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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:
From 21 December 2016 to 12 January 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Qualifier:
according to
Guideline:
other: CIPAC MT 187
Principles of method if other than guideline:
Principle of test:
The sample is initially observed using a visual microscope to determine whether sieving of the material is requiered.
The laser diffraction method which determine the mass median aerodynamic diameter (MMAD) needs the generation of a representative test atmospheres using suitable generation equipment and correct sampling techniques.
A method development for the particle size analysis on the material is then undertaken to obtain the correct parameters for the formal analysis. The method development is employed to identify the most appropriate optical properties for the material, the correct dispersant, dispersion pressures and sample compatibility. Once these parameters are obtained the final sample is then analysed using the Malvern Mastersizer 2000 Laser Diffraction Analyser.
This procedure allows the operator to obtain a better understanding of the particle characterisation of the material. This includes, but is not limited to, sample clusters and agglomerations which may provide false values in the formal particle size analysis. In these situations, where the operator can assess how easily these clusters or aggomerations are dispersed, ultrasonics may be employed. Owing to the extremely small quantities of material used in this analysis it should be noted that discrepancies can arise between the lower and upper limits of the particle size and the actual value obtained in the formal particle size analysis.

GLP compliance:
yes (incl. certificate)
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Specific details on test material used for the study:
SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material: A017 / Batch Number : 7215604684
- Expiration date of the lot/batch: NA
- Purity test date: 09 september 2016
- Purity : 99.1% ±0.1%
- Re-analysis date : NA
- Description : Cream / beige to grey flakes
Relative Density : 1.28 g/cm3 (data taken from SDS)

STABILITY AND STORAGE CONDITIONS OF TEST MATERIAL
- Storage condition of test material: NA
- Stability under test conditions: NA
- Solubility and stability of the test substance in the solvent/vehicle: NA
- Reactivity of the test substance with the solvent/vehicle of the cell culture medium: NA

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
- Treatment of test material prior to testing: no, sample is tested as received.
- Preliminary purification step (if any): no
- Final dilution of a dissolved solid, stock liquid or gel: no
- Final preparation of a solid: no
Mass median aerodynamic diameter:
>= 264.981 - <= 275.922 µm
Geometric standard deviation:
>= 2.041 - <= 2.14
Remarks on result:
other: The average Mass Median Aerodynamic diameter is 268.252 µm. Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.
Key result
Percentile:
D10
Mean:
ca. 92.293 µm
St. dev.:
2.063
Key result
Percentile:
D50
Mean:
ca. 237.103 µm
St. dev.:
3.591
Key result
Percentile:
D90
Mean:
ca. 509.337 µm
St. dev.:
3.69
No.:
#1
Size:
<= 10 µm
Distribution:
ca. 1.05 %
No.:
#2
Size:
<= 50.238 µm
Distribution:
ca. 1.79 %
No.:
#3
Size:
<= 70.963 µm
Distribution:
ca. 4.85 %
No.:
#4
Size:
<= 100 µm
Distribution:
ca. 12.19 %
No.:
#5
Size:
<= 178.25 µm
Distribution:
ca. 34.68 %
No.:
#6
Size:
<= 250 µm
Distribution:
ca. 53.05 %
No.:
#7
Size:
<= 399.052 µm
Distribution:
ca. 79.44 %
No.:
#8
Size:
<= 632.456 µm
Distribution:
ca. 96.2 %
No.:
#9
Size:
<= 900 µm
Distribution:
ca. 99.9 %
No.:
#10
Size:
<= 1 700 µm
Distribution:
ca. 100 %

Preliminary standard visual observation :

Sample observed to be coarse, medium to fine cream /beige to grey flakes with clusters and some agglomerations.

Observation at 100 x magnification :

The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 µm and the largest individual siz was approximately 563 µm.

Observation at 400 x magnification :

The sample was observed to be made up of single crystalline particles and agglomerated particles.

method development phase of the analysis trials :

The results of the SVM trials indicates that the most appropriate test and material parameters were :

Module : Small Volume Module

Dispersant : Silicone Oil

Dispersion speed : 2300 rpm

Refractive Index (sample) : 0.000 n

Absorption : 0.0 AU

Analysis Model : General Purpose (Normal)

The results of the formal analysis of the particle size distribution (volume (%) versus particle diameter) are presented above.

Conclusions:
The average mass median aerodynamic diameter of the test item is 268.252 µm.


Executive summary:

The particle size distribution was determined according to the ISO 13320 (Particle size analysis - Laser diffraction methods) and the GLP.

The results of the particle Diameter are presented below :

 Particle size analysis using small volume (wet) module (SVM)

 Average (µmeter)
 Volume weighted mean  272.504
 Median (D.50)  237.103
 Mode  278..639
 MMAD (Mass Median Aerodynamic Diameter)  268.252

 10% of material is <

 92.293
 50% of material is <  237.103
 90% of material is <  509.337
 volume of sample <10.00 µmeter  1.05%

The Coefficient of variations for D50 is less than 3%; D10 and D90 are less than 5%.

Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the ISO 13320-1 test standard.

Description of key information

The average mass median aerodynamic diameter of the test item is 268.252 µm.

Additional information

The particle size distribution was determined according to the ISO 13320 (Particle size analysis - Laser diffraction methods) and the GLP.

The results of the particle Diameter :

 Particle size analysis using small volume (wet) module (SVM)

 Average (µm)

 Volume weighted mean

 272.504

 Median (D.50)

 237.103

 Mode

 278..639

 MMAD (Mass Median Aerodynamic Diameter)

 268.252

 10% of material is <

 92.293

 50% of material is <

 237.103

 90% of material is <

 509.337

volume of sample <10.00 µm

 1.05%

The Coefficient of variations for D50 is less than 3%; D10 and D90 are less than 5%.

Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the ISO 13320-1 test standard.