Ruthenium

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: ISO 9277:2010(E)

Qualifier:

according to guideline

Guideline:

other: AA_LP_814_BET_08

Qualifier:

according to guideline

Guideline:

other: ISO 14488:2007(E)

Qualifier:

according to guideline

Guideline:

other: ISO 13320:2009(E)

Qualifier:

according to guideline

Guideline:

other: SAA_Troken_DISP, SAA LB2000

GLP compliance:

no

Type of method:

Laser scattering/diffraction

Type of particle tested:

primary particle

Type of distribution:

volumetric distribution

Percentile:

D10

Mean:

0.126 µm

Remarks on result:

other: Range; 0.125 - 0.127 µm

Percentile:

D50

Mean:

2.3 µm

Remarks on result:

other: Range; 2.3 µm

Percentile:

D90

Mean:

8.7 µm

Remarks on result:

other: Range; 8.7 - 8.8 µm

Mean specific surface area N-BET = 23.6  ± 0.1 m²/g. Range = 23.5 ± 0.02 to 23.6 ± 0.03 m²/g.

Table 1: N-BET analysis data and percentiles calculated from the particle size distribution for ruthenium black

	Analysis 1	Analysis 2	Analysis 3	Average
Specific surface area N-BET (m^2/g)	23.6 ± 0.03	23.5 ± 0.02		23.6 ± 0.1
X10;3 (μm)	0.125	0.127	0.126	0.126
X50;3 (μm)	2.3	2.3	2.3	2.3
X90;3 (μm)	8.7	8.7	8.8	8.7

Conclusions:

The average 10th, 50th and 90th percentile particle sizes for ruthenium black were 0.126, 2.3 and 8.7 μm, respectively. The average specific surface area was determined as 23.6 ± 0.1 m2/g.

Executive summary:

Potthoff (2012) is a non-GLP study but follows a standard method and is considered suitable for use as the key study for this endpoint. The average 10th, 50th and 90th percentile particle sizes for ruthenium black are 0.126, 2.3 and 8.7 μm, respectively. The average specific surface area was determined as 23.6 ± 0.1 m2/g.

Reference 2

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

other: ISO 9277:2010(E)

Qualifier:

according to guideline

Guideline:

other: AA_LP_814_BET_08

Qualifier:

according to guideline

Guideline:

other: ISO 14488:2007(E)

Qualifier:

according to guideline

Guideline:

other: ISO 13320:2009(E)

Qualifier:

according to guideline

Guideline:

other: SAA_Troken_DISP, SAA LB2000

GLP compliance:

no

Type of method:

Laser scattering/diffraction

Type of particle tested:

primary particle

Type of distribution:

volumetric distribution

Percentile:

D10

Mean:

1.85 µm

Remarks on result:

other: Range; 1.85 - 1.86 µm

Percentile:

D50

Mean:

6.1 µm

Remarks on result:

other: Range; 6.1 µm

Percentile:

D90

Mean:

17.9 µm

Remarks on result:

other: Range; 17.8 - 18.0 µm

Mean specific surface area N-BET = 0.44  ± 0.02 m²/g. Range = 0.431 ± 0.001 to 0.459 ± 0.002 m²/g.

Table 1: N-BET analysis data and percentiles calculated from the particle size distribution for ruthenium powder

	Analysis 1	Analysis 2	Analysis 3	Average
Specific surface area N-BET (m^2/g)	0.431 +- 0.001	0.459 +- 0.002		0.44 +- 0.02
X10;3 (μm)	1.85	1.86	1.85	1.85
X50;3 (μm)	6.1	6.1	6.1	6.1
X90;3 (μm)	17.8	18.0	17.9	17.9

Conclusions:

The average 10th, 50th and 90th percentile particle sizes for ruthenium powder were 1.85, 6.1 and 17.9 μm, respectively. The average specific surface area was determined as 0.44 ± 0.02 m2/g.

Executive summary:

Potthoff (2012) is a non-GLP study but follows a standard method and is considered suitable for use as the key study for this endpoint. The average 10th, 50th and 90th percentile particle sizes for ruthenium powder were 1.85, 6.1 and 17.9 μm, respectively. The average specific surface area was determined as 0.44 ± 0.02 m2/g.

