Registration Dossier

Administrative data

Endpoint:
appearance / physical state / colour
Type of information:
experimental study
Adequacy of study:
key study
Study period:
20/12/2018
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 for cross-reference:
reference to other study
Reference
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
20/12/2018 - 14/02/2019
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
test procedure in accordance with generally accepted scientific standards and described in sufficient detail
Reason / purpose for cross-reference:
reference to other study
Qualifier:
according to guideline
Guideline:
ISO 13320 (Particle size analysis - Laser diffraction methods)
Version / remarks:
2009
Qualifier:
according to guideline
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/FibreLength 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. QA statement)
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: 1.09 (see Cross-reference)

TREATMENT OF TEST MATERIAL PRIOR TO TESTING
The sample was observed to contain agglomerations and lumps of > 3500 μm. Test material was therefore manually sieved (3500 µm). Result:
66% by weight had a particle size of > 3500 μm.
34% by weight had a particle size of < 3500 μm; this fraction was used for laser diffraction analysis.
Mass median aerodynamic diameter:
439 µm
Geometric standard deviation:
2.105
Remarks on result:
other: MMAD and GSD above are both the average of 5 runs. GSD was calculated from d50/d15.78. The St.dev. in the table below is the population standard deviation [µm].
Key result
Percentile:
D10
Mean:
146 µm
St. dev.:
1.86
Key result
Percentile:
D50
Mean:
420 µm
St. dev.:
6.33
Key result
Percentile:
D90
Mean:
799 µm
St. dev.:
19.8
No.:
#1
Size:
< 10 µm
Distribution:
0 other: vol%

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 66% (w/w) of the substance had a particle size of > 3500 μm and 34% (w/w) a particle size of < 3500 μm.
Laser diffraction results for the substance fraction < 3500 µm:
D10= 146 µm, D50= 420 µm and D90= 799 µm. The MMAD was calculated to be 439 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 lumps and clusters. Manual sieve analysis was therefore performed: 66% (w/w) of the substance had a particle size of > 3500 μm and 34% (w/w) had a particle size of < 3500 μm. The laser diffraction analysis was conducted on the sample fraction < 3500 μm using the dry powder module. Each result is the average of five runs. Result for the fraction < 3500 µm:

D10= 146 µm, D50= 420 µm and D90= 799 µm. The MMAD was calculated to be 439 µm.

Data source

Reference
Reference Type:
study report
Title:
Unnamed
Year:
2019
Report date:
2019

Materials and methods

Test guideline
Qualifier:
no guideline followed
Principles of method if other than guideline:
Appearance was determined by visual observation.
GLP compliance:
yes (incl. QA statement)

Test material

Constituent 1
Chemical structure
Reference substance name:
Reaction mass of (S)-2-[(R)-2-Oxo-4-propyl-1-pyrrolidinyl]butyramide and (S)-2-[(S)-2-Oxo-4-propyl-1-pyrrolidinyl]butyramide
Cas Number:
943986-70-7
Molecular formula:
C11H20N2O2
IUPAC Name:
Reaction mass of (S)-2-[(R)-2-Oxo-4-propyl-1-pyrrolidinyl]butyramide and (S)-2-[(S)-2-Oxo-4-propyl-1-pyrrolidinyl]butyramide
Test material form:
solid
Details on test material:
- Appearance: Off-white solid
- Storage condition of test material: At room temperature protected from light

Results and discussion

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

Applicant's summary and conclusion

Conclusions:
The substance is an off-white solid.

Executive summary:

The substance was observed to be an off-white solid.