1-benzhydrylpiperazine

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:

15 June - 17 June 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°: M15BB1451
- Analytical purity: 98.8% (based on base titration)
- Expiration date: 30 January 2021
- Storage condition: at room temperature

Mass median aerodynamic diameter:

272.851 µm

Geometric standard deviation:

>= 2.832 - <= 3.137

Key result

Percentile:

D50

Mean:

252.251 µm

St. dev.:

1.78

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:

D10

Mean:

15.672 µm

St. dev.:

0.677

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:

509.637 µm

St. dev.:

15.289

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 polydispersed white powder with clusters.

(2) 100x magnification: particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 µm and the largest individual size was approximately 400 µm.

(3) 400x magnification: sample was observed to be made up of single crystalline particles which were transparent with rough surfaces. Some agglomerations were present.

Solubility and Dispersability 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 0.2 μm to 2000 μm.

The average Volume weighted Mean was 268.219 µm and the mode was 302.763 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 400µm.
The particle size distribution of T000750 determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 268.219µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 272.851µm, whereas the average D10, D50 and the D90 were determined to be 15.672µm, 252.251µm and 509.637µm, respectively.

Description of key information

The particle size distribution of T000750 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  of dimensions between 3 µm and 400 µm approximately. The MMAD (mass median aerodynamic diameter) was determined to be 272.851 µm, whereas the average D10, D50 and the D90 were determined to be 15.672µm, 252.251µm and 509.637µm, respectively.