Reaction product of salicylaldehyde and formaldehyde and phenol

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:

08 November 2018 to 22 November 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: CIPAC MT 187 “Particle Size Analysis by Laser Diffraction” Handbook K.

Version / remarks:

2007

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of particle tested:

other: sieved fraction (< 3,500 µm)

Type of distribution:

volumetric distribution

Mass median aerodynamic diameter:

890 µm

Geometric standard deviation:

2.428

Percentile:

D10

Mean:

154 µm

St. dev.:

1.52

Key result

Percentile:

D50

Mean:

791 µm

St. dev.:

5.07

Percentile:

D90

Mean:

1 350 µm

St. dev.:

17.1

No.:

#1

Size:

< 10 µm

Distribution:

0.09 %

Optical Microscope Analysis

- Standard visual observation: Test material observed to be large lumps/resin.

- Observation at 100 x magnification: Due to nature of the sample it was not possible to achieve a representative portion of the sample and some of the larger particles were not on the microscope slide.

- Observation at 400 x magnification: The test material was observed to be made up of agglomerated particles.

 

Manual Sieve Analysis

15.8 % by weight < 3,500 μm

 

Laser Diffraction Particle Size Analysis

As received, the sample consisted mostly of very large lumps, but with some finer material. The sample was sieved prior to testing to remove the > 3.5 mm fraction. Due to the small amount of sample that was < 3.5 mm in size and the fact that the sample was coloured and stained easily, it was decided that the SVM (small volume (wet) module) was most appropriate to use. Testing was performed using SVM with silicone oil as the dispersant at 3,000 rpm. The distribution graph obtained from this did not show particles above 2,100 μm even though there was a large number of particles between this value and 3,500 μm. This was due to the larger particles sinking quickly in the silicone oil and so not being circulated.

Blockages of the tubing were also caused by some of the larger particles. After discussions with the client and study director, testing was stopped at this point and results obtained reported. 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: 3,000 rpm

Refractive index (sample): 1.500 n

Absorption: 0.000 AU

Analysis Model: General Purpose

Using the identified parameters, the particle size was analysed over the range 0.01 μm to 3,500 μm.

 

	Run 1	Run 2	Run 3	Run 4	Run 5	Average	STDVP	% STDVP
VWM	810	803	793	792	801	800	N/A	N/A
Mode	894	889	883	884	891	888	N/A	N/A
D10	155	156	153	153	153	154	1.52	0.987
D50 (Median)	796	793	786	785	795	791	5.07	0.642
D90	1330	1360	1330	1340	1350	1350	17.1	1.26
MMAD	896	892	885	883	894	890	5.107	0.6
GSD	2.433	2.416	2.421	2.432	2.437	2.428	0.008	0.3

All particle size results are in μm

 

0.09 % by volume of sample was seen to be < 10.00 μm

 

Definitions

VWM: volume weighted mean

D10: 10 % of the test material is less than this particle size

D50: 50 % of the test material is less than this particle size

D90: 90 % of the test material is less than this particle size

GSD: geometric standard deviation of the lognormal particle size distribution

MMAD: Mass median aerodynamic diameter

Average: Calculated from the entirety of the data captured in each run and not a simple arithmetic mean

STDVP: Standard deviation of the population

% STDVP: Percentage standard deviation of the population

The 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 is within the acceptable limits as per the ISO 13320-1 test standard.

Conclusions:

Under the conditions of the study the median (D50) particle size of the test material was 791 µm. 90 % of the test material was < 1350 µm. 10 % of the test material was < 154 µm. 0.09 % was < 10.0 µm. The MMAD was 890 µm.

Executive summary:

The particle size distribution of the test material was assessed according to ISO 13320 and CIPAC MT 187 using the laser diffraction method.

The analysis was conducted initially using a visual microscope and then undertaken more formally using a Laser Diffraction Particle Size Analyser. 

The test material was observed under 3 conditions: direct observation, under a microscope at 100 x magnification, under a microscope at 400 x magnification.

As received, the sample consisted mostly of very large lumps, but with some finer material. The sample was sieved prior to testing to remove the > 3.5 mm fraction. Due to the small amount of sample that was < 3.5 mm in size and the fact that the sample was coloured and stained easily, it was decided that the SVM (small volume (wet) module) was most appropriate to use. Testing was performed using SVM with silicone oil as the dispersant at 3,000 rpm. Five runs were completed to ensure repeatability of results.

The distribution graph obtained from this did not show particles above 2,100 μm even though there was a large number of particles between this value and 3,500 μm. This was due to the larger particles sinking quickly in the silicone oil and so not being circulated. Blockages of the tubing were also caused by some of the larger particles. Testing was stopped at this point.

Using the identified parameters, the particle size was analysed over the range 0.01 μm to 3,500 μm.

Under the conditions of the study the median (D50) particle size of the test material was 791 µm. 90 % of the test material was < 1350 µm. 10 % of the test material was < 154 µm. 0.09 % was < 10.0 µm. The MMAD was 890 µm. 

Description of key information

Under the conditions of the study the median (D50) particle size of the test material was 791 µm. 90 % of the test material was < 1350 µm. 10 % of the test material was < 154 µm. 0.09 % was < 10.0 µm. The MMAD was 890 µm. 

Additional information

The particle size distribution of the test material was assessed according to ISO 13320 and CIPAC MT 187 using the laser diffraction method. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The analysis was conducted initially using a visual microscope and then undertaken more formally using a Laser Diffraction Particle Size Analyser. 

The test material was observed under 3 conditions: direct observation, under a microscope at 100 x magnification, under a microscope at 400 x magnification.

As received, the sample consisted mostly of very large lumps, but with some finer material. The sample was sieved prior to testing to remove the > 3.5 mm fraction. Due to the small amount of sample that was < 3.5 mm in size and the fact that the sample was coloured and stained easily, it was decided that the SVM (small volume (wet) module) was most appropriate to use. Testing was performed using SVM with silicone oil as the dispersant at 3,000 rpm. Five runs were completed to ensure repeatability of results.

The distribution graph obtained from this did not show particles above 2,100 μm even though there was a large number of particles between this value and 3,500 μm. This was due to the larger particles sinking quickly in the silicone oil and so not being circulated. Blockages of the tubing were also caused by some of the larger particles. Testing was stopped at this point.

Using the identified parameters, the particle size was analysed over the range 0.01 μm to 3,500 μm.

Under the conditions of the study the median (D50) particle size of the test material was 791 µm. 90 % of the test material was < 1350 µm. 10 % of the test material was < 154 µm. 0.09 % was < 10.0 µm. The MMAD was 890 µm.