ethyl (3-benzoyl-2,4,6-trimethylbenzoyl)(phenyl)phosphinate

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:

13 Setember 2019 to 24 September 2019

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)

Version / remarks:

2009

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”.

Version / remarks:

2007

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

Remarks on result:

not measured/tested

Key result

Percentile:

D10

Mean:

8.98 µm

St. dev.:

0.169

Key result

Percentile:

D50

Mean:

35.9 µm

St. dev.:

0.626

Key result

Percentile:

D90

Mean:

105 µm

St. dev.:

2.69

Size:

< 10 µm

Distribution:

11.42 %

Remarks on result:

other: by volume

Optical Microscope Analysis

- Direct observation: Test material observed to be a fine-medium white powder with clusters.

- Under a microscope at 100x magnification: The particles appeared to be irregular shaped crystals that consisted of individual particles and some agglomerations. The smallest individual particle size was approximately 3 µm and the largest individual size was approximately 128 µm.

- Under a microscope at 400x magnification: The test material was observed to be made up of single crystalline particles, some of which had agglomerated.

Preliminary Solubility and Dispersability

Kerosene: not soluble but well dispersed

Silicone oil: not soluble but well dispersed

Main Solubility and Dispersibility Study

The test material was well dispersed in two of the two solvents tested (kerosene and silicone oil). Silicone oil was selected for the analysis as it could hold particles in suspension for a longer duration due to its viscosity.

Laser Diffraction Particle Size Analysis

During the method development phase of the analysis trials were conducted using both the small volume (wet) module (SVM). The SVM trials were conducted using silicone oil as the dispersant. The results of these trials indicated that the most appropriate test and material parameters to obtain the optimum measurements were:

Module: SVM

Dispersant: Silicone Oil

Dispersion speed: 2200 rpm

Refractive index (sample): 0.00 n

Absorption: 0.0 AU

Analysis Model: General Purpose

Using the identified parameters, the particle size was analysed over the range 0.01 µm to 3500 µm.

Laser Diffraction Particle Size Analysis

	Run 1	Run 2	Run 3	Run 4	Run 5	Average	STDVP	% STDVP
VWM	47.2	46.2	48.5	48.1	46.9	47.47	N/A	N/A
Mode	35.4	36.0	367	38.1	38.8	36.9	N/A	N/A
d10	8.81	8.81	9.02	9.18	9.10	8.98	0.169	1.88
d50 (median)	35.4	35.1	36.2	36.6	36.1	35.9	0.626	1.75
d90	105	102	108	106	102	105	2.69	2.57
GSD	2.918	2.896	2.931	2.884	2.881	2.902	0.128	4.6

All particle size results are in µm.

VWM: Volume weighted mean.

d10: 10 % of the test item is less than this particle size.

d50: 50 % of the test item is less than this particle size.

d90: 90 % of the test item is less than this particle size.

GSD: Geometric standard deviation of the lognormal particle size distribution.

Average: Calculated from the entirety of the data captured in each run and not a simple arithmetic mean.

STDVP: Standard deviation of the population.

% STDVP: percentage standard deviation of the population.

11.42 % by volume of sample was seen to be < 10.00 µm.

The coefficient of variation for D50 is less than 3 %; D10 and D90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution is within the acceptable limits as per the ISO 13320-1 test standard.

Conclusions:

Under the conditions of the study, findings from the average of five runs revealed the following results on the particle size of the test material:
- Volume weighted mean: 47.47 µm
- D10: 8.98 µm
- D50: 35.9 µm
- D90: 105 µm
11.42 % by volume of sample was seen to be < 10.00 µm.
The coefficient of variation for D50 is less than 3 %; D10 and D90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution is within the acceptable limits as per the ISO 13320-1 test standard.

Executive summary:

The particle size distribution of the test material was determined by laser diffraction, under GLP conditions and according to the standardised guideline ISO 13320-1.

Under the conditions of the study, findings from the average of five runs revealed the following results on the particle size of the test material:

- Volume weighted mean: 47.47 µm

- D10: 8.98 µm

- D50: 35.9 µm

- D90: 105 µm

11.42 % by volume of sample was seen to be < 10.00 µm.

The coefficient of variation for D50 is less than 3 %; D10 and D90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution is within the acceptable limits as per the ISO 13320-1 test standard.

Description of key information

Under the conditions of the study, findings from the average of five runs revealed the following results on the particle size of the test material:

- Volume weighted mean: 47.47 µm

- D10: 8.98 µm

- D50: 35.9 µm

- D90: 105 µm

11.42 % by volume of sample was seen to be < 10.00 µm.

The coefficient of variation for D50 is less than 3 %; D10 and D90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution is within the acceptable limits as per the ISO 13320-1 test standard.

Additional information

The particle size distribution of the test material was determined by laser diffraction, under GLP conditions and according to the standardised guideline ISO 13320 -1.

Under the conditions of the study, findings from the average of five runs revealed the following results on the particle size of the test material:

- Volume weighted mean: 47.47 µm

- D10: 8.98 µm

- D50: 35.9 µm

- D90: 105 µm

11.42 % by volume of sample was seen to be < 10.00 µm.

The coefficient of variation for D50 is less than 3 %; D10 and D90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution is within the acceptable limits as per the ISO 13320-1 test standard.