µm and 57.824µm, respectively.

Description of key information

The particle size distribution of T003422 was determined by the laser diffraction method in a GLP study according to the methods ISO 13320:2009 and CIPAC MT 187 (Livingston, 2016). The visual examination at 100x magnification showed irregular crystals with needles and fibres of dimensions between 3 µm and 192 µm approximately. The MMAD (mass median aerodynamic diameter) was determined to be 22.131 µm, whereas the average D10, D50 and the D90 were determined to be 5.061µm, 20.287µm and 57.824µm, respectively.