Reference 3

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

supporting study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Non-GLP, guideline study, well reported, reliable without restrictions

Qualifier:

according to guideline

Guideline:

DIN 55992-1 (Determination of a parameter for the dust formation of pigments and extenders - Part 1: Rotation method)

Deviations:

no

GLP compliance:

no

Type of method:

rotating drum method

Remarks:

modified Heubach procedure

Type of particle tested:

other: dust particles

Type of distribution:

mass based distribution

Mass median aerodynamic diameter:

21.7 µm

Geometric standard deviation:

2.8

Experimental results

Quantity of substance used [g]: 1

Total dust mass in impactor [mg]: 401.12

Dust concentration in impactor [mg/m³]: 1996.05

Total dustiness [mg/g]: 401.12

Inhalable fraction [mg/g]: 265.11

Thoracic fraction [mg/g]: 119.36

Respirable fraction [mg/g]: 33.36

Mass Median Aerodynamic Diameter (MMAD) [μm]: 21.7

Geometric Standard Deviation (GSD) [μm]: 2.8

Conclusions:

The total dustiness of Ruthenium black was determined to be 401.12 mg/g. The inhalable fraction was 265.11 mg/g, the thoracic fraction was 265.11 mg/g and the respirable fraction was 33.36 mg/g. The Mass Median Aerodynamic Diameter (MMAD) was determined to be 21.7 μm with a geometric standard deviation of 2.8 μm.

Executive summary:

The dustiness of Ruthenium black was tested in a modified Heubach procedure according to the guideline DIN 55992-1:2006 'Determination of a parameter for the dust formation of pigments and extenders - Part 1: Rotation method'. The substance was mechanically stressed in a rotating drum and the airborne dust was fed into a seven-stage cascade impactor. The dust masses collected at each cascade stage were weighed to determine total dustiness. Dust from 1.00 g of sample was generated for 5 min at a temperature of 22.3 ºC, 35.4 % relative humidity and 1014.0 hPa atmosphere. The dustiness values in accordance with DIN EN 481 were calculated from the particle size distribution determined (cumulative frequency distribution) with the help of an excel macro. The study is non-GLP, but follows a standard guideline and is considered to be reliable. The total dustiness of Ruthenium black was determined to be 401.12 mg/g. The inhalable fraction was 265.11 mg/g, the thoracic fraction was 119.36 mg/g and the respirable fraction was 33.36 mg/g. The Mass Median Aerodynamic Diameter (MMAD) was determined to be 21.7 μm with a geometric standard deviation of 2.8 μm.

Reference 4

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

supporting study

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Remarks:

Non-GLP, guideline study, well reported, reliable without restrictions

Qualifier:

according to guideline

Guideline:

DIN 55992-1 (Determination of a parameter for the dust formation of pigments and extenders - Part 1: Rotation method)

Deviations:

no

GLP compliance:

no

Type of method:

rotating drum method

Remarks:

modified Heubach procedure

Type of particle tested:

other: dust particles

Type of distribution:

mass based distribution

Mass median aerodynamic diameter:

20.1 µm

Geometric standard deviation:

2.8

Experimental results

Quantity of substance used [g]: 1

Total dust mass in impactor [mg]: 48.48

Dust concentration in impactor [mg/m³]: 241.08

Total dustiness [mg/g]: 48.48

Inhalable fraction [mg/g]: 32.80

Thoracic fraction [mg/g]: 16.60

Respirable fraction [mg/g]: 5.32

Mass Median Aerodynamic Diameter (MMAD) [μm]: 20.1

Geometric Standard Deviation (GSD) [μm]: 2.8

Conclusions:

The total dustiness of Ruthenium powder was determined to be 48.48 mg/g. The inhalable fraction was 32.8 mg/g, the thoracic fraction was 16.60 mg/g and the respirable fraction was 5.32 mg/g. The Mass Median Aerodynamic Diameter (MMAD) was determined to be 20.1 μm with a geometric standard deviation of 2.8 μm.

Executive summary:

The dustiness of Ruthenium powder was tested in a modified Heubach procedure according to the guideline DIN 55992-1:2006 'Determination of a parameter for the dust formation of pigments and extenders - Part 1: Rotation method'. The substance was mechanically stressed in a rotating drum and the airborne dust was fed into a seven-stage cascade impactor. The dust masses collected at each cascade stage were weighed to determine total dustiness. Dust from 1.00 g of sample was generated for 5 min at a temperature of 22.7 ºC, 28.7 % relative humidity and 1018.0 hPa atmosphere. The dustiness values in accordance with DIN EN 481 were calculated from the particle size distribution determined (cumulative frequency distribution) with the help of an excel macro. The study is non-GLP, but follows a standard guideline and is considered to be reliable. The total dustiness of Ruthenium powder was determined to be 48.48 mg/g. The inhalable fraction was 32.8 mg/g, the thoracic fraction was 16.6 mg/g and the respirable fraction was 5.32 mg/g. The Mass Median Aerodynamic Diameter (MMAD) was determined to be 20.1 μm with a geometric standard deviation of 2.8 μm.

