4-nitrobenzenesulphonyl chloride

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:

29 August - 15 November 2017

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: ISO 13320-1

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Deviations:

no

Qualifier:

according to guideline

Guideline:

other: CTL SOP No. 417

Deviations:

no

GLP compliance:

yes (incl. QA statement)

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.