[No public or meaningful name is available]

Surface tension

Administrative data

Endpoint:

surface tension

Data waiving:

study scientifically not necessary / other information available

Justification for data waiving:

the study does not need to be conducted because water solubility is below 1 mg/L at 20°C

Cross-reference

Reason / purpose for cross-reference:

data waiving: supporting information

Reference

Endpoint:

transformation / dissolution of metals and inorganic metal compounds

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2017-08-08 to 2017-10-20

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

guideline study

Qualifier:

according to guideline

Guideline:

OECD Series on Testing and Assessment No. 29 (23-Jul-2001): Guidance document on transformation/dissolution of metals and metal compounds in aqueous media

Deviations:

no

GLP compliance:

yes (incl. QA statement)

Remarks:

signed 2016-05-31

Type of method:

flask method

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.341 µg/L

Element analysed:

Al

Loading of aqueous phase:

1 mg/L

Incubation duration:

28 d

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.341 µg/L

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

0.533 µg/L

Element analysed:

Al

Loading of aqueous phase:

1 mg/L

Incubation duration:

28 d

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.161 µg/L

Element analysed:

Al

Loading of aqueous phase:

1 mg/L

Incubation duration:

7 d

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.161 µg/L

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.161 µg/L

Element analysed:

Al

Loading of aqueous phase:

1 mg/L

Incubation duration:

7 d

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.161 µg/L

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.161 µg/L

Element analysed:

Al

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.161 µg/L

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.161 µg/L

Element analysed:

Al

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.161 µg/L

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

0.357 µg/L

Element analysed:

Fe

Loading of aqueous phase:

1 mg/L

Incubation duration:

28 d

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.085 µg/L

Element analysed:

Fe

Loading of aqueous phase:

1 mg/L

Incubation duration:

28 d

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

not determinable

Remarks:

not distinguishable from blank

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

1.34 µg/L

Element analysed:

Fe

Loading of aqueous phase:

1 mg/L

Incubation duration:

7 d

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.035 µg/L

Element analysed:

Fe

Loading of aqueous phase:

1 mg/L

Incubation duration:

7 d

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.035 µg/L

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.035 µg/L

Element analysed:

Fe

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of replicates < LOD: 0.035 µg/L

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.035 µg/L

Element analysed:

Fe

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates < LOD: 0.035 µg/L

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

0.063 µg/L

Element analysed:

Ti

Loading of aqueous phase:

1 mg/L

Incubation duration:

28 d

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.123 µg/L

Element analysed:

Ti

Loading of aqueous phase:

1 mg/L

Incubation duration:

28 d

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates at least < LOQ: 0.123 µg/L

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.123 µg/L

Element analysed:

Ti

Loading of aqueous phase:

1 mg/L

Incubation duration:

7 d

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates at least < LOQ: 0.123 µg/L

Key result

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

< 0.123 µg/L

Element analysed:

Ti

Loading of aqueous phase:

1 mg/L

Incubation duration:

7 d

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Remarks on result:

other:

Remarks:

conc. of all replicates at least < LOQ: 0.123 µg/L

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

0.103 µg/L

Element analysed:

Ti

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH = 6, separation of solid phase by filtration 0.2 µm

Type of test:

full transformation/dissolution test - metals and sparingly soluble metal compounds

Mean dissolved conc.:

0.04 µg/L

Element analysed:

Ti

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH = 8, separation of solid phase by filtration 0.2 µm

Details on results:

Solution pH, oxygen concentrations, temperature
The temperature of the thermostatically controlled room was recorded with a data logger. The mean temperature was 21.3 ± 0.3 °C. The solution pH remained relatively constant for the pH 6 treatment for the method blank vessels (6.15 – 6.37) as for the sample vessels (5.93 – 6.37).
Oxygen levels in all test vessels pH 6 were in the range recommended by the OECD Test Guidance 29 during the test: above 70 % of oxygen saturation at 8.5 mg/L (70 % of 8.5 mg/L = 6 mg/L). The solution pH for the pH 8 treatment showed a decrease of the pH during the test in the method blanks as well as in the sample vessels. In the test item vessels the pH was in the range of 7.64 – 7.93 and in method blank vessels the pH was in the range of 7.66 – 7.84. Oxygen levels in all test vessels pH 8 were in the range recommended by the OECD Test Guidance 29 during the test: above 70 % of oxygen saturation at 8.5 mg/L (70 % of 8.5 mg/L = 6 mg/L)

