Sodium 4-(4-substitutedanilino)-4-substituedbut-2-enoate

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

27 Jul - 16 Aug 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

test procedure in accordance with national standard methods

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

other: European Commission Guidance Document EUR 20268 (Determination of Particle Size Distribution, Fibre Length and Diameter Distribution of Chemical Substances)

Version / remarks:

adopted in 2002

GLP compliance:

yes (incl. QA statement)

Remarks:

Department of Health, London, UK

Type of method:

other: Sieve Screening Test + Cascade Impactor

Type of particle tested:

primary particle

Type of distribution:

mass based distribution

Test material

Test material information

Constituent 1

Specific details on test material used for the study:

Storage conditions: room temperature in the dark

Results and discussion

Remarks on result:

not determinable

Remarks:

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

Particle size distribution at different passages

Particle size distribution at different passages 1

No.:

#1

Size:

< 100 µm

Distribution:

ca. 99.5 %

Particle size distribution at different passages 2

No.:

#2

Size:

< 10 µm

Distribution:

ca. 1.18 %

Particle size distribution at different passages 3

No.:

#3

Size:

< 5.5 µm

Distribution:

ca. 0.33 %

Any other information on results incl. tables

Sieve screening test

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

Table 2

Measurement	Result
Mass of test item transferred to sieve	12.72 g
Mass of test item passed through sieve	12.65 g
Percentage of test item less than 100 μm	99.5%

 

Cascade impactor

The results of the cascade impactor procedure are shown in the following table

Table 3

Collection stage	Particle size range collected [μm]	Collected mass [g]
		Determination 1	Determination 2	Determination 3
Artificial throat	n/a	0.11	0.26	0.34
Cup 1	>10.0	2.8421	2.7082	2.6418
Cup 2	5.5 to 10.0	0.0200	0.0266	0.0302
Cup 3	2.4 to 5.5	0.0041	0.0056	0.0069
Cup 4	1.61 to 2.4	0.0014	0.0028	0.0016
Cup 5	0.307 to 1.61	0.0008	0.0013	0.0014
Final filter	<0.307	0.0006	0.0016	0.0016
Total mass of collected test item		2.9790	3.0061	3.0235
Mass of test item added		3.0055	3.0317	3.0439

 

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

Table 4

Particle size cut point [μm]	Cumulative mass [g]			Cumulative percentage [%]
	Determination 1	Determination 2	Determination 3	Determination 1	Determination 2	Determination 3
<10.0	0.0269	0.0379	0.0417	0.90	1.26	1.38
<5.5	0.0069	0.0113	0.0115	0.23	0.38	0.38
<2.4	0.0028	0.0057	0.0046	9.4E-02	0.19	0.15
<1.61	0.0014	0.0029	0.0030	4.7E-02	9.6E-02	9.9E-02
<0.307	0.0006	0.0016	0.0016	2.0E-02	5.3E-02	5.3E-02

 

Mean cumulative percentage with a particle size less than 10.0 μm: 1.18%

Mean cumulative percentage with a particle size less than 5.5 μm: 0.33%

 

 

Discussion

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 overall results from the cascade impactor were taken as limit values due to the variation between the sampling positions; this gives a worst case scenario.

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

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.

 

Conclusion

Particle size data acquired for the test item is shown in the following table

Table 5

Measurement	Method	Result
Percentage of test item with an inhalable particle size <100 μm	Sieve	99.5%
Percentage of test item with a thoracic particle size <10.0 μm	Cascade impactor	1.18%
Percentage of test item with a respirable particle size <5.5 μm	Cascade impactor	0.33%