1,4-Diazabicyclo[2.2.2]octane-2-methanol

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:

9-23 May 2014

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: ISO 13320:2009

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Principles of method if other than guideline:

laser diffraction analysis according to laboratory Standard Operating Procedure CTL SOP No. 417

GLP compliance:

yes (incl. QA statement)

Remarks:

The Department of Health of the Government of the United Kingdom

Type of method:

Laser scattering/diffraction

Type of distribution:

volumetric distribution

Mass median aerodynamic diameter:

36.578 µm

Geometric standard deviation:

>= 3.355 - <= 3.448

Percentile:

D50

Mean:

33.253 µm

Remarks on result:

other: average result calculated from the entirety of data captured in each of 5 runs and not a simple arithmetic mean (holds also for MMAD below)(migrated from fields under 'Mass median diameter' as D50 percentile. No source field for Standard deviation.)

Percentile:

D10

Mean:

6.88 µm

St. dev.:

0.097

Remarks on result:

other: average result calculated from the entirety of data captured in each of 5 runs and not a simple arithmetic mean

Percentile:

D50

Mean:

33.253 µm

St. dev.:

0.835

Remarks on result:

other: average result calculated from the entirety of data captured in each of 5 runs and not a simple arithmetic mean

Percentile:

D90

Mean:

248.338 µm

St. dev.:

9.729

Remarks on result:

other: average result calculated from the entirety of data captured in each of 5 runs and not a simple arithmetic mean

No.:

#1

Size:

< 0.55 µm

Distribution:

0.05 %

No.:

#2

Size:

< 1.445 µm

Distribution:

1.08 %

No.:

#3

Size:

< 7.586 µm

Distribution:

11.37 %

No.:

#4

Size:

< 10 µm

Distribution:

16.29 %

No.:

#5

Size:

< 34.674 µm

Distribution:

51.19 %

No.:

#6

Size:

< 50 µm

Distribution:

61.01 %

No.:

#7

Size:

< 104.713 µm

Distribution:

77.26 %

No.:

#8

Size:

< 954.993 µm

Distribution:

100 %

Optical microscope analysis

Standard visual observation: sample observed to be a medium size, white powder with lumps and clusters.

Observation at 100x magnification: the particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 μm and the largest individual size was approximately 736 μm.

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

Manual sieve analysis

56.8% by weight < 1000 µm (383.8 g of 675.9 g)

Solubility and dispersability test for particle size analysis (incl. preliminary test)

The sample proved to be insoluble, and well dispersed in kerosene. Therefore kerosene was used as the suspension fluid.

Laser diffraction particle size analysis test results

Full test results:

All results are in µm.

	Run 1	Run 2	Run 3	Run 4	Run 5	Average**
Volume weighted Mean	86.480	86.659	88.873	80.846	83.180	85.207
Median (d.50)	34.121	33.988	33.685	32.070	32.473	33.253
Mode (µm)	22.453	22.083	21.688	21.161	21.114	21.658
MMAD*	37.533	37.387	37.053	35.277	35.720	36.578
10% of material is <	7.008	6.953	6.906	6.753	6.787	6.880
50% of material is <	34.121	33.988	33.685	32.070	32.473	33.253
90% of material is <	249.106	255.294	259.159	231.634	254.818	248.338

* Mass Median Aerodynamic Diameter

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

16.29% by volume of sample was seen to be < 10.00 µm.

Standard deviation results:

Run No.	1	2	3	4	5	STDVP	% STDVP
D10	7.008	6.953	6.906	6.753	6.787	0.097	1.4
D50	34.121	33.988	33.685	32.070	32.473	0.835	2.5
D90	249.106	255.294	259.159	231.634	254.818	9.729	3.9
D15.78	9.950	9.858	9.792	9.558	9.621	0.146	1.5
GSD	3.429	3.448	3.440	3.355	3.375	0.037	1.1
MMAD	37.53	37.39	37.05	35.28	35.72	0.92	2.5

GSD = Geometric standard deviation

STDVP = standard deviation of the population

% STDVP = percentage standard deviation of the population

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.

Description of key information

D10 = 6.88 µm; D50 = 33.253 µm; D90 = 248.338 µm; MMAD = 36.578 µm (ISO 13320: 2009, CIPAC MT 187, laser diffraction analysis)

Additional information

Although there is data available for the substance in a powder form, it is to be mentioned that the substance will only be handled and used in water solution.