Benzenesulfonic acid, C14-24-alkyl derivatives, magnesium salts, overbased

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:

8 September 2017 to 22 November 2017

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

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of distribution:

volumetric distribution

Key result

Percentile:

D10

Mean:

117.782 µm

St. dev.:

2.307

Key result

Percentile:

D50

Mean:

565.432 µm

St. dev.:

6.223

Key result

Percentile:

D90

Mean:

1 241.385 µm

St. dev.:

5.055

VISUAL OBSERVATIONS

- Standard visual observation: Sample observed to be a polydispersed, brown solid with clusters.

- Observation using a 3.2 objective lens: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 19 µm and the largest individual size approximately 2640 µm.

- Observation using a 40 objective lens: The sample was observed to be made up of single crystalline particles.

 

MANUAL SIEVE ANALYSIS

- 94.1% of the test material by weight was < 2000 µm

- Results can be seen in Table 1.

Table 1: Results of the Manual Sieve Analysis

Sieve Size (µm)	Sieve Weight (g)	Sieve + Powder Weight (g)	Powder Weight (g)	% by Weight
< 2000	352.4	446.5	94.1	94.1
> 2000	326	331.9	5.9	5.9
TOTALS			100.0	100.0

 

LASER DIFFRACTION

- Results can be seen in Tables 2 and 3.

0.28 % by volume of the 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 test guideline.

 

Table 2: Laser Diffraction Full Test Results

	Run 1	Run 2	Run 3	Run 4	Run 5	Average*
Volume Weighted Mean	625.425	631.510	639.382	625.533	628.887	630.148
Median	560.036	567.089	576.622	559.745	563.377	565.432
Mode	785.801	756.215	760.814	759.382	758.984	758.847
d10: 10 % of the material is <	116.625	118.923	121.753	115.048	116.914	117.782
d50: 50 % of the material is <	560.036	567.089	576.622	559.745	563.377	565.432
d90: 90 % of the material is <	1235.891	1240.976	1250.320	1237.303	1242.339	1241.385

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

 All results are in µm.

Table 3: Laser Diffraction Standard Deviation Results

	Run 1	Run 2	Run 3	Run 4	Run 5	STDVP	%STDVP
d10: 10 % of the material is <	116.625	118.923	121.753	115.048	116.914	2.307	2.0
d50: 50 % of the material is <	560.036	567.089	576.622	559.745	563.377	6.223	1.1
d90: 90 % of the material is <	1235.891	1240.976	1250.320	1237.303	1242.339	5.055	0.4
d15.78: 15.78 % of the material is <	176.749	182.953	188.303	176.357	178.236	4.544	2.5
GSD	3.169	3.100	3.062	3.174	3.161	0.0440	1.4

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 this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.

Executive summary:

The particle size distribution of the test material was investigated in accordance with the standardised guideline ISO 13320, under GLP conditions.

The particle size was investigated using microscope analysis, manual sieving and laser diffraction.

0.28% by volume of the sample was seen to be < 10.00 µm. The coefficient of variation for d50 was 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 test guideline.

Under the conditions of this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.

Description of key information

Under the conditions of this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.

Additional information

The particle size distribution of the test material was investigated in accordance with the standardised guideline ISO 13320, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The particle size was investigated using microscope analysis, manual sieving and laser diffraction.

0.28% by volume of the sample was seen to be < 10.00 µm. The coefficient of variation for d50 was 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 test guideline.

Under the conditions of this study the d10, d50 and d90 of the test material were 117.782, 565.432 and 1241.385 µm, respectively.