Oxirane, 2,2'-[methylenebis[(2,6-dimethyl-4,1-phenylene)oxymethylene]]bis-

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:

11 January 2011

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

Deviations:

no

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)

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Specific details on test material used for the study:

The analysis was conducted using the dry powder module.

Mass median aerodynamic diameter:

645.987 µm

Geometric standard deviation:

0.04

Key result

Percentile:

D50

Mean:

645.987 µm

St. dev.:

12.16

Key result

Percentile:

D10

Mean:

160.487 µm

St. dev.:

3.28

Key result

Percentile:

D90

Mean:

1 353.261 µm

St. dev.:

10.07

No.:

#1

Size:

< 10 µm

Distribution:

0.42 %

OPTICAL MICROSCOPE ANALYSIS

- Standard visual observation: The sample was observed to be a free-flowing, coarse, gritty powder with clusters, some of the clusters were greater than 2000 μm.

- Observation at 100 x magnification: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 6.4 μm and the largest individual size was approximately 1216 μm.

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

 

MANUAL SIEVE ANALYSIS

- Result : 94.18 % by weight < 2000 μm

Table 1: Manual Sieve Analysis Results

Sieve Size (µm)	Sieve Weight (g)	Sieve + Powder Weight (g)	Powder Weight (g)	% By Weight
> 2000	326	338.3	12.3	5.82
< 2000	246.1	445.3	199.2	94.18
TOTALS			211.5	100

 

LASER DIFFRACTION PARTICLE SIZE ANALYSIS

Table 2: Laser Diffraction Analysis Results

	RUN 1	RUN 2	RUN 3	RUN 4	RUN 5	*Average
Volume Weighted Mean	715.117	712.929	699.033	717.006	696.276	708.272
Median (d.50)	656.425	653.006	634.008	657.846	628.762	645.987
Mode (µm)	855.405	856.641	833.273	880.259	839.512	853.347
10% of material is <	162.946	165.309	159.867	158.537	155.965	160.487
50% of material is <	656.425	653.006	634.008	657.846	628.762	645.987
90% of material is <	1356.892	1356.840	1340.168	1367.801	1343.341	1353.261

All results are in μm

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

0.42% by volume of sample was seen to be < 10.00 μm.

Table 3: Standard Deviation Results

Run No.	1	2	3	4	5	ST DVP	% STDV
d10	162.946	165.309	159.867	158.537	155.965	3.28	2.05
d50	656.425	653.006	634.008	657.846	628.762	12.16	1.88
d90	1356.892	1356.840	1340.168	1367.801	1343.341	10.07	0.74
d15.78	243.700	245.440	236.370	237.440	232.460	4.81	2.01
*GSD	2.694	2.661	2.682	2.771	2.705	0.04	1.37

*GSD = Geometric standard deviation

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 BS ISO 13320-1 test standard.

Conclusions:

Under the conditions of this study manual sieve analysis indicated that 94.18% by weight of the sample had a particle size of < 2000 μm. A subsequent laser diffraction analysis on the < 2000 μm sample produced the following results: Volume weighted mean = 708.272 µm, Median (d.50) = 645.987 µm, Mode = 853.347 µm, 10% of material was < 160.487 µm, 50% of material was < 645.987 µm and 90% of material was < 1353.261 µm. 0.42% by volume of the test material sample was seen to be < 10.00 μm

Executive summary:

The particle size distribution of the test material was investigated in accordance with the standardised guidelines ISO 13320:2009 and CIPAC MT 187, taking into consideration OECD guideline 110. The testing was performed under GLP conditions.

The analysis was conducted using the dry powder module.

Under the conditions of this study manual sieve analysis indicated that 94.18% by weight of the sample had a particle size of < 2000 μm. A subsequent laser diffraction analysis on the < 2000 μm sample produced the following results: Volume weighted mean = 708.272 µm, Median (d.50) = 645.987 µm, Mode = 853.347 µm, 10% of material was < 160.487 µm, 50% of material was < 645.987 µm and 90% of material was < 1353.261 µm. 0.42% by volume of the test material sample was seen to be < 10.00 μm.

Description of key information

Under the conditions of the study manual sieve analysis indicated that 94.18% by weight of the sample had a particle size of < 2000 μm. A subsequent laser diffraction analysis on the < 2000 μm sample produced the following results: Volume weighted mean = 708.272 µm, Median (d.50) = 645.987 µm, Mode = 853.347 µm, 10 % of material was < 160.487 µm, 50 % of material was < 645.987 µm and 90 % of material was < 1353.261 µm. 0.42% by volume of the test material sample was seen to be < 10.00 μm

Additional information

The particle size distribution of the test material was investigated in accordance with the standardised guidelines ISO 13320:2009 and CIPAC MT 187, taking into consideration OECD guideline 110. The testing was performed 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 analysis was conducted using the dry powder module.

Under the conditions of the study manual sieve analysis indicated that 94.18 % by weight of the sample had a particle size of < 2000 μm. A subsequent laser diffraction analysis on the < 2000 μm sample produced the following results: Volume weighted mean = 708.272 µm, Median (d.50) = 645.987 µm, Mode = 853.347 µm, 10% of material is < 160.487 µm, 50% of material is < 645.987 µm and 90% of material is < 1353.261 µm. 0.42% by volume of the test material sample was seen to be < 10.00 μm.