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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:
2015
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Reference:
Composition 1
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
Taking into consideration OECD guideline 110
Deviations:
no
Qualifier:
according to
Guideline:
other: CIPAC MT 187
Version / remarks:
Will take into consideration OECD guideline 110
Deviations:
no
GLP compliance:
yes
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Test material information:
Composition 1
Mass median aerodynamic diameter:
ca. 8.528 µm
Geometric standard deviation:
>= 3.633 - <= 3.757
Remarks on result:
other:
Remarks:
Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.
Percentile:
D10
Mean:
ca. 1.217 µm
St. dev.:
0.041
Percentile:
D50
Mean:
ca. 7.334 µm
St. dev.:
0.094
Percentile:
D90
Mean:
ca. 16.733 µm
St. dev.:
0.191
No.:
#1
Size:
10 µm
Distribution:
66.29 %

Table 4.1 : Full Test results

   RUN 1  RUN 2  RUN 3  RUN 4  RUN 5  Average
 d10 1.209 1.208 1.195 1.122 1.248  8.315
 Median (d.50)  7.245  7.258  7.278  7.422  7.474  7.334
 Mode (µm)  9.275  9.375  9.453  9.679  9.714  9.495
 MMAD  8.424  8.440  8.462  8.630  8.690  8.528
 10% of material is <  1.209  1.208  1.195  1.122  1.248  1.217
50% of material is <   7.245  7.258  7.278  7.422  7.474  7.334
 90% of material is <  16.415  16.662  16.748  16.988  16.840  16.733

All results are in µm. MMAD: Mass Median Aerodynamic Diametre. Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

66.29% by volume of sample was seen to be < 10.00 µm.

Table 4.2 : Standard deviation results

   RUN 1  RUN 2  RUN 3  RUN 4  RUN 5  STDVP  % STDVP
 d.10 1.209 1.208  1.195  1.122  1.248  0.041  3.4
 d.50  7.245  7.258  7.278  7.422  7.474  0.094 1.3
d.90  16.415  16.662  16.748  16.988  16.840  0.191  1.1
 d.15.78  1.994  1.972  1.937  1.995  2.038  0.033  1.7
GSD  3.633  3.681  3.757  3.720  3.667  0.043  1.2
MMAD  8.42  8.44  8.46  8.63  8.69  0.11  1.3

GSD: Geometric standard deviation, STDVP: Standard deviation of the population, % STDVP: Percentage standard deviation of the population

Conclusions:
66.29 % by volume of sample was seen to be < 10.00 µm averaged over 5 runs.
Average Mass Median Aerodynamic Diameter (MMAD) was 8.528 µm.
Executive summary:

The sample 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 final sample is then analysed using the Malvern Mastersizer 2000 Laser Diffraction Analyser. It is normal practice to complete 5 runs to ensure repeatability of results.

During the method development phase of the analysis trials were conducted using the dry powder module (DPM). The results of these trials indicated that the most appropriate test and material parameters to obtain the optimum measurements were:

  • Module : DPM
  • Dispersant : Air
  • Dispersion pressure : 1.0 barg
  • Refractive index (sample) : 0.000 n
  • Absorption : 0 AU
  • Analysis Model : General Purpose (Normal)

66.29 % by volume of sample was seen to be < 10.00 µm averaged over 5 runs.

Average Mass Median Aerodynamic Diameter (MMAD) was 8.528 µm.

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 are within the acceptable limits as per the ISO 13320-1 test standard.

Description of key information

66.29 % by volume of sample was seen to be < 10.00 µm averaged over 5 runs. Average Mass Median Aerodynamic Diameter (MMAD) was 8.528 µm.

Additional information

The sample 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 final sample is then analysed using the Malvern Mastersizer 2000 Laser Diffraction Analyser. It is normal practice to complete 5 runs to ensure repeatability of results.

During the method development phase of the analysis trials were conducted using the dry powder module (DPM). The results of these trials indicated that the most appropriate test and material parameters to obtain the optimum measurements were:

  • Module : DPM
  • Dispersant : Air
  • Dispersion pressure : 1.0 barg
  • Refractive index (sample) : 0.000 n
  • Absorption : 0 AU
  • Analysis Model : General Purpose (Normal)

66.29 % by volume of sample was seen to be < 10.00 µm averaged over 5 runs.

Average Mass Median Aerodynamic Diameter (MMAD) was 8.528 µm.

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 are within the acceptable limits as per the ISO 13320-1 test standard.