Aluminate(2),[[N,N'-1,2-ethanediylbis[N-(carboxymethyl)glycinato]](4-)-N,N',O,O',ON]hydroxy-,disodium

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

16/04/2015-17/04/2015

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

comparable to guideline study

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Test guideline 2

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Test guideline 3

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions - Method A: Particle Size Distribution (effective hydrodynamic radius)

Principles of method if other than guideline:

- PRINCIPLE OF TEST:
The test is conducted to determine the particle size distribution of X300 with a laser diffraction particle size analysis. The guidelines were chosen because of the high solubility of the test item in water and presents as agglomerates.
The analysis is conducted initially using a visual microscope and is then undertaken more formally using a Laser Diffraction Particle Size Analyzer. The benefit of this procedure is that it allows the operator to obtain a better understanding of the particle characterization of the material.
The sample is also initially observed to determine whether sieving of the material is required.
A method development for the particle size analysis on the material is then undertaken to obtain the correct parameters for the formal analysis. The method development is employed to identify the most appropriate optical properties for the material, the correct dispersant, dispersion pressures and sample compatibility. Once these parameters are obtained the final sample is then analyzed using the Malvern Mastersizer 2000 Laser Diffraction Analyzer. It is normal practice to complete 5 runs to ensure repeatability of results.

- SHORT DESCRIPTION OF TEST CONDITIONS:
Optical Microscope Analysis:
The sample is observed under 3 conditions.
• Direct observation
• Under a microscope with 100 x magnification
• Under a microscope with 400 x magnification

Preliminary solubility and dispersability assays are also undergone in order to define the best dispersant for the test item:
In order to select a suitable dispersant, a small quantity of sample is added to approximately 25 ml of solvent. The mixture is shaken for 10 seconds and if the sample is seen to be soluble, then the test is repeated using a different solvent. Testing continues until a suitable dispersant is selected. The complete solubility and dispersability test is then performed using this selected dispersant. In some cases the selected dispersant may be found to be unsuitable after the full test has been performed. The preliminary screening test is then repeated until a suitable solvent is attained. Silicone oil dispersant was selected.
During the method development phase of the analysis trials were conducted using both the dry powder module (DPM) and the small volume (wet) module (SVM). The SVM trials were conducted using silicone oil 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 : Silicon Oil
Dispersion pressure : 2400 rpm
Refractive index (sample) : 0.000 n
Absorption : 0 AU
Analysis Model : General Purpose (Normal)

- Parameters analysed / observed:
During the optical Microscope analysis: The physical characteristics of the material are recorded, noting such items as shape and size distribution.
During the laser diffraction analysis: particule size analysed over the range 0.02 µm to 2000 µm and standard deviation results (d10, d50, d90, d15.78, geometric standard deviation, % standard deviation of the population.

GLP compliance:

yes

Type of method:

Laser scattering/diffraction

Type of particle tested:

agglomerate

Type of distribution:

volumetric distribution

Test material

Test material information

Constituent 1

Test material form:

solid: flakes

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material:040801#
FORM AS APPLIED IN THE TEST (if different from that of starting material): the test item is sieved < 1000 μm prior to testing to remove agglomerations

Results and discussion

Mass median aerodynamic diameter:

ca. 436.737 µm

Geometric standard deviation:

0.041

Remarks on result:

other: standard deviation of the population, or 1.2% (percentage of the standard deviation of the population)

Particle size

Particle size 1

Key result

Percentile:

D10

Mean:

ca. 68.365 µm

St. dev.:

1.184

Remarks on result:

other: 1.7% Percentage standard deviation of the population

Particle size 2

Key result

Percentile:

D50

Mean:

ca. 341.139 µm

St. dev.:

6.757

Remarks on result:

other: 2.0% Percentage standard deviation of the population

Particle size 3

Key result

Percentile:

D90

Mean:

ca. 856.753 µm

St. dev.:

13.873

Remarks on result:

other: 1.6% Percentage standard deviation of the population

Applicant's summary and conclusion

Conclusions:

Particle Size Analysis using small volume module (SVM) with silicon oil as a dispersant:

Volume weighted mean = 407.774 µm
Median (d.50) = 341.139 µm
Mode = 540.097 µm
MMAD (Mass Median Aerodynamic Diameter) mean = 436.737 µm
10 % of material is < 68.365 µm (average)
50 % of material is < 341.139 µm (average)
90 % of material is < 856.753 µm (average)
by volume of sample was seen to be < 10.00 μm = 1.18%

Executive summary:

The granulometry of the substance which is a powder was determined by the laser diffraction method according to the ISO 13320:2009 and CIPAC MT 187 standards. The tests was run with the small volume module (SVM) using the silicone oil as a dispersant and the results were as follow: Volume weighted mean = 407.774 µm Median (d.50) = 341.139 µm Mode = 540.097 µm MMAD (Mass Median Aerodynamic Diameter) mean = 436.737 µm