Registration Dossier

Administrative data

Endpoint:
appearance / physical state / colour
Type of information:
experimental study
Adequacy of study:
key study
Study period:
05 October 2017 - 01 March 2018
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Cross-reference
Reason / purpose:
reference to same study
Reference
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
05 October 2017 - 01 March 2018
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
Qualifier:
according to
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
2009
Qualifier:
according to
Guideline:
other: CIPAC MT 187 (Particle size analysis by laser diffraction)
Version / remarks:
Handbook K, 2007
Principles of method if other than guideline:
According to REACH Article 13(3) tests on substances shall be conducted in accordance with the test methods laid down in a Commission Regulation or in accordance with other international test methods recognised by the Commission or the Agency as being appropriate. No particle size distribution test method is laid down in regulation (EC) No 440/2008. OECD 110 TG ‘Particle Size Distribution/Fibre Length and Diameter Distributions’ dates from 1981 and describes two methods in detail; both methods have restrictions and are not applicable to the entire size range. ECHA’s Guidance on information requirements and Chemical Safety Assessment-Chapter R.7a stipulates that many methods are available for particle size measurements but none of them is applicable to the entire size range. The guidance mentions Laser scattering/diffraction as a method for particles of all kind and makes reference to ISO 13320:2009.

According to Guidance document EUR 20268 (2002), the laser diffraction technique is applicable to particles of respirable and inhalable size. The MMAD can be calculated when density is known.
GLP compliance:
yes (incl. certificate)
Remarks:
certificate issued on 13 Jan 2016
Type of method:
Laser scattering/diffraction
Type of particle tested:
primary particle
Type of distribution:
volumetric distribution
Specific details on test material used for the study:
Relative density: 1.19

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
The sample was observed to contain agglomerations and lumps of > 2000 μm. Test material was therefore manually sieved (2000 µm).
Result:
10.9% by weight had a particle size of > 2000 μm.
89.1% by weight had a particle size of < 2000 μm; this fraction was used for laser diffraction analysis.


Mass median aerodynamic diameter:
600.355 µm
Geometric standard deviation:
>= 2.166 - <= 2.172
Remarks on result:
other: The MMAD above is the average of 5 runs. GSD was calculated from d50/d15.78. The min. and max. GSD values of 5 runs are provided above. The St.dev. in the table below is the population standard deviation [µm].
Remarks:
Result based on the fraction of the sample which was < 2000 μm.
Key result
Percentile:
D10
Mean:
178.736 µm
St. dev.:
2.376
Key result
Percentile:
D50
Mean:
550.344 µm
St. dev.:
7.873
Key result
Percentile:
D90
Mean:
1 128.075 µm
St. dev.:
19.247
No.:
#1
Size:
< 10 µm
Distribution:
0.82 %
Remarks on result:
other: volume of sample (based on the fraction of the sample which was < 2000 μm)

Conclusion of visual and microscopic evaluation:

- visual observation: coarse to medium powder with some fines and larger solid lumps

- microscope using 3.2 objective lens : irregular shaped crystals; smallest individual particle size was approximately 9 μm and the largest individual size was approximately 864 μm

- microscope using 40 objective lens: single crystalline particles

Laser Diffraction Particle Size Analysis:

Coefficient of variation for D50 is < 3%; D10 and D90 are < 5%. These values are within the acceptable limits mentioned in the ISO 13320 standard.

Conclusions:
Manual sieve analysis showed that 10.9% (w/w) of the substance had a particle size of > 2000 μm and 89.1% (w/w) a particle size of < 2000 μm.
Laser diffraction results for the substance fraction < 2000 µm:
D10 = 178.736 µm, D50 = 550.344 µm and D90 = 1128.075 µm.
0.82% of the sample volume was determined to be < 10 µm.
The MMAD was calculated to be 600.355 µm.

Executive summary:

The particle size distribution of the substance was performed in a GLP study according to ISO 13320 and CIPAC MT 187.

The sample was observed to contain agglomerations and lumps of > 2000 μm. Manual sieve analysis was therefore performed: 10.9% (w/w) of the substance had a particle size of > 2000 μm and 89.1% (w/w) had a particle size of < 2000 μm. The laser diffraction analysis was conducted on the sample fraction < 2000 μm using the small volume wet module. Each result is the average of five runs.

Result for the fraction < 2000 µm: D10 = 178.736 µm, D50 = 550.344 µm and D90 = 1128.075 µm. 0.82% of the sample volume (fraction < 2000 μm) was < 10 µm. The MMAD was calculated to be 600.355 µm.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2018
Report Date:
2018

Materials and methods

Test guideline
Qualifier:
no guideline followed
Principles of method if other than guideline:
The appearance was determined by visual observation (direct and under a microscope). No guideline was followed for the appearance determination but sufficient details were given in the study report.
GLP compliance:
yes (incl. certificate)
Remarks:
certificate issued 13 Jan 2016

Test material

Reference
Name:
Unnamed
Type:
Constituent
Test material form:
solid: particulate/powder
Details on test material:
Physical appearance: white powder
Storage conditions: at room temperature

Results and discussion

Physical state at 20°C and 1013 hPa:
solid
Form / colour / odour
Key result
Form:
solid: particulate/powder
Colour:
White
Odour:
other: not determined
Substance type:
organic

Any other information on results incl. tables

By standard visual inspection, a test substance sample was observed to be a coarse to medium powder with some fines and larger solid lumps.

Based on observation using a 3.2 objective lens, the particles appeared to be irregular shaped crystals.

Based on observation using a 40 objective lens, the sample was observed to be made up of single crystalline particles.

Applicant's summary and conclusion

Conclusions:
The substance is a white powder at room temperature.