Reaction products of cyclohexylamine, alkan-1-amine and 1,1'-methanediylbis(4-isocyanatobenzene)

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:

From 2008-10-14 to 2008-11-10

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

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

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

other: image analysis

Type of particle tested:

primary particle

Type of distribution:

mass based distribution

Specific details on test material used for the study:

- Analytical purity: > 95.0%
- Lot/batch No.: 2008-9-16

No.:

#1

Size:

> 105 µm

Distribution:

11.8 %

No.:

#2

Size:

> 60 - <= 105 µm

Distribution:

18.3 %

No.:

#3

Size:

> 30 - <= 60 µm

Distribution:

13.2 %

No.:

#4

Size:

> 10.4 - <= 30 µm

Distribution:

8.8 %

No.:

#5

Size:

> 0.5 - <= 10.4 µm

Distribution:

2.5 %

Sieve Analysis

A portion (10 g) of the test substance was weighed into the coarsest of a nest of sieves (100 mm diameter) of aperture sizes 400, 125, 75, 30 and 10 microns. The nest was shaken for 30 minutes with tapping (Pascall Inclyno sieve shaker), and the proportion of the test material passing through each sieve determined gravimetrically. The test was performed in duplicate, and the results are summarised thus:  

Particle Size (µm)	% in range by weight
	Test 1	Test 2	Test 3
> 400	3.5	3.4	3.5
400 – 125	40.7	40.7	40.7
125 – 75	17.7	17.5	17.6
75 – 30	33.6	30.1	31.9
30 – 10	3.9	7.2	5.6
< 10	0.0	0.0	0.0

 

Image Analysis (based on BS3406, Part 4, 1993) 

A suitable suspending medium was experimentally determined to fulfill the following properties. 

i)  low solubility

ii) different refractive index

iii) low volatility

iv) good dispersion

 

Six replicate samples, each approximately 5 g in weight, were individually weighed into a 125 micron sieve and the contents sieved by shaking for 10 minutes. The proportion of each sample passing through the sieve was determined gravimetrically. A portion of the sieved material was suspended by agitation and mounted on a microscope slide for image analysis. 

Particle size (µm)	% Mass
	Test 1	Test 2	Test 3	Test 4	Test 5	Test 6	Mean
> 125 (sieved)	46.3	45.5	44.9	45.2	45.2	45.9	45.5
> 105	8.1	16.7	12.2	6.6	17.1	10.1	11.8
60.0 – 105	22.6	16.7	20.0	22.8	11.4	16.3	18.3
30.0 – 60.0	14.5	13.3	13.0	11.7	10.8	15.8	13.2
10.4 – 30.0	6.9	6.2	7.7	11.3	11.1	9.4	8.8
0.5 – 10.4	1.7	1.6	2.2	2.3	4.5	2.5	2.5

 The observed particles were irregular and crystalline in nature.

Conclusions:

The results indicated that 2.5% w/w of test item was smaller than 10 µm.

Executive summary:

Particle size was determined in accordance with OECD Guideline 110. The particle size distribution was initially examined using sieve analysis. As greater than 10% by weight of the test substance was found to pass a 75 micron sieve, it was further examined by image analysis.

The results indicated that 2.5% w/w of test item was smaller than 10 µm.

Description of key information

Particle size was determined in accordance with OECD Guideline 110.

The results indicated that 2.5% w/w of test item was smaller than 10 µm.