disodium 5-{4-chloro-6-[N-ethyl-3-(vinylsulfonyl)anilino]-1,3,5-triazin-2-ylamino}-4-hydroxy-3-[(4-vinylsulfonyl)phenylazo]naphthalene-2,7-disulfonate; reaction mass of: trisodium 5-{4-chloro-6-[N-ethyl-(3-(2-sulfonatooxy)ethylsulfonyl)anilino]-1,3,5-triazin-2-ylamino}-4-hydroxy-3-[4-(vinylsulfonyl)phenylazo]naphthalene-2,7-disulfonate; tetrasodium 5-{4-chloro-6-[N-ethyl-3-(2-(sulfonatooxy)ethylsulfonyl)anilino]-1,3,5-triazin-2-ylamino}-3-[4-(2-(sulfonatooxy)ethylsulfonyl)phenylazo]-4-hydroxynaphthalene-2,7-disulfonate; trisodium 5-{4-chloro-6-[N-ethyl-3-(vinylsulfonyl)anilino]-1,3,5-triazin-2-ylamino}-4-hydroxy-3-[4-(2-(sulfonatooxy)ethylsulfonyl)phenylazo]naphthalene-2,7-disulfonate

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

October 17, 2002 - November 20, 2002

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other:

Version / remarks:

EUROPEAN COMMISSION, Directorate General Xll-JRC, Science Research and Development-Joint Research Centre. "Particle Size Distribution, Fibre Length and Diameter Distribution" Guidance Document, ECB/TM/February 1996.

Qualifier:

equivalent or similar to guideline

Guideline:

OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions) - Method B: Fibre Length and Diameter Distributions

Version / remarks:

The laser scattering / diffraction method has been applied. As specified in OECD TG 110, there is no standard procedure for method B (fibre length and diameter distributions). The sample preparation for method B suggested in OECD TG 110 is different from the one followed in the current study but this is not a major deviation. Quality criteria for repeatability (measurement in duplicate) and sensitivity (diameter between 0.2 and 300 µm) are met.

Principles of method if other than guideline:

The laser scattering / diffraction method has been applied. As specified in OECD TG 110, there is no standard procedure for method B (fibre length and diameter distributions). The sample preparation for method B suggested in OECD TG 110 is different from the one followed in the current study but this is not a major deviation. Quality criteria for repeatability (measurement in duplicate) and sensitivity (diameter between 0.2 and 300 µm) are met.

GLP compliance:

yes

Type of method:

Laser scattering/diffraction

Type of particle tested:

other: not specified

Type of distribution:

other: mass median diameter

Mass median aerodynamic diameter:

31.7 µm

Geometric standard deviation:

1.471

Key result

Percentile:

D10

Mean:

< 15.2 µm

St. dev.:

0.964

Key result

Percentile:

D50

Mean:

< 31.7 µm

St. dev.:

1.471

Key result

Percentile:

D90

Mean:

< 60.6 µm

St. dev.:

2.934

The individual measurements and the results obtained using the laser diffraction of Red Rwa 4565 are summarised in Table 1 and Table 2. The tables represent rounded results obtained by using the exact measurement data.

 

Table 1: Particle size distribution of Red Rwa 4565

%	1. Run Particle Size µm	2. Run Particle Size µm	3. Run Particle Size µm	4. Run Particle Size µm	Mean Particle Size µm	Stand. Dev. [±]
5	<10.54	<10.38	<11.93	<11.76	<11.2	0.805
10	<14.44	<14.30	<16.14	<15.92	<15.2	0.964
50	<30.51	<30.35	<33.27	<32.59	<31.7	1.471
90	<58.42	<57.94	<64.02	<62.12	<60.6	2.934

* The MMD of the test item indicates that 50 % of the particles are smaller than 31.7 µm.

 

Table 2: Particle size distribution of Red Rwa 4565 (% at the relevant particle size)

%	1. Run %	2. Run %	3. Run %	4. Run %	Mean %	Stand. Dev. [±]
<0.3	-	-	-	-
<0.5	0.15	0.15	0.14	0.14	0.15	0.01
<1.0	0.45	0.46	0.39	0.40	0.43	0.04
<2.0	0.84	0.87	0.76	0.79	0.82	0.05
<3.0	1.13	1.17	1.06	1.10	1.12	0.05
<4.0	1.46	1.51	1.36	1.41	1.44	0.06
<5.0	1.84	1.90	1.67	1.73	1.79	0.10
<6.0	2.24	2.32	1.99	2.06	2.15	0.15
<7.0	2.69	2.78	2.32	2.40	2.55	0.22
<8.0	3.19	3.29	2.69	2.77	2.99	0.30
<9.0	3.79	3.91	3.12	3.21	3.51	0.40
<10.0	4.53	4.67	3.64	3.75	4.15	0.53
<20.0	21.92	22.31	17.22	17.92	19.84	2.64
<30.0	48.68	49.10	42.00	43.52	45.82	3.59
<40.0	70.13	70.49	64.29	65.96	67.72	3.07
<50.0	83.41	83.74	79.02	80.42	81.65	2.30
<60.0	91.03	91.34	87.80	88.87	89.76	1.71
<70.0	95.10	95.38	92.71	93.48	94.17	1.28
<80.0	97.44	97.68	95.67	96.20	96.75	0.97
<90.0	98.75	98.94	97.45	97.80	98.24	0.72
<100.0	99.47	99.63	98.52	98.73	99.09	0.54
<125.0	100.0	100.0	99.71	99.74	99.86	0.16
<150.0	100.0	100.0	100.0	100.0	100.0	0.0
<175.0	100.0	100.0	100.0	100.0	100.0	0.0
<200.0	100.0	100.0	100.0	100.0	100.0	0.0
<225.0	100.0	100.0	100.0	100.0	100.0	0.0
<250.0	100.0	100.0	100.0	100.0	100.0	0.0
<275.0	100.0	100.0	100.0	100.0	100.0	0.0
<300.0	-	-	-	-

Conclusions:

Using a laser diffraction apparatus to study the particle size of Red Rwa 4565 in the range between 0.3 µm and 300 µm the mass median diameter (MMD) was determined to be 31.7 µrm. The particle size distribution was found to range from approximately 0.3 µm to 150 µm.

Executive summary:

The determination of the particle size distribution of Red Rwa 4565 was performed according to the European Commission, Document ECB/TM/February 1996: "Particle Size Distribution, Fibre Length and Diameter Distribution" Guidance Document using the laser diffraction method.

Red Rwa 4565 is a dark red fine powder. Under the microscope (with a magnification of 400) round red, crystalline structures with various sizes were observed. A solubility test showed, that the test item is both: sparingly soluble and well dispersible in 2-propanol. The particle size distribution of Red Rwa 4565 was performed with two samples of the stock dispersion each measured in duplicate.

The results obtained during the measurements showed no relevant difference. The standard deviation is smaller than 5% therefore the study is considered to be valid and no further testing is necessary.

ln conclusion using a laser diffraction apparatus to study the particle size of Red Rwa 4565 in the range between 0.3 µm and 150 µm the mass median diameter (MMD) was determined to be 31.7 µm. The particle size distribution was found to range from approximately 0.3 µm to 150 µm.

Description of key information

Using a laser diffraction apparatus to study the particle size of Red Rwa 4565 in the range between 0.3 µm and 300 µm the mass median diameter (MMD) was determined to be 31.7 µrm. The particle size distribution was found to range from approximately 0.3 µm to 150 µm.