lithium hydrogen 7-{(E)-[2-amino-4-(2-naphthyl)-1,3-thiazol-5-yl]diazenyl}naphthalene-1,3,5-trisulfonate (2:1:1)

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Study test phase 2014-01-30 to 2014-02-25. Report complete 2014-04-15.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Meets the criteria for classification as reliable without restriction according to Klimisch et al (1997).

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2014

Report date:

2014

Materials and methods

Test guideline

Qualifier:

according to guideline

Guideline:

other: European Commission Technical Guidance Document EUR 20268: Determination of Particle Size Distribution, Fibre Length and Diameter Distribution of chemical substances (2002).

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

cascade impaction

Type of distribution:

mass based distribution

Test material

Test material information

Constituent 1

Reference substance name:

lithium hydrogen 7-{(E)-[2-amino-4-(2-naphthyl)-1,3-thiazol-5-yl]diazenyl}naphthalene-1,3,5-trisulfonate (2:1:1)

EC Number:

940-433-0

Molecular formula:

C23H14Li2N4O9S4

IUPAC Name:

lithium hydrogen 7-{(E)-[2-amino-4-(2-naphthyl)-1,3-thiazol-5-yl]diazenyl}naphthalene-1,3,5-trisulfonate (2:1:1)

Test material form:

solid: particulate/powder

Remarks:

migrated information: powder

Results and discussion

Mass median aerodynamic diameter:

other:

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:

62.4 %

Remarks on result:

other: Sieving

Particle size distribution at different passages 2

No.:

#2

Size:

< 10 µm

Distribution:

<= 0.817 %

Remarks on result:

other: Cascade Impactor

Particle size distribution at different passages 3

No.:

#3

Size:

< 5.5 µm

Distribution:

<= 0.247 %

Remarks on result:

other: Cascade Impactor

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	17.61 g
Mass of test item passed through sieve	10.98 g
Proportion of test item <100 µm	62.4 %

 

 

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	86.0653	88.4178	2.3525
Cup 2	5.5 to 10.0	85.5313	85.5484	0.0171
Cup 3	2.4 to 5.5	85.8885	85.8914	0.0029
Cup 4	1.61 to 2.4	85.6855	85.6885	0.0030
Cup 5	0.307 to 1.61	85.8572	85.8583	0.0011
Filter	<0.307	0.1165	0.1169	0.0004

 

Mass of test item found in artificial throat: 0.62 g
Total mass of test item recovered from artificial throat, sample cups and filter: 3.00 g

 

Determination 2

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.0654	87.6761	1.6107
Cup 2	5.5 to 10.0	85.5317	85.5451	0.0134
Cup 3	2.4 to 5.5	85.8890	85.8917	0.0027
Cup 4	1.61 to 2.4	85.6877	85.6893	0.0016
Cup 5	0.307 to 1.61	85.8580	85.8592	0.0012
Filter	<0.307	0.1174	0.1178	0.0004

 

Mass of test item found in artificial throat: 1.51 g
Total mass of test item recovered from artificial throat, sample cups and filter: 3.14 g

 

Determination 3

Collection Stage	Particle Size Range Collected (µm)	Mass (g)
		Pre-sampling	Post-sampling	Difference
Cup 1	>10.0	86.0656	87.9492	1.8836
Cup 2	5.5 to 10.0	85.5313	85.5364	0.0051
Cup 3	2.4 to 5.5	85.8893	85.8900	0.0007
Cup 4	1.61 to 2.4	85.6884	85.6886	0.0002
Cup 5	0.307 to 1.61	85.8582	85.8582	0
Filter	<0.307	0.1180	0.0083	0.0003

 

Mass of test item found in artificial throat: 1.19 g
Total mass of test item recovered from artificial throat, sample cups and filter: 3.08 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	0.0245	0.0193	0.0063	0.817	0.615	0.205
5.5	0.0074	0.0059	0.0012	0.247	0.188	0.039
2.4	0.0045	0.0032	0.0005	0.150	0.102	0.016
1.61	0.0015	0.0016	0.0003	0.050	0.051	0.010
0.307	0.0004	0.0004	0.0003	0.013	0.013	0.010

 

 

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	Overall
<10.0 µm	0.817	0.615	0.205	≤0.817
<5.5 µm	0.247	0.188	0.039	≤0.247

Applicant's summary and conclusion

Conclusions:

The proportion of the test material that can be inhaled by the mouth of nose was determined to be 62.4%. The proportion of test material that is capable of passing the larynx was determined to be <0.817% and the proportion that is capable of reaching the alveoli was determined to be <0.247%.

Executive summary:

Introduction

This study was undertaken to determine the particle size distribution of the test material. The method used is based on a procedure designed to be compatible with that given in ‘European Commission Technical Guidance Document EUR 20268 ‘Determination of Particle Size Distribution, Fibre Length and Diameter Distribution of chemical substances’ (2002).

Results & Conclusions

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

The proportion of the test material that can be inhaled by the mouth of nose was determined to be 62.4%. The proportion of test material that is capable of passing the larynx was determined to be <0.817% and the proportion that is capable of reaching the alveoli was determined to be <0.247%.