Lupine, L. albus, ext.

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:

7 April 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

The study was conducted according to an internationally recognised method, and under GLP. The test substance is adequately characterised. Therefore, full validation applies.

Qualifier:

according to guideline

Guideline:

OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: ISO 13320-1:1999

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: NFX11-507 (1989)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

GLP certificate (inspected on 22 and 23 December 2014/signed on 28 July 2015)

Type of method:

sieving

Type of distribution:

mass based distribution

Key result

Percentile:

D50

Mean:

ca. 130 µm

Remarks on result:

other: 'Mass median diameter' as D50 percentile. No source field for Standard deviation.

Results

Preliminary sieving

Ambient humidity About 34%

Temperature About 22 °C

Mass of test item used 50.07 g

Table 4.5.2

Test sieve	25 mm	4 mm	1 mm	0.1 mm	Collecting pan (<0.1 mm)	Total mass after sieving (g)
Mass of residue(g)	/	/	0.00	38.75*	11.27	50.02
Percentage of residue (%)	/	/	0.0	77.4	22.5
Time of mechanical sieving (min)	/	/	30	30	30
Time of manual sieving (min)	/	/	1	6	/

The loss of test item was 0.1%.

Remark: The particles size was visibly lower than 1 mm. So, the sieves of 25 mm and 4 mm were not used.

*The distribution of the test item has shown that the major part of the test item was retained by the 100-μm sieve. In this case, the maximal volume of the test item which can be retained by the sieve (46 cm3) was reached, knowing that the density of the test item was determined at 0.689 g/cm3 during the study No. 16-919076-002.

So as to have a representative particle size distribution, a minimum quantity of about 50 g of the test item was necessary even if this quantity is higher than the quantity prescribed by the guideline.

The maximal volumes of the material which can be retained of sieves indicated in the Table No. 4.5.1 is given to have an optimal sieving. With a higher charge of product retained on the sieve, the complete surface is occupied and some particles with a lower size can be blocked by particles retained on the sieve with a higher size. As a mechanical and a manual sieving is done, this situation does not exist. It may exist when the sieve is static. The quantity of the particles between the collecting pan (<0.1 mm) and the sieve of 1 mm is higher than 20% of the charge. So, the principal sieving was made with sieves with mesh sizes lower than 1 mm.

Principal sieving

From 710 μm to 125 μm

Ambient humidity About 33%

Temperature About 22 °C

Mass of test item used 38.45 g (from the preliminary sieving) corresponding

to 76.8% of the initial mass of the test item

Table No. 4.5.3

Test sieve	710 µm	500 µm	355 µm	250 µm	180 µm	125 µm	Collecting pan	Total mass after sieving (g)
Particles size (µm)	>710	500-710	355-500	250-355	180-250	125-180	100-125	/
Mass of residue (g)	0.00	0.02	0.11	1.09	7.78	17.74	11.71	38.45
Percentage of residue (% w/w) related to the initial mass used (50.07 g)	0.0	0.0	0.2	2.2	15.5	35.4	23.4
Cumulated undersized particles (% w/w of the substance < Test sieve)	100.0	100.0	99.7	97.6	82.0	46.6	23.2
Time of mechanical sieving (min)	30	30	30	30	30	30	/
Time of manual sieving (min)	1	1	2	2	7	13	/

No loss of mass was recorded.After sieving, the maximal volume of the test item which can be retained by each sieve was not reached.

From 90 μm to 20 μm

Ambient humidity About 30%

Temperature About 22 °C

Mass of test item used 11.23 g (from the preliminary sieving) corresponding

to 22.4% of the initial mass of the test item

Table No. 4.5.4

Test sieve	90 µm	63 µm	45 µm	32 µm	25 µm	20 µm	Collecting pan	Total mass after sieving(g)
Particles size (µm)	90-100	63-90	45-63	32-45	25-32	20-25	<20	/
Mass of residue (g)	5.32	4.77	0.76	0.20	0.05	0.00	0.00	11.10
Percentage of residue (% w/w) related to the initial mass used (50.07 g)	10.6	9.5	1.5	0.4	0.1	0.0	0.0
Cumulated undersized particles (% w/w of the substance < Test sieve)	11.5	2.0	0.5	0.1	0.0	0.0	0.0
Time of mechanical sieving (min)	30	30	30	30	30	30	/
Time of manual sieving (min)	7	5	3	2	1	/	/

A loss of mass of about 1.2%was observed, which may be due to the loss of material during the handling of the substance and the thickness of the particles. After sieving, the maximal volume of the test item which can be retained by each sieve was not reached.

Summary of the particle size distribution

Particles size (µm)	>710	500-710	355-500	250-355	180-250	125-180	100-125	90-100	63-90	45-63	32-45	25-32	20-25	<20
Mass of residue(g)	0.00	0.02	0.11	1.09	7.78	17.74	11.71	5.32	4.77	0.76	0.20	0.05	0.00	0.00
Percentage of residue(%w/w)	0.0	0.0	0.2	2.2	15.5	35.4	23.4	10.6	9.5	1.5	0.4	0.1	0.0	0.0

Conclusion

 

After the preliminary test, it was shown that the majority of the particles (77.4%) was between a size of 1 mm and 100 µm. 22.5% of the particles has a size lower than 100 µm.

 

After the main test, it was shown thatthe particle size distribution of the test item was found to range approximately between 25 µm to 500 µm and only 11.5% are lower than 90 µm. 76.7% of the test item has got a size between 100 µm and 500 µm.

 

The median diameter was calculated at 130 µm.

Conclusions:

After the preliminary test, it was shown that the majority of the particles (77.4%) was between a size of 1 mm and 100 µm. 22.5% of the particles has a size lower than 100 µm.
After the main test, it was shown that the particle size distribution of the test item was found to range approximately between 25 µm to 500 µm and only 11.5% are lower than 90 µm. 76.7% of the test item has got a size between 100 µm and 500 µm. The median diameter was calculated at 130 µm.

Executive summary:

The particle size distribution of the test substance was determined under GLP according to the Guideline OECD No. 110 (1981), ISO 13320-1:2009 and NFX11-507 (1989).

After the preliminary test, it was shown that the majority of the particles (77.4%) was between a size of 1 mm and 100 μm. 22.5% of the particles has a size lower than 100 μm.

After the main test, it was shown that the particle size distribution of the test item was found to range approximately between 25 μm to 500 μm and only 11.5% are lower than 90 μm. 76.7% of the test item has got a size between 100 μm and 500 μm. The median diameter was calculated at 130 μm.

Description of key information

The median diameter was calculated at 130 μm.

Additional information

After the preliminary test, it was shown that the majority of the particles (77.4%) was between a size of 1 mm and 100 μm. 22.5% of the particles has a size lower than 100 μm. After the main test, it was shown that the particle size distribution of the test item was found to range approximately between 25 μm to 500 μm and only 11.5% are lower than 90 μm. 76.7% of the test item has got a size between 100 μm and 500 μm. The median diameter was calculated at 130 μm.