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Particle size distribution (Granulometry)

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Reference
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
29 August - 15 November 2017
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to
Guideline:
other: ISO 13320-1
Deviations:
no
Qualifier:
according to
Guideline:
other: CIPAC MT 187
Deviations:
no
Qualifier:
according to
Guideline:
other: CTL SOP No. 417
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
Laser scattering/diffraction
Type of distribution:
volumetric distribution
Specific details on test material used for the study:
-Batch number: M16LB4523
-Purity / composition: 99.80% area (based on chromatographic purity)
-Test item storage: At room temperature
-Expiration date : 01 December 2017 (retest date)
Mass median aerodynamic diameter:
823.564 µm
Geometric standard deviation:
>= 1.749 - <= 1.758
Percentile:
D10
Mean:
294.216 µm
St. dev.:
1.997
Remarks on result:
other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.
Key result
Percentile:
D50
Mean:
624.342 µm
St. dev.:
4.162
Remarks on result:
other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.
Percentile:
D90
Mean:
1 137.853 µm
St. dev.:
10.52
Remarks on result:
other: Average result is calculated from the entirety of data captured in each run and is not a simple arithmetic mean.

Visual Microscope Analysis

(1) Standard visual observation: medium and coarse, slightly yellow to yellowish brown, crystalline powder.

(2) 3.2 objective lens: particles appeared to be irregular shaped crystals (smallest +/- 19 µm and largest +/- 1056 µm).

(3) 40 objective lens: sample was observed to be made up of single crystalline particles.

 

Solubility and Dispersability Test

The sample proved to be insoluble and well dispersed in water. Therefore, water was used as the suspension fluid.

 

Laser Diffraction Particle Size Analysis

Using the identified parameters, the particle size was analysed over the range 0.2 μm to 2000 μm.

The average Volume weighted Mean was 671.141µm and the mode was 665.768µm. The Coefficient of Variation for d50 was <3%; d10 and d90 were <5%. Thus the repeatability of the characteristic particles in the size distribution was within the acceptable limits according to the ISO 13320-1 test standard.

Conclusions:
Visual examination using 3.2 objective lens showed irregular shaped crystals between approximately 19 µm and 1056 µm.
The particle size distribution of 4-nitrobenzene-1-sulfonylchloride determined by the laser diffraction method led to the conclusion that the average volume weighted mean based on 5 runs was 229.014µm and the Mass Median Aerodynamic Diameter (MMAD) based on 5 runs was 671.141 µm, whereas the average D10, D50 and the D90 were determined to be 294.216 µm, 624.342 µm and 1137.853 µm, respectively.

Description of key information

The particle size distribution of 4-Nitrobenzene-1-sulfonyl chloride was determined by the laser diffraction method in a GLP study according to Chilworth Technology Ltd SOP n°417, ISO 13320:2009 and CIPAC MT 187 (Livingston, 2017). The visual examination using 3.2 objective lens showed irregular crystals between approximately 19 µm and 1056 µm. The MMAD was determined to be 671.141 µm, whereas the average D10, D50 and the D90 were determined to be 290.216 µm, 624.342 µm and 1137.853 µm, respectively.

Additional information