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

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

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:

2015

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Version / remarks:

2009

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 X330 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 Analyser. The benefit of this procedure is that it allows the operator to obtain a better understanding of the particle characterisation 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 analysed using the Malvern Mastersizer 2000 Laser Diffraction Analyser. 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 : DPM
Dispersant : Air
Dispersion pressure : 0 barg
Refractive index (sample) : 0.000 n
Absorption : 0 AU
Analysis Model : General Purpose (Normal)
Poor data fit was obtained from the SVM analysis as a result, the DPM at optimum dispersion pressure of 0 bar was used for the analysis.

- 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: particulate/powder

Specific details on test material used for the study:

SOURCE OF TEST MATERIAL
- Source and lot/batch No.of test material:040802#

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:

301.1 µm

Geometric standard deviation:

0.022

Remarks on result:

other: 0.7%

Remarks:

Percentage standard deviation of the population

Particle size

Particle size 1

Key result

Percentile:

D10

Mean:

51.087 µm

St. dev.:

0.631

Remarks on result:

other: 1.2%

Remarks:

Percentage standard deviation of the population

Particle size 2

Key result

Percentile:

D50

Mean:

227.608 µm

St. dev.:

4.802

Remarks on result:

other: 2.1%

Remarks:

Percentage standard deviation of the population

Particle size 3

Key result

Percentile:

D90

Mean:

661.336 µm

St. dev.:

8.125

Remarks on result:

other: 1.2%

Remarks:

Percentage standard deviation of the population

Any other information on results incl. tables

Optical microscope Analysis:

Standard visual observation: Sample observed to have gritty, fine, medium and coarse, free flowing, white powder with lumps and clusters. Observation at 100 x magnification: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3.2 μm and the largest individual size was approximately 864.0 μm.

Observation at 400 x magnification: The sample was observed to be made up of single crystalline particles with agglomeration Agglomerations were sieved out prior to the distribution analysis.

After manual sieve analysis: 31% by weight <1000 µm.

Comments: As agglomerations were observed during the optical microscope analysis, the sieve analysis was performed to remove the agglomerations. A 1000 μm sieve was selected as the largest particle measured during the optical microscope analysis was found to be 864 μm.

Solubility And Dispersability Test

The substance in insoluble and well dispersed in silicone oil, which was used for the suspension fluid.

Silicone oil : no solubility and good dispersability (screening test)

table of solubility results (in silicone oil):

	SERIES 1			SERIES 2
Time elapsed	1 (1.5 mg)	2  (1.5 mg)	3  (1.5 mg)	1  (5.0 mg)	2  (5.0 mg)	3  (4.9 mg)
10 seconds	Well dispersed			Well dispersed
30 minutes	Well dispersed			Well dispersed
60 minutes	Well dispersed			Well dispersed
90 minutes	Well dispersed			Well dispersed
120 minutes	Well dispersed			Well dispersed

Laser diffraction Particle Size analysis:

Full test results:

	RUN 1	RUN 2	RUN 3	RUN 4	RUN 5	Average*
Volume weighted mean	297.218	297.443	293.016	302.720	305.589	299.197
Median (d.50)	225.135	225.159	221.451	232.749	233.841	227.608
mode (µm)	304.666	310.238	298.350	327.509	330.266	314.530
MMAD	297.83	297.86	292.95	307.90	309.34	301.10
d10	50.780	50.765	20.284	51.956	51.713	51.087
d50	225.135	225.159	221.451	232.749	233.841	227.608
d90	658.576	659.378	649.335	664.826	674.081	661.336

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

standard deviation results:

RUN n°	1	2	3	4	5	Standard deviation of the population	% standard dev. of the population
d10	50.780	50.765	50.284	51.956	51.713	0.631	1.2
d50	225.135	225.159	221.451	232.749	233.841	4.802	2.1
d90	658.576	659.378	649.335	664.826	674.081	8.125	1.2
Geometric standard deviation	3.092	3.105	3.084	3.125	3.145	0.022	0.7
MMAD	297.83	297.86	292.95	307.90	309.34	6.35	2.1

1.54 % by volume of 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 ISO 13320-1 test standard.

Applicant's summary and conclusion

Conclusions:

Particle Size Analysis using dry powder module (DPM) with Air as a dispersant:

Volume weighted mean = 299.197 µm
Median (d.50) = 227.608 µm
Mode = 314.530 µm
MMAD (Mass Median Aerodynamic Diameter) mean = 301.098 µm
10 % of material is < 51.087 µm (average)
50 % of material is < 227.608 µm (average)
90 % of material is < 661.336 µm (average)
by volume of sample was seen to be < 10.00 μm = 1.54%

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 dry powder module using the air as a dispersant and the results were as follow: Volume weighted mean = 299.197 µm Median (d.50) = 227.608 µm Mode = 314.530 µm MMAD (Mass Median Aerodynamic Diameter) mean = 301.098 µm.