Condensation products of phenol and salicylaldehyde

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:

21 June 2016 to 23 June 2016

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)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Key result

Percentile:

D10

Mean:

26.22 µm

St. dev.:

0.366

Key result

Percentile:

D50

Mean:

197.131 µm

St. dev.:

2.287

Key result

Percentile:

D90

Mean:

534.74 µm

St. dev.:

5.764

Visual Observations

- Standard visual observation: Sample observed to be a coarse, gritty free flowing red to brown solid. Most of the sample

particles appear to be > 2 000 μm, therefore sieve analysis was employed.

- Observation at 100 x magnification: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 μm and the largest individual size was >2 000 μm.

- Observation at 400 x magnification: The sample was observed to be made up of single crystalline particles.

 

Manula Sieve Analysis

- 13.7 % of the test material by weight was < 2 000 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	241.6	295.8	54.2	13.7
>2000	325.8	667.4	341.6	86.3
TOTALS			395.8	100.0

 

Solubility Test

- The sample proved to be insoluble, and well dispersed in silicone oil. Therefore silicone oil was used as a dispersant for the analysis.

LASER DIFFRACTION

- Results can be seen in Tables 2 and 3.

4.58 % 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	245.696	248.554	252.004	243.708	247.208	247.434
Median (d.50)	199.867	198.637	198.288	195.050	193.856	197.131
Mode (μm)	298.621	293.195	290.881	292.856	285.551	292.154
*MMAD	223.904	222.526	222.136	218.508	217.171	220.84
10 % of material is <	26.698	26.469	26.339	25.915	25.700	26.220
50 % of material is <	199.867	198.637	198.288	195.050	193.856	197.131
90 % of material is <	530.283	540.910	542.311	527.894	532.738	534.740

* Mass Median Aerodynamic Diameter

**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	26.698	26.469	26.339	25.915	25.700	0.366	1.4
d50	199.867	198.637	198.288	195.050	193.856	2.287	1.2
d90	530.283	540.910	542.311	527.894	532.738	5.764	1.1
d15.78	47.201	46.737	46.520	45.798	45.330	0.670	1.4
GSD	4.234	4.250	4.262	4.259	4.277	0.014	0.3
MMAD	223.90	222.53	222.14	218.51	217.17	2.56	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 this study the d10, d50 and d90 of the test material were 26.220, 197.131 and 534.740 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.

4.58 % 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 26.220, 197.131 and 534.740 µm, respectively.

Description of key information

Under the conditions of this study the d10, d50 and d90 of the test material were 26.220, 197.131 and 534.740 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.

4.58 % 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 26.220, 197.131 and 534.740 µm, respectively.