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Physical & Chemical properties

Particle size distribution (Granulometry)

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Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2020
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
study well documented, meets generally accepted scientific principles, acceptable for assessment
Principles of method if other than guideline:
TEM images of nanoparticles and measuring the width (the short side) and the length (the long side) with MOUNTECH, Mac-View Ver. 4
Type of method:
microscopic examination
Remarks:
TEM images
Type of particle tested:
primary particle
Type of distribution:
counted distribution
Percentile:
D10
Mean:
>= 25 - <= 31 nm
Remarks on result:
other: Standard deviation not provided
Percentile:
D50
Mean:
>= 46 - <= 48 nm
Remarks on result:
other: Standard deviation not provided
Percentile:
D90
Mean:
>= 70 - <= 79 nm
Remarks on result:
other: Standard deviation not provided

We drew the minimum bounding rectangle on each particle of the test material in the TEM images, measured the width (the short side) and the length (the long side) with MOUNTECH, Mac-View Ver. 4 (herein, treat the width as the length of the shortest dimension, and the length as the length of the longest dimension, respectively), and calculated the length/width ratio as the aspect ratio.The number based size distribution is plotted. The d10, d50, and d90 were 25-31, 46-48, and 70-79 nm, respectively.

Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
14 June 2011
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: see 'Remark'
Remarks:
According to appendix R7-1 of ECHA Guidance on Information Requirements and Chemical Safety Assessment multiple techniques should be applied to investigate phys. chem. properties of particulates, although different measurement methods may not provide comparable results. Laser diffraction is the well experienced standard procedure for pigments to determine particle size distribution of the pigment as it is manufactured and delivered.
Qualifier:
according to guideline
Guideline:
other: ISO 13320-1
Principles of method if other than guideline:
Particle size determination by laser diffraction
Type of method:
Laser scattering/diffraction
Type of distribution:
volumetric distribution
Percentile:
D10
Mean:
1 µm
St. dev.:
0.05
Percentile:
D50
Mean:
5.6 µm
St. dev.:
0.7
Percentile:
D90
Mean:
16.2 µm
St. dev.:
3.1

For further percentiles see attached report.


Given standard deviation is based on the general experience with the method and pigments. The estimated values are typical standard deviations for pigments:


D10: 4% of D10 (minimum value 0.05 µm)


D50: 13% of D50 (minimum value 0.1 µm)


D90: 29% of D90 - D50

Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
2012
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: see 'Remark'
Remarks:
According to appendix R7-1 of ECHA Guidance on Information Requirements and Chemical Safety Assessment multiple techniques should be applied to investigate phys. chem. properties of particulates, although different measurement methods may not provide comparable results. Specific surface area by BET measurement complements the results of laser diffraction, which is the standard procedure for pigments to determine particle size distribution of the pigment as it is manufactured and delivered.
Qualifier:
according to guideline
Guideline:
other: DIN 66132
Type of distribution:
other: BET - specific surface area
Percentile:
D50
Remarks on result:
other: No source field for Standard deviation.

Based on the variables weighted sample, differential pressure and charging pressure the specific surface area is calculated using the single-point evaluation of the BET-equation:

BET surface area: 37.6 m2/g

Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
2012
Reliability:
2 (reliable with restrictions)
Rationale for reliability incl. deficiencies:
other: see 'Remark'
Remarks:
According to appendix R7-1 of ECHA Guidance on Information Requirements and Chemical Safety Assessment multiple techniques should be applied to investigate phys. chem. properties of particulates, although different measurement methods may not provide comparable results. TEM images complement the results of laser diffraction, which is the standard procedure to determine particle size distribution of the pigment as it is manufactured and delivered. TEM in addition enables qualitative assessment of size, shape and agglomeration of particles.
Qualifier:
according to guideline
Guideline:
other: company guideline
Type of distribution:
other: TEM - image
Percentile:
D50
Remarks on result:
other: Due to the significant agglomeration quantitative determination of size distribution of primary particles is not possible.

Images with different magnifications were taken.

TEM images indicate, that the test substance mainly consists of aggregates and/or agglomerates. Due to the significant agglomeration quantitative determination of size distribution of primary particles is not possible. Therefore manual statistical evaluation of the TEM images was not performed.

Description of key information

The number based size distribution of primary particle is plotted. The d10, d50, and d90 were 25-31, 46-48, and 70-79 nm, respectively.

In addition in the past, the particle size determinations of the aggregates/agglomaerates by laser diffraction have been performed, which are now used as supporting information only:

D10: mean value 1.0 µm

D50: mean value 5.6 µm

D90: mean value 16.2 µm

Additional information