Reference 5

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

1 November 2010

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)

Version / remarks:

Screening Test

Principles of method if other than guideline:

The method used is based on a procedure designed to comply with that given in 'Particle size distribution, fibre length and diameter distribution', June 1996 European Commission technical guidance document, which satisfies the requirements of OECD Guideline 110

GLP compliance:

yes (incl. QA statement)

Type of method:

sieving

Type of particle tested:

primary particle

Type of distribution:

mass based distribution

No.:

#1

Size:

< 100 µm

Distribution:

83.5 %

The results of the sieving procedure are shown below:

Measurement	Result
Mass of test item transferred to sieve	10.03g
Mass of test item passed through sieve	8.37g
Proportion of test item <100µm	83.5%

Conclusions:

The proportion of ruthenium <100 μm was 83.5%.

Executive summary:

Tremain and Atwal (2011) is a GLP compliant study following OECD guideline 110 (Screening method) and is considered suitable for use as a supporting study for this endpoint. The proportion of ruthenium <100 μm is 83.5%.

Reference 6

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

Not reported

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:

Ultrasonic: 60 s(+M), Concentration: 245

GLP compliance:

not specified

Type of method:

other: ultrasonic shaking

Percentile:

D50

Mean:

5.47 µm

Percentile:

D10

Mean:

1.25 µm

Percentile:

D90

Mean:

15.59 µm

10% diameter = 1.25µm. 50% diameter = 5.47µm. 90% diameter = 15.59µm

Conclusions:

The 10th, 50th and 90th percentile particle sizes for ruthenium are 1.25 µm, 5.47 µm and 15.59 µm, respectively.

Executive summary:

This study is considered to be suitable for use as a supporting study for this endpoint. The 10^th, 50^thand 90^th percentile particle sizes for ruthenium are 1.25 µm, 5.47 µm and 15.59 µm, respectively.

Description of key information

 The average 10th, 50th and 90th percentile particle sizes for ruthenium powder were 1.85, 6.1 and 17.9 μm, respectively. The average specific surface area was determined as 0.44 ± 0.02 m2/g. The average 10th, 50th and 90th percentile particle sizes for ruthenium black are 0.126, 2.3 and 8.7 μm, respectively. The average specific surface area was determined as 23.6 ± 0.1 m2/g.

Additional information

Particle size distribution and specific surface area were assessed for both ruthenium powder and ruthenium black. Potthoff (2012) is a non-GLP study but follows standard methods. Particle size was assessed by laserlight diffraction following dry dispersion and specific surface area was assessed by N-BET. This study is considered suitable for use as the key study for this endpoint. The average 10th, 50th and 90th percentile particle sizes for ruthenium powder were 1.85, 6.1 and 17.9 μm, respectively. The average specific surface area was determined as 0.44 ± 0.02 m2/g. The average 10th, 50th and 90th percentile particle sizes for ruthenium black are 0.126, 2.3 and 8.7 μm, respectively. The average specific surface area was determined as 23.6 ± 0.1 m2/g.

A screening study is available that used a sieving method to assess the particle size of ruthenium powder. Tremain and Atwal (2011) is a GLP compliant study following OECD guideline 110 (Screening method) and is considered suitable for use as a supporting study for this endpoint. The proportion of ruthenium <100 μm is 83.5%.

A second supporting study is also available (CILAS 2006). Although limited details are available, the study used a standard method and is considered to be reliable with restrictions. The 10th, 50^thand 90^th percentile particle sizes for ruthenium are 1.25 µm, 5.47 µm and 15.59 µm, respectively.

The dustiness of ruthenium powder and ruthenium black was tested in a modified Heubach procedure according to the guideline DIN 55992-1:2006 (Selck and Parr 2012). The studies are non-GLP, but follow a standard guideline and are considered to be reliable. The total dustiness of ruthenium powder was determined to be 48.48 mg/g. The inhalable fraction was 32.8 mg/g, the thoracic fraction was 16.6 mg/g and the respirable fraction was 5.32 mg/g. The Mass Median Aerodynamic Diameter (MMAD) was determined to be 20.1 μm with a geometric standard deviation of 2.8 μm. The total dustiness of ruthenium black was determined to be 401.12 mg/g. The inhalable fraction was 265.11 mg/g, the thoracic fraction was 119.36 mg/g and the respirable fraction was 33.36 mg/g. The Mass Median Aerodynamic Diameter (MMAD) was determined to be 21.7 μm with a geometric standard deviation of 2.8 μm.