Iodonium, bis[4-(1,1-dimethylethyl)phenyl]-, hexafluorophosphate(1-) (1:1)

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

15 Nov 2011 – 13 Jan 2012

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP study according to EU and OECD methods

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Report date:

2012

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

other: European Commission technical guidance document, June 1996

Deviations:

no

Test guideline 2

Qualifier:

equivalent or similar to guideline

Guideline:

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

Version / remarks:

adopted in 1981

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

Department of Health, UK GLP Monitoring Authority (2011)

Type of distribution:

volumetric distribution

Test material

Test material information

Constituent 1

Reference substance name:

bis(4-tert-butylphenyl)iodanium; hexafluoro-λ⁵-phosphanuide

EC Number:

620-341-4

Cas Number:

61358-25-6

Molecular formula:

C20H26F6IP

IUPAC Name:

bis(4-tert-butylphenyl)iodanium; hexafluoro-λ⁵-phosphanuide

Details on test material:

- Name of test material (as cited in study report): PF-6
- Physical state: white powder
- Analytical purity: 99.2 %
- Batch No.: 20101020
- Expiration date of the batch: 12 April 2012
- Storage condition of test material: In the dark, at room temperature

Results and discussion

Particle size

Percentile:

D50

Remarks on result:

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

Particle size distribution at different passages

Particle size distribution at different passages 1

No.:

#1

Size:

< 100 µm

Distribution:

50.3 %

Remarks on result:

other: screening test

Particle size distribution at different passages 2

No.:

#2

Size:

< 10 µm

Distribution:

0.783 %

Remarks on result:

other: cumulative percentage, mean of 3 determinations

Particle size distribution at different passages 3

No.:

#3

Size:

< 5.5 µm

Distribution:

0.212 %

Remarks on result:

other: cumulative percentage, mean of 3 determinations

Any other information on results incl. tables

Screening test (sieve method)
The results of the sieving procedure are shown in the following table:

 

Measurement	Result
Mass of test item transferred to sieve	1607 g
Mass of test item passed through sieve	8.09 g
Proportion of test item < 100 µm	50.3 %

 

Definitive test (cascade impactor method)

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

Determination 1
Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.1227	89.1431	3.0204
Cup 2	5.5 to 10.0	85.5586	85.5846	0.0260
Cup 3	2.4 to 5.5	85.9064	85.9109	00045
Cup 4	1.61 to 2.4	85.6891	85.6902	0.0011
Cup 5	0.307 to 1.61	85.8601	85.8606	0.0005
Filter	< 0.307	75.5584	75.5600	0.0016

 

Mass of test item found in artificial throat: 0.06 g.

Total mass of test item recovered from artificial throat, sample cups and filter: 3.1141 g.

 

Determination 2
Collection Stage		Particle Size Range Collected (µm)	Mass (g)
			Pre-sampling	Post-sampling	Difference
Cup 1		>10.0	86.1232	88.9498	2.8266
Cup 2		5.5 to 10.0	85.5581	85.5744	0.0163
Cup 3		2.4 to 5.5	85.9066	85.9102	0.0036
Cup 4		1.61 to2.4	85.6883	85.6895	0.0012
Cup 5		0.307 to 1.61	85.8601	85.8604	0.0003
Filter		< 0.307	75.5609	75.5622	0.0013

Mass of test item found in artificial throat: 0.15 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 2.9993 g.

 

Determination 3
Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.1231	88.8464	27233
Cup 2	5.5 to 10.0	85.5584	85.5689	0.0105
Cup 3	2.4 to 5.5	85.9070	85.9101	0.0031
Cup 4	1.61 to2.4	85.6885	85.6898	0.0013
Cup 5	0.307 to 1.61	85.8600	85.8602	0.0002
Filter	< 0.307	75.5631	75.5640	0.0009

Mass of test item found in artificial throat: 0.39 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.12939.

Cumulative amounts
The cumulative amounts of test item found in the three determinations for the individual particle size cut-points are shown in the following table:

Particle Size Cut-point (µm)	Cumulative Mass (g)			Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Determination 1	Determination 2	Determination 3
10.0	0.0337	0.0227	0.0160	1.08	0.757	0.511
5.5	0,0077	0.0064	0.0055	0.247	0.213	0.176
2.4	0.0032	0.0028	0.0024	0.103	9.34 x 10^-2	7.67 x 10^-2
1.61	0.0021	0.0016	0.0011	6.74 x 10^-2	5,34 x 10^-2	3.52 x 10^-2
0.307	0.0016	0.0013	0.0009	5.14 x 10^-2	4.33 x 10^-2	2.88 x 10^-2

 

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

Particle size	Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Mean
< 10.0 µm	1.08	0.757	0.511	0.783
< 5.5 µm	0.247	0.213	0.176	0.212

 

Discussion
Too few particles were of a size less than 10.0 µm to allow accurate assessment of the mass median aerodynamic diameter.

Sampling for the cascade impactor determinations was performed by rolling the test item container for approximately 10 minutes then sampled from the top, middle and bottom.

The inhalable fraction is defined as the mass fraction of particles which can be inhaled by nose or mouth, the thoracic fraction is defined as the mass fraction of particles that passes the larynx and the respirable fraction is defined as the mass fraction of particles that reaches the alveoli.

Applicant's summary and conclusion

Conclusions:

The particle size distribution of PF-6 was determined using the sieve method (screening test) and the cascade impactor method (definitive test): 50.3 wt-% had an inhalable particle size < 100 µm, 0.783 wt-% had a thoracic particle size < 10 µm and 0.212 % had a respirable particle size < 5.5 µm.