6,6'-[(3,3'-di-tert-butyl-5,5'-dimethoxybiphenyl-2,2'-diyl)bis(oxy)]bis(dibenzo[d,f][1,3,2]dioxaphosphepine)

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Testing was conducted between 20 April 2010 and 29 April 2010.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study conducted in compliance with agreed protocols, with no or minor deviations from standard test guidelines and/or minor methodological deficiencies, which do not affect 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:

UK GLP standards (Schedule 1, Good Laboratory Practice Regulations 1999 (SI 1999/3106 as amended by SI 2004/0994)). These Regulations are in accordance with GLP standards published as OECD Principles on Good Laboratory Practice (revised 1997, ENV/MC/CHEM

Type of distribution:

other: Cascade Impactor

Test material

Test material information

Constituent 1

Reference substance name:

9-[(3,3'-di-tert-butyl-2'-{8,10-dioxa-9-phosphatricyclo[9.4.0.0²,⁷]pentadeca-1(11),2(7),3,5,12,14-hexaen-9-yloxy}-5,5'-dimethoxy-[1,1'-biphenyl]-2-yl)oxy]-8,10-dioxa-9-phosphatricyclo[9.4.0.0²,⁷]pentadeca-1(11),2(7),3,5,12,14-hexaene

EC Number:

700-178-6

Cas Number:

121627-17-6

Molecular formula:

C46H44O8P2

IUPAC Name:

9-[(3,3'-di-tert-butyl-2'-{8,10-dioxa-9-phosphatricyclo[9.4.0.0²,⁷]pentadeca-1(11),2(7),3,5,12,14-hexaen-9-yloxy}-5,5'-dimethoxy-[1,1'-biphenyl]-2-yl)oxy]-8,10-dioxa-9-phosphatricyclo[9.4.0.0²,⁷]pentadeca-1(11),2(7),3,5,12,14-hexaene

Details on test material:

Sponsor's identification : L17
Description : off white solid
Purity : not supplied
Batch number : not supplied
Date received : 06 April 2010
Expiry date : 15 October 2010
Storage conditions : room temperature, in the dark

Results and discussion

Particle size

Particle size 1

Percentile:

D50

Mean:

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

Remarks on result:

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

Particle size 2

Mean:

other: Not applicable

Particle size distribution at different passages

Particle size distribution at different passages 1

No.:

#1

Size:

< 100 other: µm

Distribution:

9.4 %

Particle size distribution at different passages 2

No.:

#2

Size:

< 10 other: µm

Distribution:

0.074 %

Particle size distribution at different passages 3

No.:

#3

Size:

< 5.5 other: µm

Distribution:

0.052 %

Any other information on results incl. tables

Results

Screening Test

           

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

Measurement	Result
Mass of test item transferred to sieve	10.96 g
Mass of test item passed through sieve	1.03 g
Proportion of test item <100 µm	9.40%

Definitive Test

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

Determination1

Collection Stage	Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.4433	89.4429	2.9996
Cup 2	5.5 to 10.0	85.7506	85.7515	0.0009
Cup 3	2.4 to 5.5	86.1906	86.1908	0.0002
Cup 4	1.61 to 2.4	85.9245	85.9246	0.0001
Cup 5	0.307 to 1.61	86.0687	86.0688	0.0001
Filter	<0.307	75.6600	75.6604	0.0004

Mass of test item found in artificial throat: 0.00 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.0013 g.

Determination 2

Collection Stage	Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.4423	89.4371	2.9948
Cup 2	5.5 to 10.0	85.7508	85.7511	0.0003
Cup 3	2.4 to 5.5	86.1894	86.1898	0.0004
Cup 4	1.61 to 2.4	85.9234	85.9240	0.0006
Cup 5	0.307 to 1.61	86.0683	86.0689	0.0006
Filter	<0.307	75.6601	75.6601	0.0000

Mass of test item found in artificial throat: 0.01 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.0067 g.

Determination 3

Collection Stage	Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.4438	89.4435	2.9997
Cup 2	5.5 to 10.0	85.7502	85.7510	0.0008
Cup 3	2.4 to 5.5	86.1891	86.1900	0.0009
Cup 4	1.61 to 2.4	85.9236	85.9241	0.0005
Cup 5	0.307 to 1.61	86.0674	86.0683	0.0009
Filter	<0.307	75.6600	75.6598	-0.0002*

Mass of test item found in artificial throat: 0.01 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.0128 g.

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	0.0017	0.0019	0.0031	5.66 x 10^-2	6.32 x 10^-2	0.103
5.5	0.0008	0.0016	0.0023	2.67 x 10^-2	5.32 x 10^-2	7.63 x 10^-2
2.4	0.0006	0.0012	0.0014	2.00 x 10^-2	3.99 x 10^-2	4.65 x 10^-2
1.61	0.0005	0.0006	0.0009	1.67 x 10^-2	2.00 x 10^-2	2.99 x 10^-2
0.307	0.0004	0.0000	0.0000	1.33 x 10^-2	0.000	0.000

 

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	5.66 x 10^-2	6.32 x 10^-2	0.103	7.43 x 10^-2
<5.5 µm	2.67 x 10^-2	5.32 x 10^-2	7.63 x 10^-2	5.21 x 10^-2

*Value of 0.000 g used in further calculations. Negative value within the uncertainty of the balance.

Applicant's summary and conclusion

Conclusions:

Particle size data acquired for the test item is shown below:

Proportion of test item having an inhalable particle size <100 µm by the sieve method was 9.40%
Proportion of test item having a thoracic particle size <10.0 µm by the Cascade Impactor was 7.43 x 10-2 %
Proportion of test item having a respirable particle size <5.5 µm by the Cascade Impactor was 5.21 x 10-2 %

Executive summary:

Summary

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

Measurement	Method	Result
Proportion of test item having an inhalable particle size <100 µm	Sieve	9.40%
Proportion of test item having a thoracic particle size <10.0 µm	Cascade Impactor	7.43 x 10^-2%
Proportion of test item having a respirable particle size <5.5 µm	Cascade Impactor	5.21 x 10^-2%