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Physical & Chemical properties

Particle size distribution (Granulometry)

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Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
22/07/2012-01/08/2012
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Guideline:
other: ISO 13320:2009 and CIPAC MT 187
GLP compliance:
yes (incl. QA statement)
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Mass median aerodynamic diameter:
>= 327.38 - <= 345.769 µm
Geometric standard deviation:
>= 1.845 - <= 1.867
Percentile:
D50
Remarks on result:
not measured/tested

Standard visual observation

Sample observed to be a coarse, free flowing, white powder.

Observation at 100 x magnification

The particles appeared to be irregular shape. The smallest individual particle size was approximately 16 μm and the largest individual size was approximately 1440 μm.

Observation at 400 x magnification

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

LASER DIFFRACTION PARTICLE SIZE ANALYSIS

Table 1 : Full Test Results

 

 

 

RUN 1

RUN 2

RUN 3

RUN 4

RUN 5

**Average

Volume weighted Mean

333.191

355.433

347.543

347.979

353.630

347.555

Median (d.50)

286.033

302.099

296.555

296.020

302.008

296.449

Mode (μm)

289.311

302.114

298.840

298.022

304.734

298.492

*MMAD

327.380

345.769

339.423

338.810

345.663

339.301

10 % of material is <

130.341

136.709

134.278

133.062

136.259

134.072

50 % of material is <

286.033

302.099

296.555

296.020

302.008

296.449

90 % of material is <

606.719

654.299

636.252

640.084

647.881

637.121

 

All results are in μm

*Mass Median Aerodynamic Diameter

**Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

0.0 % by volume of sample was seen to be < 10.00 μm.

 

Table 2 : Standard Deviation results

 

Run No.

1

2

3

4

5

STDVP

% STDVP

d10

130.341

136.709

134.278

133.062

136.259

2.31

1.72

d50

286.033

302.099

296.555

296.020

302.008

5.86

1.97

d90

606.719

654.299

636.252

640.084

647.881

16.40

2.57

d15.78

155.024

162.636

159.839

158.595

162.377

2.79

1.75

*GSD

1.845

1.858

1.855

1.867

1.860

0.01

0.38

MMAD

327.380

345.769

339.423

338.810

345.663

6.70

1.97

 

*GSD = Geometric standard deviation

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.

Conclusions:
The average Mass Median Aerodynamic Diameter (MMAD) of the test material was 339.301 μm.
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
weight of evidence
Study period:
19/07/2012 - 01/08/2012
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Guideline:
other: ISO 13320:2009 and CIPAC MT 187
GLP compliance:
yes (incl. QA statement)
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Mass median aerodynamic diameter:
>= 545.032 - <= 597.083 µm
Geometric standard deviation:
>= 1.891 - <= 1.948
Percentile:
D50
Remarks on result:
not measured/tested

Standard visual observation

Sample observed to be a coarse, free flowing, white powder.

Observation at 100 x magnification

The particles appeared to be irregular shape. The smallest individual particle size was approximately 16 μm and the largest individual size was approximately 1456 μm.

Observation at 400 x magnification

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

LASER DIFFRACTION PARTICLE SIZE ANALYSIS

Table 1 : Full Test Results

 

 

 

RUN 1

RUN 2

RUN 3

RUN 4

RUN 5

**Average

Volume weighted Mean

574.341

549.815

581.982

587.755

602.399

579.259

Median (d.50)

495.949

476.196

501.543

507.103

521.674

500.103

Mode (μm)

508.045

489.839

525.669

531.551

550.904

520.127

*MMAD

567.639

545.032

574.042

580.405

597.083

572.394

10 % of material is <

219.263

210.744

213.073

216.370

224.007

216.551

50 % of material is <

495.949

476.196

501.543

507.103

521.674

500.103

90 % of material is <

1058.101

1009.712

1081.177

1089.773

1111.359

1070.499

 

All results are in μm

*Mass Median Aerodynamic Diameter

**Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

0.0 % by volume of sample was seen to be < 10.00 μm.

 

Table 2 : Standard Deviation results

 

Run No.

1

2

3

4

5

STDVP

% STDVP

d10

219.263

210.744

213.073

216.370

224.007

4.66

2.15

d50

495.949

476.196

501.543

507.103

521.674

14.86

2.97

d90

1058.101

1009.712

1081.177

1089.773

1111.359

34.65

3.24

d15.78

261.735

251.772

257.463

261.016

269.425

5.77

2.22

*GSD

1.895

1.891

1.948

1.943

1.936

0.02

1.27

MMAD

567.639

545.032

574.042

580.405

597.083

17.01

2.97

 

*GSD = Geometric standard deviation

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.

Conclusions:
The average Mass Median Aerodynamic Diameter (MMAD) of the test material was 572.394 μm.

Description of key information

The particle size distribution of two commercial grades of the substance were measured. The average Mass Median Aerodynamic Diameter (MMAD) of the coarse grade was 339.301 μm, whilst the average MMAD of the flake grade was 572.394 μm.

Additional information

The particle size distribution of two commercial grades of the substance were measured in accordance with ISO 13320:2009 and CIPAC MT 187 using a Malvern Mastersizer 2000 Laser Diffraction Particle Size Analyzer. The average Mass Median Aerodynamic Diameter (MMAD) of the coarse grade was 339.301 μm, whilst the average MMAD of the flake grade was 572.394 μm.