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Particle size distribution (Granulometry)

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Reference
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
02 April 2019 - 15 July 2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
2009
Deviations:
no
Qualifier:
according to
Guideline:
other: CIPAC MT 187: Particle Size Analysis by Laser Diffraction, Handbook K.
Version / remarks:
2007
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
Laser scattering/diffraction
Remarks:
Laser Diffraction Analysis, using the medium volume (wet) module (MVM)
Type of particle tested:
primary particle
Type of distribution:
mass based distribution
Specific details on test material used for the study:
Physical Description: Off-white powder
Storage Conditions: At room temperature protected from light desiccated
Purity/Composition correction factor: No correction factor required
Test item handling: Use amber glassware or wrap container in aluminum foil
Chemical name: 1-{4-[(4-benzoylphenyl)sulfanyl]phenyl}-2-methyl-2-(4-methylbenzenesulfonyl)propan-1-one
CAS number: 272460-97-6
EC Number: 429-040-0
Molecular weight: 515
Mass median aerodynamic diameter:
6.2 µm
Geometric standard deviation:
9.976
Percentile:
D10
Mean:
0.106 µm
St. dev.:
0.001
Percentile:
D50
Mean:
5.34 µm
St. dev.:
0.101
Percentile:
D90
Mean:
90.6 µm
St. dev.:
1.71

Solubility and Dispersability Test

Preliminary test

The results of the preliminary test to select a suitable dispersant are given below:

Solvent used Soluble (Yes/No) Comments
Milli-Ro water No floats on the surface
2-Propanol No Well dispersed
Cyclohexane No Well dispersed
Methanol No Well dispersed
Polyethyleneglycol 300 No poor dispersability

2-Propanol and methanol were identified as suitable dispersants, as the substance visually did not dissolve, and because it was homogenously and there was no tendency to agglomerate formation dispersed.

Main Test

In the preliminary test, the substance was concluded to be visually insoluble in the dispersant, thus only dispersability was investigated in the main test. The result of the main test are given below:

Dispersability in 2-Propanol

  Test 1 (1.5 mg)  Test 2 (5.0 mg)
Time elapsed  1 2 1 2
10 seconds Well dispersed Well dispersed
30 minutes Well dispersed Well dispersed
60 minutes Well dispersed Well dispersed
90 minutes Well dispersed Well dispersed

Dispersability in Methanol

  Test 1 (1.5 mg)  Test 2 (5.0 mg)
Time elapsed  1 2 1 2
10 seconds Well dispersed Well dispersed
30 minutes Well dispersed Well dispersed
60 minutes Well dispersed Well dispersed
90 minutes Well dispersed Well dispersed

The test item proved to be homogeneously and well dispersed in both 2-propanol and methanol.  2-Propanol was used as the dispersant in the Laser Diffraction Analysis.

Particle Size Distribution by Laser Diffraction Analysis

The particle size distribution of the test item was analysed over the range 0.01 µm to 3500 µm.

The results of the analysis are presented below. A graph of volume fraction (%) versus particle diameter (µm) and the full particle size distribution list is provide in the attached illustration (average of 5 runs).

  Run 1 Run 2 Run 3 Run 4 Run 5 Mean STDVP %STDVP
Volume weighted mean 30.2 29.9 28.8 30.3 29.6 29.8 0.603 2.03
Mode 3.01 3.01 3.01 3.01 3.01 3.01 0.00252 0.0837
d10 (10% of material is <) 0.107 0.107 0.106 0.106 0.106 0.106 0.000516 0.486
d50 (50% of material is <) 5.49 5.37 5.28 5.36 5.22 5.34 0.101 1.89
d90 (90% of material is <) 91.9 90.3 88.1 92.6 90.3 90.6 1.71 1.89
GSD  9.987 9.959 9.894 10.041 10.001 9.976 0.055 0.55
MMAD 6.2

All results are in µm.

Definitions

GSD - geometric standard deviation of the lognormal particle size distribution

MMAD - mass median aerodynamic diameter

Mean - 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

The coefficient of variation for d50 is less than 3%, d10 and d90 are less than 5%. It can be concluded that the repeatability of the characteristic particles in the size distribution are within the acceptable limits.

Conclusions:
The particle size distribution of the test item was determined by means of Laser Diffraction Analysis using the medium volume (wet) module (MVM).
The D50 of the test item was determined to be 5.34 µm, the D10 was 0.106 µm and the D90 was 90.6 µm. The MMAD of the test item was calculated to be 6.20 µm.
Executive summary:

The objective of this study was to determine the particle size distribution of Esacure 1001 M.

The summary of the results is listed below:

Particle Size Analysis using medium volume (wet) module (MVM) Average (µm)
Volume weighted mean 29.8
Mode 3.01
D10 (10% of material is <) 0.106
D50 (50% of material is <) 5.34
D90 (90% of material is <) 90.6
MMAD (mass median aerodynamic diameter) 6.2
Volume of sample <10.00 µm 0.61% (<9.86 µm)

The particle size distribution of the test item was determined by means of Laser Diffraction Analysis using the medium volume (wet) module (MVM).

The D50 of the test item was determined to be 5.34 µm, the D10 was 0.106 µm and the D90 was 90.6 µm. The MMAD of the test item was calculated to be 6.20 µm.

Description of key information

The particle size distribution of the test item was determined by means of Laser Diffraction Analysis using the medium volume (wet) module (MVM).

The D50 of the test item was determined to be 5.34 µm, the D10 was 0.106 µm and the D90 was 90.6 µm. The MMAD of the test item was calculated to be 6.20 µm.

Additional information

Study conducted to recognised testing guidelines with GLP certification.