Tungsten Oxide (WO3), caesium and tin-doped

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:

07 December 2017 to 04 January 2018

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Version / remarks:

2009

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: IPAC MT 187 “Particle Size Analysis by Laser Diffraction”

Version / remarks:

Handbook K, 2007.

Deviations:

no

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:

45.396 µm

Geometric standard deviation:

0.007

Key result

Percentile:

D10

Mean:

3.27 µm

St. dev.:

0.025

Key result

Percentile:

D50

Mean:

17.486 µm

St. dev.:

0.213

Key result

Percentile:

D90

Mean:

47.431 µm

St. dev.:

1.059

- During the method development phase of the analysis trials were conducted using the small volume (wet) module (SVM) only. The SVM trials were conducted using water 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: Water

Dispersion speed: 1500 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. The results of the formal analysis are presented in Table 1.

- 30.79 % by volume of sample was seen to be < 10.00 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.

Table 1: Full Test Results

	Run 1	Run 2	Run 3	Run 4	Run 5	Average **
Volume weighted mean	23.243	23.401	23.227	22.013	22.473	22.872
Median	17.671	17.724	17.570	17.272	17.199	17.486
Mode	23.629	23.574	23.580	23.636	23.281	23.539
MMAD	45.877	46.015	45.615	44.839	44.652	45.396
d10- 10 % of material is <	3.290	3.300	3.279	3.245	3.237	3.270
d50- 50 % of material is <	17.671	17.724	17.570	17.272	17.199	17.486
d90- 90 % of material is <	49.171	49.603	48.673	46.795	47.431	48.313

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.

 

Table 2: Standard Deviation Results

	Run 1	Run 2	Run 3	Run 4	Run 5	STDVP	% STDVP
d10 - 10 % of material is <	3.290	3.300	3.279	3.245	3.237	0.025	0.8
d50 - 50 % of material is <	17.671	17.724	17.570	17.272	17.199	0.213	1.2
d90 - 90 % of material is <	49.171	49.603	48.673	46.795	47.431	1.059	2.2
d15.78 - 15.78 % of material is <	4.922	4.931	4.888	4.825	4.808	0.050	1.0
GSD	3.590	3.594	3.595	3.580	3.577	0.007	0.2
MMAD	45.877	46.015	45.615	44.839	44.652	0.552	1.2

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

Conclusions:

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.

Executive summary:

The particle size distribution of the test material was determined in accordance with the standardised guidelines ISO 13320:2009 and CIPAC MT 187 under GLP conditions using particle size apparatus based on laser diffraction.

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.

Description of key information

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.

Additional information

The particle size distribution of the test material was determined in accordance with the standardised guidelines ISO 13320:2009 and CIPAC MT 187 under GLP conditions using particle size apparatus based on laser diffraction. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Under the conditions of the study, the test material was determined to have d10, d50 and d90 values of 3.270, 17.486 and 48.313 μm, respectively. 30.79 % of the sample had a volume < 10.00 µm.