N,N'-hexamethylenebis(cinnamylideneamine)

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:

December 16, 2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

test procedure in accordance with generally accepted scientific standards and described in sufficient detail

Qualifier:

according to guideline

Guideline:

other: ASTM B 822-92

GLP compliance:

no

Type of method:

Laser scattering/diffraction

Type of distribution:

volumetric distribution

Specific details on test material used for the study:

Instruments and Devices
-Particle Analyzer
Producer: Coulter
Model: LS200
Serial Number: AB26386
Equipped with:
-sample cell for small volumes (Small Volume Module-SVM)
-software for the instrument control and data management
 -Ultrasonic bath
Producer: LIARRE
Model: Starsonic 60 Digit
Serial Number: C000550/08
-Laboratory glassware
-Sampling trier system, consisting of two coaxial tubes, closed at the bottom and with two lateral windows
 
Reagents and Materials
_Silicon oil with a viscosity of 3cSt: e.g. Tegiloxan 3.
_Certified reference standard: 38mm glass microspheres
_Certified reference standard: 106mm glass microspheres
Analytical Method
Coulter Particle Analyzer Check
The Coulter LS 200 particle analyzer was checked using 38mm and 106mm certified reference standards. The reference standards were calibrated by the producer using reference materials traceable to the International Unit of Length.
Instrument verification with 38mm reference standard
The instrument check was performed measuring the particle size distribution of a dispersion of the reference standard 38mm glass microspheres in silicon oil. From the observed results, the median value was determined and compared with the median value reported on the calibration certificate of the reference standard. For the determination of the particle size distribution of the reference standard, the following operations were undertaken:
a) Rinse the sample cell with silicon oil. Fill the sample cell with silicon oil. Measure the background.
b) Disperse the 38mm reference standard in silicon oil immersing the dispersion in an ultrasonic bath at room temperature for 6 min. Fill the sample cell with the dispersion until an obscuration level of 8 %-12 % is achieved.
c) Perform three runs by 60 sec each, with a pause time of 5 sec between each run. For each run, the values of the distribution median and of the standard deviation were calculated by the software.
Instrument verification with 106mm reference standard
The instrument check was performed measuring the particle size distribution of a dispersion of the reference standard 106mm glass microspheres in silicon oil. From the observed results, the median value was determined and compared with the median value.
For the determination of the particle size distribution of the reference standard, the following procedure was applied:
a) Rinse the sample cell with silicon oil. Fill the sample cell with silicon oil. Measure the background.
b) Disperse the 106 mm reference standard in silicon oil immersing the dispersion in an ultrasonic bath at room temperature for 6 min. Fill the sample cell with the dispersion until an obscuration level of 8 %-12 % is achieved.
c) Perform three runs by 60 sec each, with a pause time of 5 sec between each run. For each run, the values of the distribution median and of the standard deviation were calculated by the software.
Sampling method
The test items were sampled from drums containing ~15 Kg of product using a sampling trier system for powders, consisting in two coaxial tubes, closed at the bottom and with two lateral windows. For the sampling of each test item, the following procedure was applied:
a) Lower the closed sampling trier system down to the bottom of the drum containing the product. Briefly mix the content of the drum by applying circular movements to the sampling trier system. Open the two lateral windows of the sampling trier system by
rotating the head. Applying circular or diagonal movement to the opened sampling trier system, fill the sampling trier system with the product. Close the sampling trier system by rotating the head and remove the sampling trier system from the drum. Empty the
content of the sampling trier system (~0.1 Kg of product) into a proper container.
b) Repeat 4 times step a), taking care every time to sample the product in a different area of the drum. Combine the 4 samples obtained, each one consisting of ~0.1 Kg of product, in order to obtain a single sample of ~0.4 Kg of product.
From the 0.4 Kg sample, about 15 g of product were withdrawn. The method of the quartering was applied to the 15 g sample as follows:
a) pour in a watch glass approximately 15 g of sample;
b) subdivide the sample in four parts and draw approximately 1/5 of material from each part;
c) mix the four drawings in a second watch glass;
d) repeat four times operations b) and c) in order to obtain a ~20 mg sample.
The ~20 mg sample was dispersed in silicon oil and the dispersion submitted to diffrattometric analysis.
Dispersing Method
Each of the ~20 mg samples, was dispersed in 50 ml of polymethylsiloxane (Tegiloxan 3) by ultrasonication for 10 min at room temperature. A temperature of the ultrasonic bath higher than 30 ºC may lead to agglomeration of particles that would cause erroneous results of the particle size distribution.
The diffrattometric analysis of each sample was carried out on ~4 ml of the dispersion so obtained.
For each sample, the test was performed in duplicate, by analysing further 4 ml of the same dispersion.

CONDUCT OF THE STUDY
The tests for the determination of the particle size distribution were carried out in duplicate on three samples of different lots of the test substance. Therefore, the following procedure was applied in an identical manner to each sample analyzed and to each duplicate test of the samples. The obtained results will be referred to as Sample 1, Sample 2 and Sample 3, and for each sample as Test 1 and Test 2.
1 Suspend a ~20 mg sample in 50 ml of Tegiloxan 3. Disperse the sample in the ultrasonic bath for 10 min at room temperature.
2 Rinse the sample cell of the analyzer with Tegiloxan 3.
3 Fill the sample cell with Tegiloxan 3. Make sure that no bubble evolution takes place from the sample cell, interfering with the measurement. Measure the background.
4 Transfer to the sample cell, ~4 ml of the product dispersion, prepared at point 1, until the obscuration level of 8-12 % is achieved.
5 Wait until the obscuration level is stable and start the analysis, consisting of three runs of 60 sec each with a pause time of 5 sec between each run.

Mass median aerodynamic diameter:

ca. 4.934 µm

Percentile:

D10

Mean:

ca. 0.805 µm

Remarks on result:

other: ultrasonic bath at room temperature for 6 min.

Key result

Percentile:

D50

Mean:

ca. 4.573 µm

Remarks on result:

other: ultrasonic bath at room temperature for 6 min.

Percentile:

D90

Mean:

ca. 9.52 µm

Remarks on result:

other: ultrasonic bath at room temperature for 6 min.

Sample1

average value of the particle diameter = 4.971 µm

maximum particle diameter = 18.86 µm

Sample2

average value of the particle diameter = 4.086 µm

maximum particle diameter = 17.18 µm

Sample3

average value of the particle diameter = 5.744 µm

maximum particle diameter = 18.86 µm

Conclusions:

The mean particle size value of the test substance is 4.934 µm.
The D50 is 4.573 µm.

Executive summary:

Method

The test method ASTM B 822-92 was used to determine the particle size distribution of the test substance. The method adopted consists in a diffrattometic analysis. The tests for the determination of the granulometry were performed in duplicate on three samples of different lots of product.. For the conduction of the study, the samples, properly dispersed in silicon oil, were introduced in the sample cell of a Coulter LS 200 Particle Analyzer and analysed.

Results

The mean particle size value of the test substance is 4.934 µm.

The D50 is 4.573 µm.

Description of key information

The mean particle size value of the test substance is 4.934 µm.

The D50 is 4.573 µm.

Additional information

The test method ASTM B 822-92 was used to determine the particle size distribution of the test substance. The method adopted consists in a diffrattometic analysis.