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EC number: 686-016-4 | CAS number: 881302-73-4
Particle size distribution (Granulometry)
Administrative data
- Endpoint:
- particle size distribution (granulometry)
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
Data source
Reference
- Reference Type:
- study report
- Title:
- Unnamed
- Year:
- 2 020
- Report date:
- 2020
Materials and methods
Test guideline
- Qualifier:
- according to guideline
- Guideline:
- ISO 13320 (Particle size analysis - Laser diffraction methods)
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Type of method:
- Laser scattering/diffraction
- Type of distribution:
- volumetric distribution
Test material
- Reference substance name:
- 5-(dihydroxyboranyl)benzene-1,3-dicarboxylic acid
- Cas Number:
- 881302-73-4
- Molecular formula:
- C8H7BO6
- IUPAC Name:
- 5-(dihydroxyboranyl)benzene-1,3-dicarboxylic acid
- Test material form:
- solid
Constituent 1
Results and discussion
- Mass median aerodynamic diameter:
- ca. 50.112 µm
- Geometric standard deviation:
- ca. 2.338
Particle sizeopen allclose all
- Key result
- Percentile:
- D90
- Mean:
- ca. 96.1 µm
- St. dev.:
- 1.68
- Key result
- Percentile:
- D50
- Mean:
- ca. 39.3 µm
- St. dev.:
- 0.269
- Key result
- Percentile:
- D10
- Mean:
- ca. 16.3 µm
- St. dev.:
- 0.068
Particle size distribution at different passagesopen allclose all
- No.:
- #5
- Size:
- ca. 39.3 µm
- Distribution:
- ca. 50 %
- No.:
- #4
- Size:
- ca. 38.8 µm
- Distribution:
- ca. 50 %
- No.:
- #3
- Size:
- ca. 39.4 µm
- Distribution:
- ca. 50 %
- No.:
- #2
- Size:
- ca. 39.5 µm
- Distribution:
- ca. 50 %
- No.:
- #1
- Size:
- ca. 39.3 µm
- Distribution:
- ca. 50 %
Any other information on results incl. tables
During the method development phase of the analysis trials were
conducted using 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 : 1500 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).
|
Run 1 |
Run 2 |
Run 3 |
Run 4 |
Run 5 |
Average |
STDVP % |
STDVP |
VWM |
49.2 |
48.5 |
49.9 |
48.5 |
49.8 |
49.2 |
N/A |
N/A |
Mode |
38.1 |
38.5 |
37.8 |
37.6 |
38.0 |
38.0 |
N/A |
N/A |
d10 |
16.3 |
16.3 |
16.4 |
16.2 |
16.4 |
16.3 |
0.0679 |
0.416 |
d50 (Median) |
39.3 |
39.5 |
39.4 |
38.8 |
39.3 |
39.3 |
0.269 |
0.685 |
d90 |
96.7 |
94.1 |
97.8 |
94.6 |
97.5 |
96.1 |
1.68 |
1.74 |
MMAD |
50.160 |
50.367 |
50.319 |
49.519 |
50.207 |
50.112 |
0.307 |
0.6 |
GSD |
2.349 |
2.326 |
2.344 |
2.327 |
2.345 |
2.338 |
0.010 |
0.4 |
All particle size results are in μm
4.82 % by volume of sample was seen to be < 10.00 μm
Definitions
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
MMAD : mass median aerodynamic diameter
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
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:
- Average STDVP % STDVP
VWM 49.2 N/A N/A
Mode 38.0 N/A N/A
d10 16.3 0.0679 0.416
d50 (Median) 39.3 0.269 0.685
d90 96.1 1.68 1.74
MMAD 50.112 0.307 0.6
GSD 2.338 0.010 0.4 - Executive summary:
The test is conducted to determine the particle size distribution of
3,5-Dicarboxyphenylboronic acid. The test item is initially observed to determine whether sieving of the material is required. 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 test item is then analysed using the Malvern Mastersizer 3000 Laser Diffraction Analyser. It is normal practice to complete 5 runs to ensure repeatability of results. The test is conducted in accordance with ISO 13320:2009 “Particle Size Analysis – Laser Diffraction Methods”, 2009 and CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”, Handbook K, 2007.During the method development phase of the analysis trials were conducted using 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 : 1500 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 the following table:Average
STDVP %
STDVP
VWM
49.2
N/A
N/A
Mode
38.0
N/A
N/A
d10
16.3
0.0679
0.416
d50 (Median)
39.3
0.269
0.685
d90
96.1
1.68
1.74
MMAD
50.112
0.307
0.6
GSD
2.338
0.010
0.4
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