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Physical & Chemical properties

Particle size distribution (Granulometry)

Administrative data

Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
30 April 2019 to 30 May 2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019

Materials and methods

Test guideline
Qualifier:
according to
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions - Method A: Particle Size Distribution (effective hydrodynamic radius)
Deviations:
no
GLP compliance:
yes
Type of method:
continuous drop method
Type of particle tested:
agglomerate
Type of distribution:
volumetric distribution

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
liquid
Specific details on test material used for the study:
Test item: Esacure 3644
Appearance: Light yellow solid
Test item storage: At room temperature protected from light
Expiry date: 06 July 2019
Relative density: 1.14 (determined by Charles River Laboratories)

Results and discussion

Particle sizeopen allclose all
Key result
Percentile:
D10
Mean:
19.3 µm
St. dev.:
0.105
Key result
Percentile:
D50
Mean:
75.2 µm
St. dev.:
0.64
Key result
Percentile:
D90
Mean:
222 µm
St. dev.:
6.57
Key result
Percentile:
other: MMAD (mass median aerodynamic diameter)
Mean:
80.3 µm
St. dev.:
0.611
Key result
Percentile:
other: Volume of sample < 10.00 µm
Mean:
0.65 other: %
Remarks on result:
other: 0.65 % by volume of sample was seen to be < 10.00 µm

Any other information on results incl. tables

Solubility Test for Particle Size Analysis

Preliminary Solubility And Dispersability For Particle Size Analysis

The test item was well dispersed in both solvents tested. For the full solubility and dispersability test both solvents were selected.

Solubility And Dispersability Test For Particle Size Analysis

Dispersant used: 2-Propanol & Silicone Oil

The test item proved to be insoluble and well dispersed in both solvents. Both solvents were therefore trialled as the dispersant.

During the method development phase of the analysis trials were conducted using the small volume (wet) module only. The trials were conducted using 2-propanol and 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 : Small volume module

Dispersant : Silicone oil

Dispersion speed : 1800 rpm

Refractive index (sample) : 0.000 n

Absorption : 0.000 AU

Analysis Model : General Purpose

Using the identified parameters, the particle size was analysed over the range 0.01 µm to 3500 µm. The results of the formal analysis are presented in Table 10:1. In addition, a graph of volume (%) versus Particle Diameter (µm), and full particle size distribution, is provided in Graph 10.A (Average of 5 runs).

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.

Applicant's summary and conclusion

Conclusions:
In conclusion, 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:

Particle Size Distribution test was performed under GLP conditions on the test substance.  In conclusion, 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.