2-Thiazolamine, 4-(2-naphthalenyl)-

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Between 29 May 2012 and 31 May 2012.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: see 'Remark'

Remarks:

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. The study report was conclusive, done to a valid guideline and the study was conducted under GLP conditions.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2012

Report date:

2012

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

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

Deviations:

no

Principles of method if other than guideline:

The method used is based on a procedure designed to be compatible with that given in ‘Particle Size Distribution, Fibre Length and Diameter Distribution’, June 1996 European Commission technical guidance document, which satisfies the requirements of OECD Guideline 110.

GLP compliance:

yes

Type of method:

cascade impaction

Remarks:

A sieve test was also completed.

Type of distribution:

other: The method used is based on a procedure designed to be compatible with that given in ‘Particle Size Distribution, Fibre Length and Diameter Distribution’, June 1996 European Commission technical guidance document, which satisfies the requirements of OECD

Test material

Test material information

Constituent 1

Reference substance name:

4-(naphthalen-2-yl)-1,3-thiazol-2-amine

EC Number:

606-740-6

Cas Number:

21331-43-1

Molecular formula:

C13H10N2S

IUPAC Name:

4-(naphthalen-2-yl)-1,3-thiazol-2-amine

Test material form:

solid: particulate/powder

Details on test material:

Sponsor's identification : 4-(2-naphthalenyl)-2-thiazolamine
Description : Off white powder
Purity : 98.8%
Batch number : 107 (ex Pentagon)
Date received : 08 May 2012
Expiry date : Not supplied
Storage conditions : Room temperature in the dark

Results and discussion

Particle size distribution at different passages

Particle size distribution at different passages 1

No.:

#1

Size:

< 100 µm

Distribution:

7.71 %

Remarks on result:

other: Sieve

Particle size distribution at different passages 2

No.:

#2

Size:

< 10 µm

Distribution:

1.41 %

Remarks on result:

other: Cascade Impactor

Particle size distribution at different passages 3

No.:

#3

Size:

< 5.5 µm

Distribution:

0.06 %

Remarks on result:

other: Cascade Impactor

Any other information on results incl. tables

         

Results

Screening Test (Sieve Method)

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

 

Table 3.1

 

Measurement	Result
Mass of test item transferred to sieve	10.25 g
Mass of test item passed through sieve	0.79 g
Proportion of test item <100 µm	7.71 %

 

     

Definitive Test (Cascade Impactor Method)

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

 

Determination 1

Table 3.2

 

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.1186	88.3573	2.2387
Cup 2	5.5 to 10.0	85.5584	85.5960	0.0376
Cup 3	2.4 to 5.5	85.9094	85.9100	0.0006
Cup 4	1.61 to 2.4	85.6873	85.6876	0.0003
Cup 5	0.307 to 1.61	85.8589	85.8589	0.0000
Filter	<0.307	75.5367	75.5375	0.0008

 

Mass of test item found in artificial throat: 0.74 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.0180 g.

 

Determination 2

Table 3.3

 

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.1198	88.6059	2.4861
Cup 2	5.5 to 10.0	85.5593	85.5827	0.0234
Cup 3	2.4 to 5.5	85.9110	85.9120	0.0010
Cup 4	1.61 to 2.4	85.6895	85.6895	0.0000
Cup 5	0.307 to 1.61	85.8603	85.8603	0.0000
Filter	<0.307	75.5415	75.5423	0.0008

 

Mass of test item found in artificial throat: 0.51 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 3.0213 g

 

Determination 3

Table 3.4

 

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.1201	88.6715	2.5514
Cup 2	5.5 to 10.0	85.5596	85.6199	0.0603
Cup 3	2.4 to 5.5	85.9116	85.9126	0.0010
Cup 4	1.61 to 2.4	85.6896	85.6896	0.0000
Cup 5	0.307 to 1.61	85.8606	85.8606	0.0000
Filter	<0.307	75.5381	75.5391	0.0010

 

Mass of test item found in artificial throat: 0.35 g.
Total mass of test item recovered from artificial throat, sample cups and filter: 2.9637 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:

 

Table 3.5

 

Particle Size Cut-point (µm)	Cumulative Mass (g)			Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Determination 1	Determination 2	Determination 3
10.0	0.0393	0.0252	0.0623	1.30	0.834	2.10
5.5	0.0017	0.0018	0.0020	0.06	0.06	0.07
2.4	0.0011	0.0018	0.0010	0.04	0.03	0.03
1.61	0.0008	0.0018	0.0010	0.03	0.03	0.03
0.307	0.0008	0.0018	0.0010	0.03	0.03	0.03

 

 

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:

 

Table 3.6

 

Particle size	Cumulative Percentage (%)
	Determination 1	Determination 2	Determination 3	Mean
<10.0 µm	1.30	0.834	2.10	1.41
<5.5 µm	0.06	0.06	0.07	0.06

 

 

Applicant's summary and conclusion

Conclusions:

Particle size data acquired for the test item is shown in the table below in the Executive Summary Section.

Executive summary:

The method used is based on a procedure designed to be compatible with that given in ‘Particle Size Distribution, Fibre Length and Diameter Distribution’, June 1996 European Commission technical guidance document, which satisfies the requirements of OECD Guideline 110.

       

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. 

   

Conclusion

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

 

Table 3.7

 

Measurement		Method		Result
Proportion of test item having an inhalable particle size <100 µm		Sieve		7.71 %
Proportion of test item having a thoracic particle size <10.0 µm		Cascade Impactor		1.41 %
Proportion of test item having a respirable particle size <5.5 µm		Cascade Impactor		0.06 %