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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:
07 June 2017 to 18 July 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2017
Report Date:
2017

Materials and methods

Test guidelineopen allclose all
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Deviations:
not specified
Qualifier:
according to
Guideline:
other: CIPAC MT 187
Deviations:
not specified
GLP compliance:
yes (incl. certificate)
Remarks:
The Department of Health of the Government of the United Kingdom
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution

Test material

Reference
Name:
Unnamed
Type:
Constituent

Results and discussion

Mass median aerodynamic diameter:
189.093 µm
Particle sizeopen allclose all
Percentile:
D10
Mean:
46.848 µm
St. dev.:
0.739
Percentile:
D50
Mean:
171.197 µm
St. dev.:
1.866
Percentile:
D90
Mean:
401.832 µm
St. dev.:
4.009

Any other information on results incl. tables

Optical Microscope Conclusions

Standard visual observation:

Sample observed to be a polydispersed, off-white powder with clusters.

Observation using 3.2 objective lens:

The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 µm and the largest individual size was approximately 432 µm.

Observation using 40 objective lens:

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

 

Laser Diffraction Conclusions

Summary of Results:

The results of the laser diffraction test conducted to determine the particle size of

4,4'-[isopropylidenebis(4,1-phenyleneoxy)]dianiline are summarised in table below. The analysis was conducted using the dry powder module (DPM).

Particle Size Analysis using dry powder module (DPM)

Average (µm)

Volume weighted mean

201.074

Median

171.197

Mode

211.034

MMAD(massmedianaerodynamicdiameter)

189.093

d10-10% of materialis

46.848

d50-50% of materialis

171.197

d90-90% of materialis

401.832

volume of sample <10.00 µm

0.96%

Full Test Results:

 

RUN1

RUN2

RUN3

RUN4

RUN5

Average**

Volume weighted mean

200.031

203.357

203.809

198.817

199.354

201.074

Median

170.203

173.107

173.729

168.944

170.059

171.197

Mode

209.337

212.029

214.059

207.298

212.405

211.034

MMAD*

187.996

191.203

191.890

186.605

187.837

189.093

d10-10% of materialis

46.286

47.691

47.799

46.504

46.023

46.848

d50-50% of materialis

170.203

173.107

173.729

168.944

170.059

171.197

d90-90% of materialis

400.137

406.276

406.896

397.603

398.060

401.832

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.

0.96 % by volume of sample was seen to be < 10.00 µm.

 

Standard Deviation Results:

RunNo.

1

2

3

4

5

STDVP

%STDVP

d10-10% of materialis

46.286

47.691

47.799

46.504

46.023

0.739

1.6

d50-50% of materialis

170.203

173.107

173.729

168.944

170.059

1.866

1.1

d90-90% of materialis

400.137

406.276

406.896

397.603

398.060

4.009

1.0

d15.78-15.78% of materialis

66.058

67.784

67.827

66.004

65.639

0.945

1.4

GSD

2.577

2.554

2.561

2.560

2.591

0.013

0.5

MMAD

187.996

191.203

191.890

186.605

187.837

2.061

1.1

GSD = Geometric standard deviation of the lognormal particle size distribution (calculated from d50/d15.78)

STDVP = standard deviation of the population

% STDVP = percentage standard deviation of the population

 

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.

Applicant's summary and conclusion