Bis(5-oxo-L-prolinato-N1,O2)zinc

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:

18 August 2016 to 22 August 2016

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Deviations:

no

Qualifier:

according to guideline

Guideline:

ISO 13320 (Particle size analysis - Laser diffraction methods)

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of particle tested:

agglomerate

Type of distribution:

mass based distribution

Mass median aerodynamic diameter:

300.954 µm

Geometric standard deviation:

>= 5.394 - <= 5.555

Percentile:

D10

Mean:

23.416 µm

St. dev.:

0.472

Percentile:

D50

Mean:

236.671 µm

St. dev.:

4.46

Percentile:

D90

Mean:

567.394 µm

St. dev.:

6.26

No.:

#1

Size:

< 10 µm

Distribution:

4.64 %

Optical Microscope Analysis

Standard visual observation

Sample observed to be a coarse, medium to fine white powder with clusters.

Observation at 100 x magnification

The particles appeared to be irregular shaped crystals. The smallest individual particle size was approximately 3 μm and the largest individual size was approximately 352 μm.

Observation at 400 x magnification

The sample was observed to be made up of single crystalline particles.

 

Laser diffraction

During the method development phase of the analysis trials were conducted using the dry powder module (DPM). The results of these trials indicated that the most appropriate test and material parameters to obtain the optimum measurements were:

Module: DPM

Dispersant: Air

Dispersion pressure: 0.5 barg

Refractive index (sample): 0.000 n

Absorption: 0.0 AU

Analysis Model: General Purpose (Fine)

Using the identified parameters, the particle size was analysed over the range 0.02 μm to 2000 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 ISO 13320-1 test standard.

Full test results

	Run 1	Run 2	Run 3	Run 4	Run 5	** Average
Volume weighted mean	272.577	264.908	268.301	265.157	268.029	267.794
Mean (d.50)	240.744	231.889	236.919	231.377	242.322	236.671
Mode (µm)	406.679	395.037	403.302	400.554	402.498	401.650
*MMAD	306.134	294.874	301.269	294.222	308.140	300.954
10 % of material is <	23.490	23.148	23.482	22.797	24.222	23.416
50 % of material is <	240.744	231.889	236.919	231.377	242.322	236.671
90 % of material is <	577.964	564.151	569.012	567.297	558.963	657.394

All results are in μm

* Mass Median Aerodynamic Diameter

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

Standard Deviation Results 

Run No.	1	2	3	4	5	STDVP %	STDVP
d10	23.490	23.148	23.482	22.797	24.222	0.472	2.0
d50	240.744	231.889	236.919	231.377	242.322	4.460	1.9
d90	577.964	564.151	569.012	567.297	558.963	6.260	1.1
d15.78	43.336	42.556	43.076	41.688	44.923	1.065	2.5
GSD	5.555	5.449	5.500	5.550	5.394	0.061	1.1
MMAD	306.13	294.87	301.27	294.22	308.14	5.67	1.9

GSD = Geometric standard deviation of the lognormal particle size distribution

STDVP = standard deviation of the population

% STDVP = percentage standard deviation of the population

Conclusions:

Under the conditions of the test the d50 of the test material was 236.671 µm. The d10 was 23.416 µm, the d90 was 567.394 µm.
4.64 % was seen to be < 10 µm.
The MMAD was 300.954 µm.

Executive summary:

The particle size distribution of the test material was assessed in accordance with ISO 13320:2009 and CIPAC MT 187 and took into consideration OECD guideline 110.

The analysis was conducted initially using a visual microscope and then undertaken more formally using a Laser Diffraction Particle Size Analyser.

The sample was initially observed to determine whether sieving of the material is required. A method development for the particle size analysis on the material was then undertaken to obtain the correct parameters for the formal analysis. The method development was employed to identify the most appropriate optical properties for the material, the correct dispersant, dispersion pressures and sample compatibility. Once these parameters were obtained the final sample was then analysed using the Malvern Mastersizer 2000 Laser Diffraction Analyser. It is normal practice to complete 5 runs to ensure repeatability of results.

Using the identified parameters, the particle size was analysed over the range 0.02 μm to 2000 μm.

Coefficient of variation for d50 was less than 3%; d10 and d90 were less than 5%. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits

Under the conditions of the test the d50 of the test material was 236.671 µm.  The d10 was 23.416  µm, the d90 was 567.394  µm.

4.64 % was seen to be < 10 µm.

The MMAD was 300.954  µm.

Description of key information

Under the conditions of the test the d50 of the test material was 236.671 µm.  The d10 was 23.416  µm, the d90 was 567.394  µm.

4.64 % was seen to be < 10 µm.

The MMAD was 300.954  µm.

Additional information

The particle size distribution of the test material was assessedin accordance with ISO 13320:2009 and CIPAC MT 187 and took into consideration OECD guideline 110.

The analysis was conducted initially using a visual microscope and then undertaken more formally using a Laser Diffraction Particle Size Analyser.

The sample was initially observed to determine whether sieving of the material is required. A method development for the particle size analysis on the material was then undertaken to obtain the correct parameters for the formal analysis. The method development was employed to identify the most appropriate optical properties for the material, the correct dispersant, dispersion pressures and sample compatibility. Once these parameters were obtained the final sample was then analysed using the Malvern Mastersizer 2000 Laser Diffraction Analyser. It is normal practice to complete 5 runs to ensure repeatability of results.

Using the identified parameters, the particle size was analysed over the range 0.02 μm to 2000 μm.

Coefficient of variation for d50 was less than 3%; d10 and d90 were less than 5%. Thus repeatability of the characteristic particles in the size distribution are within the acceptable limits

Under the conditions of the test the d50 of the test material was 236.671 µm.  The d10 was 23.416  µm, the d90 was 567.394  µm.

4.64 % was seen to be < 10 µm.

The MMAD was 300.954  µm.