α,α'-dichloro-p-xylene

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

22/03/2018 to 11/04/2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Reason / purpose for cross-reference:

reference to same study

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Version / remarks:

ISO 13320:2009 “Particle Size Analysis – Laser Diffraction Methods”, 2009

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Version / remarks:

CIPAC MT 187 “Particle Size Analysis by Laser Diffraction”, Handbook K, 2007.

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of particle tested:

aggregate

Type of distribution:

mass based distribution

Specific details on test material used for the study:

No further details specified.

Mass median aerodynamic diameter:

496.146 µm

Geometric standard deviation:

> 1.47 - < 1.559

Key result

Percentile:

D10

Mean:

236.133 µm

St. dev.:

5.539

Key result

Percentile:

D50

Mean:

395.654 µm

St. dev.:

7.782

Key result

Percentile:

D90

Mean:

653.894 µm

St. dev.:

30.812

Solubility and Dispersability Test for Particle Size Analysis

Table of solubility results

 

Dispersant used: Sunflower oil

	Series 1			Series 2
Time elapsed	1 (1.5 mg)	2 (1.5 mg)	3 (1.5 mg)	1 (5.1 mg)	2 (5.0 mg)	3 (5.0 mg)
10 seconds	Well dispersed			Well dispersed
30 minutes	Well dispersed			Well dispersed
60 minutes	Well dispersed			Well dispersed
90 minutes	Well dispersed			Well dispersed
120 minutes	Well dispersed			Well dispersed

 

Dispersant used: Silicone oil

	Series 1			Series 2
Time elapsed	1 (1.5 mg)	2 (1.5 mg)	3 (1.5 mg)	1 (4.9 mg)	2 (5.0 mg)	3 (5.0 mg)
10 seconds	Well dispersed			Well dispersed
30 minutes	Well dispersed			Well dispersed
60 minutes	Well dispersed			Well dispersed
90 minutes	Well dispersed			Well dispersed
120 minutes	Well dispersed			Well dispersed

 

Comments: Sunflower oil was initially selected for the test but showed poor reproducibility. The sample was well dispersed in silicone oil. Therefore, silicone oil was used as the dispersant.

 

Laser Diffraction Particle Size Analysis

Test Results

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: 2600 rpm

Refractive index (sample): 0.000 n

Absorption: 0 AU

Analysis Model: General Purpose (Normal)

 

Using the identified parameters, the particle size was analysed over the range 0.02 μm to 2000 μm.

 

Full Test Results

	RUN 1	RUN 2	RUN 3	RUN 4	RUN 5	Average**
Volume weighted mean	421.122	421.130	434.047	405.720	440.820	424.568
Median	396.058	395.986	405.836	382.148	399.767	395.654
Mode	399.495	406.593	408.362	386.131	399.194	399.324
MMAD*	469.626	469.54	481.219	453.132	474.023	469.146
d10 (10% of material is <)	242.044	232.257	243.006	235.089	228.705	236.133
d50 (50% of material is <)	396.058	395.986	405.836	382.148	399.767	395.654
d90 (90% of material is <)	639.242	650.062	669.361	612.078	704.251	653.894

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.

0.00% by volume of sample was seen to be <10.00 µm.

 

Standard Deviation results

Run No.	1	2	3	4	5	STDVP	% STDVP
d10 (10% of material is <)	242.044	232.257	243.006	235.089	228.705	5.539	2.3
d50 (50% of material is <)	396.058	395.986	405.836	382.148	399.767	7.782	2.0
d90 (90% of material is <)	639.242	650.062	669.361	612.078	704.251	30.812	4.7
d15.78	268.077	259.523	270.268	259.922	256.437	5.350	2.0
GSD	1.477	1.526	1.502	1.470	1.559	0.033	2.2
MMAD	469.626	469.540	481.219	453.132	474.023	9.227	2.0

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

Executive summary:

To characterise the particle size distribution of the powder. The analysis is conducted initially using a visual microscope and is then undertaken more formally using a Laser Diffraction Particle Size Analyser.

 

Summary of Results

Particle Size Analysis using small volume (wet) module (SVM)	Average (µm)
Volume weighted mean	424.568
Median (d.50)	395.654
Mode	399.324
MMAD (Mass Median Aerodynamic Diameter)	469.146
10% of material is <	236.133
50% of material is <	395.654
90% of material is <	653.894
By volume of sample was seen to be <10.00 µm	0.00%

 

Description of key information

To characterise the particle size distribution of the powder. The analysis is conducted initially using a visual microscope and is then undertaken more formally using a Laser Diffraction Particle Size Analyser.

 

Summary of Results

Particle Size Analysis using small volume (wet) module (SVM)	Average (µm)
Volume weighted mean	424.568
Median (d.50)	395.654
Mode	399.324
MMAD (Mass Median Aerodynamic Diameter)	469.146
10% of material is <	236.133
50% of material is <	395.654
90% of material is <	653.894
By volume of sample was seen to be <10.00 µm	0.00%