Reaction mass of hydrogen [1-[(2-hydroxy-4-nitrophenyl)azo]-2-naphtholato(2-)][1-[(2-hydroxy-5-nitrophenyl)azo]-2-naphtholato(2-)]chromate(1-) , compound with 3-[(2-ethylhexyl)oxy]propylamine (1:1) and hydrogen bis[1-[(2-hydroxy-4-nitrophenyl)azo]-2-naphtholato(2-)]chromate(1-) , compound with 3-[(2-ethylhexyl)oxy]propylamine (1:1) and hydrogen bis[1-[(2-hydroxy-5-nitrophenyl)azo]-2-naphtholato(2-)]chromate(1-) , compound with 3-[(2-ethylhexyl)oxy]propylamine (1:1)

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:

13 July 2017 to 21 July 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Version / remarks:

2009

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Mass median aerodynamic diameter:

2.59 µm

Geometric standard deviation:

0.008

Key result

Percentile:

D10

Mean:

0.761 µm

St. dev.:

0.006

Key result

Percentile:

D50

Mean:

2.242 µm

St. dev.:

0.01

Key result

Percentile:

D90

Mean:

5.598 µm

St. dev.:

0.047

Visual Observations

- Standard visual observation: Sample observed to be a fine, black powder with clusters.

- Observation using 3.2 objective lens: The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3.2 μm and the largest individual size was approximately 12.8 μm.

- Observation using 40 objective lens: The sample was observed to be made up of single crystalline particles with agglomerations.

Laser Diffraction

- Results can be seen in Tables 1 and 2.

97.87 % by volume of the sample was seen to be < 10.00 µm.

- Coefficient of variation for d50 is less than 3 %; d10 and d90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the test guideline.

Table 1: Laser Diffraction Full Test Results

	RUN 1	RUN 2	RUN 3	RUN 4	RUN 5	**Average
Volume weighted Mean	2.912	2.965	2.961	2.905	2.871	2.923
Median (d.50)	2.242	2.253	2.250	2.241	2.223	2.242
Mode	2.569	2.580	2.560	2.553	2.553	2.563
*MMAD	2.591	2.604	2.599	2.589	2.569	2.59
d10- 10 % of material is <	0.756	0.762	0.768	0.766	0.753	0.761
d50- 50 % of material is <	2.242	2.253	2.250	2.241	2.223	2.242
d90- 90 % of material is <	5.614	5.649	5.632	5.581	5.517	5.598

* Mass Median Aerodynamic Diameter

**Average result is calculated from the entirety of the data captured in each run and is not a simple arithmetic mean.

 All results are in µm.

Table 2: Laser Diffraction Standard Deviation Results

	RUN 1	RUN 2	RUN 3	RUN 4	RUN 5	STDVP	%STDVP
d10	0.756	0.762	0.768	0.766	0.753	0.006	0.8
d50	2.242	2.253	2.250	2.241	2.223	0.010	0.5
d90	5.614	5.649	5.632	5.581	5.517	0.047	0.8
d15.78	0.963	0.969	0.974	0.971	0.958	0.006	0.6
GSD	2.328	2.325	2.310	2.308	2.320	0.008	0.3
MMAD	2.591	2.604	2.599	2.589	2.569	0.012	0.5

GSD = Geometric standard deviation of the lognormal particle size distribution [calculated from d50/d15.78]

STDVP = Standard deviation of the population

% STDVP = Percentage standard deviation of the population

Conclusions:

Under the conditions of this study the d10, d50 and d90 of the test material were 0.761, 2.242 and 5.598 µm, respectively.

Executive summary:

The particle size distribution of the test material was investigated in accordance with the standardised guideline ISO 13320, under GLP conditions.

The particle size was investigated using microscope analysis and laser diffraction with the Malvern Mastersizer 2 000 Laser Diffraction Analyser.

97.87 % by volume of the sample was seen to be < 10.00 µm. The coefficient of variation for d50 was less than 3 %; d10 and d90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the test guideline

Under the conditions of this study the d10, d50 and d90 of the test material were 0.761, 2.242 and 5.598 µm, respectively.

Description of key information

Under the conditions of this study the d10, d50 and d90 of the test material were 0.761, 2.242 and 5.598 µm, respectively.

Additional information

The particle size distribution of the test material was investigated in accordance with the standardised guideline ISO 13320, under GLP conditions. The study was awarded a reliability score of 1 in accordance with the criteria set forth by Klimisch et al. (1997).

The particle size was investigated using microscope analysis and laser diffraction with the Malvern Mastersizer 2 000 Laser Diffraction Analyser.

97.87 % by volume of the sample was seen to be < 10.00 µm. The coefficient of variation for d50 was less than 3 %; d10 and d90 are less than 5 %. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits as per the test guideline

Under the conditions of this study the d10, d50 and d90 of the test material were 0.761, 2.242 and 5.598 µm, respectively.