Analytical measurements: Within and between vessel variations of elemental concentrations (Fe, Ti, Al)
Within and between vessel variations are not always in compliance with the guidance for the tests. For these samples the observed variations of > 20 % (between-vessel) or > 10 % (within-vessel) are probably due to the low dissolution and the majority of measurements being close to – or below – the respective quantification limit of the method

Method validation summary (ICP-OES)

Limits of detection (LODs), limits of quantification (LOQs) and correlation coefficients (r)

Limits of detection (LOD) within all measurement series: 0.161 -0.341 μg Al / L, 0.035 - 0.085 µg / L Fe

Limits of quantification (LOQ) within all measurement series: 0.482 - 1.02 μg Al / L, 0.106 - 0.255 µg / L Fe

Correlation coefficients (r) within all measurement series: > 0.999926 (Al calibration), > 0.999868 (Fe calibration)

Mean recovery of fortified samples (concentration range 6 - 160 µg, n > 5): 95,2 - 119 % (Al fortification), 95 - 108 % (Fe fortification)

Mean recovery for certified reference material TMDA-52.4 (lot no. 0615, Environment Canada): 99.9 - 104 % (Al measurement, n = 15), 98.4 - 103 % (Fe measurement, n = 13)

date	Chosen wavelength [nm]	LOD (µg/L)	LOQ (µg/L)	correlation coefficient	Sum of quality assurance samples	Recovery of quality assurance samples [%]
August 17, 2017; measurement of test samples (24 h and 7 d) and method blank samples (24 h and 7 d) – pH 6 and 8	Al: 167.019* Fe: 238.204*	Al: 0.161 Fe: 0.035	Al: 0.482 Fe: 0.106	Al: 0.999926 Fe: 0.999868	Al: 17 Fe: 17	Al: 88.2 Fe: 88.2

date	Chosen wavelength [nm]	LOD (µg/L)	LOQ (µg/L)	correlation coefficient	Sum of quality assurance samples	Recovery of quality assurance samples [%]
September 29, 2017; measurement of test samples (28 d) and method blank samples (28 d)	Al: 167.019* Fe: 238.204*	Al: 0.341 Fe: 0.085	Al: 1.02 Fe: 0.255	Al: 0.999974 Fe: 0.999940	Al: 26 Fe: 26	Al: 88.5 Fe: 92.3

date	Chosen wavelength [nm]	LOD (µg/L)	LOQ (µg/L)	correlation coefficient	Sum of quality assurance samples	Recovery of quality assurance samples [%]
October 20, 2017; measurement of mass balance samples – filters and test vessels pH 6 and 8	Al: 394.401* Fe: 260.709* Ti: 307.866*	Al: 2.16 Fe: 0.300 Ti: 0.149	Al: 6.48 Fe: 0.900 Ti: 0.448	Al: 0.999942 Fe: 0.999965 Ti: 0.999923	Al: 21 Fe: 21 Ti: 21	Al: 81.0 Fe: 95.5 Ti: 100

Method validation summary (ICP-MS)

Limits of detection (LODs), limits of quantification (LOQs) and correlation coefficients (r)

Limits of detection (LOD) within all measurement series: 0.041 μg Ti / L.

Limits of quantification (LOQ) within all measurement series: 0.123 μg Ti / L.

Correlation coefficients (r) within all measurement series: > 0.9997

Recovery of fortified samples (n = 4): 106 -110 %

Mean recovery of certified reference material TMDA-52.4 (lot no. 0615, Environment Canada): 102% (n=5)

Conclusions:

The transformation/dissolution test (OECD Series on Testing and Assessment Number 29, 2001) of "Titanium, iron and aluminium pseudobrookite and rutile (Pigment Black 12)" at a loading of 1 mg/L at pH 6 and 8, performed for 28d, resulted in maximum quantified Al concentrations of 0.533 µg/L (pH = 8, 28d), maximum Fe concentrations of 0.357 µg/L (pH = 6, 28d) als well as maximum Ti concentrations of 0.063 µg/L (pH = 6, 28d). Thus, the extent to which "Pigment Titanium, iron and aluminium pseudobrookite and rutile (Pigment Black 12)" can produce soluble available ionic and other metal-bearing species in aqueous media is limited.