Reaction products of 4,4'-methylenebis(2,6-dimethylaniline) and 4-aminobenzenesulfonic acid with 2,4,6-trichloro-1,3,5-triazine, diazotised and subsequently coupled with N-(2-methoxyphenyl)-3-oxobutanamide

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:

01 October 2007 to 02 October 2007

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: European Commission Directorate General XII-JRC, Science Research and Development - Joint Research Centre. "Particle Size Distribution, Fibre Length and Diameter Distribution" Guidance Document ECB/TM/February 1996.

Version / remarks:

February 1996

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: European Commission Directorate General JRC, Joint Research Centre. "Particle Size Distribution, Fibre Length and Diameter Distribution" Draft Guidance Document EUR 20268 EN (2002), Part 5.2 “Laser scattering / diffraction”.

Version / remarks:

2002

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of distribution:

mass based distribution

Mass median aerodynamic diameter:

1.6 µm

Geometric standard deviation:

0.075

Remarks on result:

other: Geometric standard deviation not reported.

Percentile:

D10

Mean:

< 0.6 µm

St. dev.:

0.035

Percentile:

D50

Mean:

< 1.6 µm

St. dev.:

0.075

Percentile:

D90

Mean:

< 4.4 µm

St. dev.:

0.166

No.:

#1

Size:

< 0.5 µm

Distribution:

7 %

No.:

#2

Size:

< 1 µm

Distribution:

27.75 %

No.:

#3

Size:

< 2 µm

Distribution:

59.28 %

No.:

#4

Size:

< 3 µm

Distribution:

77.24 %

No.:

#5

Size:

< 4 µm

Distribution:

87.45 %

No.:

#6

Size:

< 5 µm

Distribution:

93.36 %

No.:

#7

Size:

< 6 µm

Distribution:

96.75 %

No.:

#8

Size:

< 7 µm

Distribution:

98.6 %

No.:

#9

Size:

< 8 µm

Distribution:

99.66 %

No.:

#10

Size:

< 9 µm

Distribution:

99.97 %

The test material is a fine yellow powder. Under the microscope (with a magnification of 400) partly agglutinated, fine-grained, crystalline structures were observed. After the mixture was sonicated for 5 min the test material was more evenly spread.

A solubility test showed that the test material is both sparingly soluble and well dispersible in water containing 5 drops Sympatens. The particle size distribution of the test material was performed with two samples of the stock dispersion each measured in duplicate.

The results obtained during the measurements showed no relevant difference. Therefore the study is considered to be valid and no further testing is necessary.

Using the laser diffraction method to study the particle size ranging between 0.3 µm and 300 µm, the mass median diameter (MMD) was determined to be 1.6 µm. The particle size was found to range from approximately 0.3 µm to 9.0 µm.

Particle Size Distribution of the Test Material

[%]	1^stRun particle size [µm]	2^ndRun particle size [µm]	3^rdRun particle size [µm]	4^thRun particle size [µm]	Mean particle size [µm]	Stand. Dev. [±]
5	< 0.43	< 0.43	< 0.47	< 0.47	< 0.5	0.023
10	< 0.55	< 0.55	< 0.61	< 0.61	< 0.6	0.035
50	< 1.57	< 1.58	< 1.70	< 1.71	< 1.6*	0.075
90	< 4.20	< 4.23	< 4.48	< 4.52	< 4.4	0.166

* The MMD of the test material indicates that 50 % (by mass) of the particles are smaller than 1.6 µm.

 

Particle Size Distribution of the Test Material in % at the Relevant Particle Size

[µm]	1^stRun [%]	2^ndRun [%]	3^rdRun [%]	4^thRun [%]	Mean [%]	Stand. Dev. [%]
< 0.3	*****	*****	*****	*****
< 0.5	7.86	7.84	6.15	6.16	7.00	0.98
< 1.0	29.56	29.45	26.03	25.97	27.75	2.02
< 2.0	61.17	60.95	57.62	57.38	59.28	2.06
< 3.0	78.76	78.50	76.01	75.70	77.24	1.61
< 4.0	88.56	88.34	86.59	86.32	87.45	1.61
< 5.0	94.13	93.95	92.78	92.56	93.36	0.80
< 6.0	97.26	97.13	96.38	96.22	96.75	0.52
< 7.0	98.93	98.85	98.37	98.26	98.60	0.34
< 8.0	99.85	99.81	99.52	99.45	99.66	0.20
< 9.0	100.00	99.99	99.95	99.94	99.97	0.03
< 10.0	100.00	100.00	100.00	100.00	100.00	0.00
< 20.0	100.00	100.00	100.00	100.00	100.00	0.00
< 30.0	100.00	100.00	100.00	100.00	100.00	0.00
< 40.0	100.00	100.00	100.00	100.00	100.00	0.00
< 50.0	100.00	100.00	100.00	100.00	100.00	0.00
< 60.0	100.00	100.00	100.00	100.00	100.00	0.00
< 70.0	100.00	100.00	100.00	100.00	100.00	0.00
< 80.0	100.00	100.00	100.00	100.00	100.00	0.00
< 90.0	100.00	100.00	100.00	100.00	100.00	0.00
< 100.0	100.00	100.00	100.00	100.00	100.00	0.00
< 125.0	100.00	100.00	100.00	100.00	100.00	0.00
< 150.0	100.00	100.00	100.00	100.00	100.00	0.00
< 175.0	100.00	100.00	100.00	100.00	100.00	0.00
< 200.0	100.00	100.00	100.00	100.00	100.00	0.00
< 225.0	100.00	100.00	100.00	100.00	100.00	0.00
< 250.0	100.00	100.00	100.00	100.00	100.00	0.00
< 275.0	100.00	100.00	100.00	100.00	100.00	0.00
< 300.0	*****	*****	*****	*****

