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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.

Data source

Materials and methods

Results and discussion

Applicant's summary and conclusion