N,N,N-tributylbutan-1-aminium ({[(2S,5R)-2-carbamoyl-7-oxo-1,6-diazabicyclo[3.2.1]oct-6-yl]oxy}sulfonyl)oxidanide

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

From 21 January 2016 to 17 February 2016.

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

test procedure in accordance with generally accepted scientific standards and described in sufficient detail

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2016

Report date:

2016

Materials and methods

Test guideline

Test guideline 1

Qualifier:

according to guideline

Guideline:

other: ISO 13320:2009

Test guideline 2

Qualifier:

according to guideline

Guideline:

other: CIPAC MT 187

Principles of method if other than guideline:

According to REACH Regulation (EC) No 1907/2006 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 the relevant Regulation (EC) No 440/2008. The international OECD 110 test guideline ‘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 document ‘Guidance on information requirements and Chemical SafetyAssessment-Chapter R.7a: Endpoint specific guidance’ stipulates that many methods are available for particle size measurements but none of them is applicable to the entire size range. ECHA’s guidance mentions the Laser scattering/diffraction as a method suitable for particles of all kind and makes reference to ISO 13320:2009.

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

GLP compliance:

yes (incl. QA statement)

Type of method:

Laser scattering/diffraction

Type of particle tested:

primary particle

Type of distribution:

volumetric distribution

Test material

Test material information

Constituent 1

Reference substance name:

N,N,N-tributylbutan-1-aminium ({[(2S,5R)-2-carbamoyl-7-oxo-1,6-diazabicyclo[3.2.1]oct-6-yl]oxy}sulfonyl)oxidanide

EC Number:

812-038-2

Cas Number:

1192651-80-1

Molecular formula:

C23 H46 N4 O6 S

IUPAC Name:

N,N,N-tributylbutan-1-aminium ({[(2S,5R)-2-carbamoyl-7-oxo-1,6-diazabicyclo[3.2.1]oct-6-yl]oxy}sulfonyl)oxidanide

Test material form:

solid

Details on test material:

- Name of test material (as cited in study report): SAM-3
- Lot/batch No.: SAM-3/660-137/K1
- Material number: P60689-51
- Storage conditions: ambient temperature, dry, well ventilated area protected from sunlight.

Specific details on test material used for the study:

- Relative density at 20°C: 1.12 (see endpoint 4.4)
- Tested as received

Results and discussion

Mass median aerodynamic diameter:

166.763 µm

Geometric standard deviation:

>= 4.883 - <= 5.068

Particle size

Particle size 1

Key result

Percentile:

D10

Mean:

17.305 µm

St. dev.:

0.367

Remarks on result:

other: population standard deviation [µm]

Particle size 2

Key result

Percentile:

D50

Mean:

157.576 µm

St. dev.:

2.293

Remarks on result:

other: population standard deviation [µm]

Particle size 3

Key result

Percentile:

D90

Mean:

427.977 µm

St. dev.:

8.53

Remarks on result:

other: population standard deviation [µm]

Any other information on results incl. tables

-6.03% by volume was seen to be < 10.00 µm.

-Population standard dev. (MMAD)= 2.43 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 standard.

Applicant's summary and conclusion

Conclusions:

In a GLP-compliant study in accordance with ISO 13320 and CIPAC MT 187 using laser diffraction analysis (dry powder module), the particle size distribution of the substance was determined: 6.0% < 10.00 µm, 10% < 17.3 µm, 50% < 158 µm and 90% < 428 µm. MMAD= 167 µm.