 

Conclusions:

Under the conditions of the study the mass median diameter was determined to be 1.6 µm. The particle size was found to range from approximately 0.3 µm to 9.0 µm.

Executive summary:

The particle size distribution of the test material was assessed according to European Commission Directorate General Guidance Document ECB/TM/February 1996 and the European Commission Directorate General JRC Draft Guidance Document EUR 20268 EN (2002), Part 5.2 “Laser scattering / diffraction” in compliance with GLP.

Visual examinations were performed macroscopically and microscopically under magnification of 400, using a light microscope to judge the colour and structure of the test material. 

A solubility test was performed to choose a suitable dispersing agent. During the solubility test, water containing 5 drops of Sympatens was selected as an appropriate dispersing agent for this study.

In the main test the dispersing apparatus was rinsed and filled with pre-saturated water containing 5 drops of Sympatens solution. A few mL of the stock solution dispersion were added slowly until the absorption of the laser was reduced by about 10 %. The particle size distribution in the suspension was quantified by laser diffraction. The test was performed with two samples of the stock solution dispersion and each measured in duplicate.

The test material is a fine yellow powder. Under the microscope (with a magnification of 400) partly agglutinated, fine-grained, crystalline structures were observed. After the mixture was sonicated for 5 min the test material was more evenly spread.

A solubility test showed that the test material is both sparingly soluble and well dispersible in water containing 5 drops Sympatens. The particle size distribution of the test material was performed with two samples of the stock dispersion each measured in duplicate.

The results obtained during the measurements showed no relevant difference. Therefore the study is considered to be valid and no further testing is necessary.

Using the laser diffraction method to study the particle size ranging between 0.3 µm and 300 µm, the mass median diameter (MMD) was determined to be 1.6 µm. The particle size was found to range from approximately 0.3 µm to 9.0 µm.

Description of key information

Under the conditions of the study the mass median diameter was determined to be 1.6 µm. The particle size was found to range from approximately 0.3 µm to 9.0 µm.

Additional information

The particle size distribution of the test material was assessed according to European Commission Directorate General Guidance Document ECB/TM/February 1996 and the European Commission Directorate General JRC Draft Guidance Document EUR 20268 EN (2002), Part 5.2 “Laser scattering / diffraction” in compliance with GLP. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

Visual examinations were performed macroscopically and microscopically under magnification of 400, using a light microscope to judge the colour and structure of the test material. 

A solubility test was performed to choose a suitable dispersing agent. During the solubility test, water containing 5 drops of Sympatens was selected as an appropriate dispersing agent for this study.

In the main test the dispersing apparatus was rinsed and filled with pre-saturated water containing 5 drops of Sympatens solution. A few mL of the stock solution dispersion were added slowly until the absorption of the laser was reduced by about 10 %. The particle size distribution in the suspension was quantified by laser diffraction. The test was performed with two samples of the stock solution dispersion and each measured in duplicate.

The test material is a fine yellow powder. Under the microscope (with a magnification of 400) partly agglutinated, fine-grained, crystalline structures were observed. After the mixture was sonicated for 5 min the test material was more evenly spread.

A solubility test showed that the test material is both sparingly soluble and well dispersible in water containing 5 drops Sympatens. The particle size distribution of the test material was performed with two samples of the stock dispersion each measured in duplicate.

The results obtained during the measurements showed no relevant difference. Therefore the study is considered to be valid and no further testing is necessary.

Using the laser diffraction method to study the particle size ranging between 0.3 µm and 300 µm, the mass median diameter (MMD) was determined to be 1.6 µm. The particle size was found to range from approximately 0.3 µm to 9.0 µm.