Cyclohexane-1,3-dione

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 Dec 2009 to 11 Feb 2010

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted to GLP and in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do no effect the quality of the relevant results.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2010

Report date:

2010

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

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

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

Date of inspection: 15-09-2009 Date of Signature: 26-11-2009

Type of method:

Laser scattering/diffraction

Type of distribution:

other: by mass

Test material

Test material information

Constituent 1

Reference substance name:

Cyclohexane-1,3-dione

EC Number:

207-980-0

EC Name:

Cyclohexane-1,3-dione

Cas Number:

504-02-9

Molecular formula:

C6H8O2

IUPAC Name:

cyclohexane-1,3-dione

Details on test material:

- Name of test material (as cited in study report): 1,3 cyclohexane dione
- Substance type: Powder
- Physical state: Solid
- Analytical purity: 1,3 Cyclohexane Dione >97% W/W
- Impurities (identity and concentrations): Sodium Chloride 1%W/W Maximum
Water 0.5%W/W Maximum
- Composition of test material, percentage of components: 1,3 Cyclohexane Dione 99.2% W/W
Sodium Chloride 0.25%W/W
Water 0.4%W/W

- Purity test date: 18 November 2009
- Lot/batch No.: 184731091224
- Expiration date of the lot/batch: 18 May 2010
- Radiochemical purity (if radiolabelling): N/A
- Stability under test conditions: Stable
- Storage condition of test material: approximately 4 deg C in the dark

Results and discussion

Particle size

Percentile:

D50

Remarks on result:

other: Too few particles were of a size less than 10µm to allow accurate assessment of mass median aerodynamic diameter(migrated from fields under 'Mass median diameter' as D50 percentile. No source field for Standard deviation.)

Any other information on results incl. tables

Calculations

Using the values obtained from the cascade impactor method determinations, the cumulative mass and cumulative percentage were calculated as follows:

Table 10.22

Collection Stage	Mass at Stage (g)	Cumulative Mass (g)	Cumulative Percentage (%)
Artificial Throat	m0	M0	100
Sample Cup 1	m1	M1	100 x M1/M0
Sample Cup 2	m2	M2	100 x M2/M0
Sample Cup 3	m3	M3	100 x M3/M0
Sample Cup 4	m4	M4	100 x M4/M0
Sample Cup 5	m5	M5	100 x M5/M0
Final Filter	m6	M6	100 x M6/M0

where:

m=mass of test material (g) found at collection stage
M=cumulative mass (g) from collection stage on (eg M₃= m₃+ m₄+ m₅+ m₆)

Results

Screening test (sieve method)

The results of the sieving procedure are shown in the following table:

Table 10.23

Measurement	Result
Mass of test material transferred to sieve	15.23 g
Mass of test material passed through sieve	9.97 g
Proportion of test material <100 µm	65.5 %

Definitive test (cascade impactor method)

The results of the cascade impactor method determinations are shown as follows:

Determination1

Table 10.24

Collection Stage	Particle Size Range Collected (µm)	Masses (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.3155	88.8033	2.4878
Cup 2	5.5 to 10.0	85.6313	85.6683	0.0370
Cup 3	2.4 to 5.5	86.0832	86.0934	0.0102
Cup 4	1.61 to 2.4	85.6145	85.6195	0.0050
Cup 5	0.307 to 1.61	85.9546	85.9595	0.0049
Filter	<0.307	75.6423	75.6484	0.0061

Mass of test material found in artificial throat: 0.38 g.
Total mass of test material recovered in artificial throat, sample cups and filter: 2.9310 g.

Determination 2

Table 10.25

Collection Stage	Particle Size Range Collected (µm)	Masses (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.3163	88.8433	2.5270
Cup 2	5.5 to 10.0	85.6322	85.6585	0.0263
Cup 3	2.4 to 5.5	86.0838	86.0915	0.0077
Cup 4	1.61 to 2.4	85.6154	85.6189	0.0035
Cup 5	0.307 to 1.61	85.9557	85.9589	0.0032
Filter	<0.307	75.6502	75.6536	0.0034

Mass of test material found in artificial throat: 0.36 g.
Total mass of test material recovered in artificial throat, sample cups and filter: 2.9311 g.

Determination 3

Table10.26

Collection Stage	Particle Size Range Collected (µm)	Masses (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	85.9562	88.4845	2.5283
Cup 2	5.5 to 10.0	85.6172	85.6309	0.0137
Cup 3	2.4 to 5.5	86.0856	86.0883	0.0027
Cup 4	1.61 to 2.4	85.6341	85.6347	0.0006
Cup 5	0.307 to 1.61	86.3181	86.3192	0.0011
Filter	<0.307	75.6401	75.6418	0.0017

Mass of test material found in artificial throat: 0.42 g.
Total mass of test material recovered in artificial throat, sample cups and filter: 2.9681 g.

Cumulative amounts

The cumulative amounts of test material found in the three determinations for the individual particle size cut-points (µm) are shown in the following table:

Table 10.27

Particle Size Cut-point (µm)	Cumulative Mass (g)			Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Determination 1	Determination 2	Determination 3
10.0	0.0632	0.0441	0.0198	2.16	1.51	0.667
5.5	0.0262	0.0178	0.0061	0.894	0.607	0.206
2.4	0.0160	0.0101	0.0034	0.546	0.345	0.115
1.61	0.0110	0.0066	0.0028	0.375	0.225	9.43 x 10^-2
0.307	0.0061	0.0034	0.0017	0.208	0.116	5.73 x 10^-2

The overall cumulative percentage (%) of test material with a particle size less than 10.0 µm and 5.5 µm are shown in the following table:

Table10.28

Particle size	Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Mean
<10.0 µm	2.16	1.51	0.667	1.44
<5.5 µm	0.894	0.607	0.206	0.569

Applicant's summary and conclusion

Conclusions:

Particle size data for the test material was as follows:
The proportion of test material having an inhalable particle size <100 µm, as determined by sieve method, was 65.5%
The proportion of test material having thoracic particle size <10.0 µm, as determined by cascade impactor was 1.44%
The proportion of test material having a respirable particle size <5.5 µm, as determined by cascade impactor was 0.569%

Executive summary:

Particle Size Distribution. Particle size data have been acquired using a procedure designed to comply with the European Commission technical guidance document 'Particle Size Distribution, Fibre Length and Diameter Distribution' (June 1996), which satisfies the requirements of OECD Guideline 110. The results are as follows:

Measurement	Method	Result
Proportion of test material having an inhalable particle size less than 100 µm	Sieve	65.5%
Proportion of test material having a thoracic particle size less than 10.0 µm	Cascade Impactor	1.44%
Proportion of test material having a respirable particle size less than 5.5 µm	Cascade Impactor	0.569%