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Reference
Endpoint:
transformation / dissolution of metals and inorganic metal compounds
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2017-08-07 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.:
0.355 µg/L
Element analysed:
Cr
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.:
0.314 µg/L
Element analysed:
Cr
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.:
4.42 µg/L
Element analysed:
Cr
Loading of aqueous phase:
100 mg/L
Incubation duration:
7 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.:
0.229 µg/L
Element analysed:
Cr
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.:
0.2 µg/L
Element analysed:
Cr
Loading of aqueous phase:
1 mg/L
Incubation duration:
7 d
Test conditions:
pH = 8, 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.:
4.17 µg/L
Element analysed:
Cr
Loading of aqueous phase:
100 mg/L
Incubation duration:
24 h
Test conditions:
pH = 8, 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.:
0.079 µg/L
Element analysed:
Cr
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.:
0.111 µg/L
Element analysed:
Cr
Loading of aqueous phase:
1 mg/L
Incubation duration:
24 h
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.:
0.532 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.:
0.136 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
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
< 0.463 µg/L
Element analysed:
Fe
Loading of aqueous phase:
100 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: 0.463 µg/L
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 = 6, 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.:
< 0.085 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: 0.085 µg/L
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
< 0.463 µg/L
Element analysed:
Fe
Loading of aqueous phase:
100 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: 0.463 µg/L
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
0.123 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
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
0.273 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
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 = 6, separation of solid phase by filtration 0.2 µm
Remarks on result:
other:
Remarks:
conc. of all replicates < LOD / LOQ: 0.041 µg/L / 0.123 µg/L
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
0.022 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
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
< 0.042 µg/L
Element analysed:
Ti
Loading of aqueous phase:
100 mg/L
Incubation duration:
7 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.:
< 0.041 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 < LOD: 0.041 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.:
< 0.042 µg/L
Element analysed:
Ti
Loading of aqueous phase:
100 mg/L
Incubation duration:
24 h
Test conditions:
pH = 8, separation of solid phase by filtration 0.2 µm
Remarks on result:
not determinable
Remarks:
not distinguishable from blank
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:
24 h
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
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:
24 h
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.:
3.52 µg/L
Element analysed:
Zn
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.:
4.78 µg/L
Element analysed:
Zn
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.:
23.3 µg/L
Element analysed:
Zn
Loading of aqueous phase:
100 mg/L
Incubation duration:
7 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.:
0.929 µg/L
Element analysed:
Zn
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.:
3.68 µg/L
Element analysed:
Zn
Loading of aqueous phase:
1 mg/L
Incubation duration:
7 d
Test conditions:
pH = 8, 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.:
20.5 µg/L
Element analysed:
Zn
Loading of aqueous phase:
100 mg/L
Incubation duration:
24 h
Test conditions:
pH = 8, 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.:
< 0.052 µg/L
Element analysed:
Zn
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:
not determinable
Remarks:
not distinguishable from blank
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
2.17 µg/L
Element analysed:
Zn
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:
Background correction:
All data presented are corrected for background when possible, i.e., when measured Cr, Fe, Zn or Ti concentrations in blanks >LOQ.

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 and 21.2 ± 0.3 °C for the additional test with 100 mg loading pH=8. 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 (5.83 – 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 of the pH 8 remained relatively constant during the test in the method blanks (7.83 – 7.98) as well as in the sample vessels (7.78 – 7.97) for both the 1 mg loading and the 100 mg loading experiment. 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 (Cr, Fe, Zn, Ti)
Within and between vessel variations are not always in compliance with the guidance for the tests. The particle size distribution of each loading replicate may differ and thus resulting in different overall total surface areas per vessel. For these samples the observed variations of > 20 % (between-vessel) or > 10 % (within-vessel) were mainly in the recommended range for Cr and Zn pH 6. For iron (both pHs), Ti (both pHs) and Zn (pH 8, mainly only the between-vessel variation) variations were not in the recommended range, 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: 0.049 -0.052 μg Zn / L, 0.035 - 0.085 µg / L Fe

Limit of detection (LOD) for measurements of 100 mg/L loading test: 0.215 µg Zn / L, 0.463 µg Fe / L

Limits of quantification (LOQ) within all measurement series: 0.148 - 0.156 μg Zn / L, 0.106 - 0.255 µg / L Fe

Limit of quantification (LOQ) for measurements of 100 mg/L loading test: 0.645 μg Zn / L, 1.39 µg / L Fe

Correlation coefficients (r) within all measurement series: > 0.999865 (Zn calibration), > 0.999868 (Fe calibration)

Mean recovery of fortified samples (concentration range 25 - 300 µg, n = 8): 97.1 - 106 % (Fe fortification), 102 - 109 % (Zn fortification)

Mean recovery for certified reference material TMDA-52.4 (lot no. 0615, Environment Canada): 99.5 - 103 % (Fe measurement, n = 14), 101 - 104 % (Zn measurement, n = 14)

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) – only pH 6

Fe: 238.204* Zn: 213.857*

Fe: 0.035

Zn: 0.052

Fe: 0.106

Zn: 0.155

Fe: 0.999868

Zn: 0.999865

Fe: 17

Zn:17

Fe: 88.2

Zn: 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) pH 6; pH 8 all test samples and method blank samples(24 h, 7d and 28 d)

Fe: 238.204*

Zn: 213.857*

Fe: 0.085

Zn: 0.049

Fe: 0.255

Zn: 0.148

Fe: 0.999940

Zn: 0.999960

Fe: 28

Zn: 28

Fe: 92.9

Zn: 85.7

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: 0.008 - 0.041 μg Ti / L ; 0.005 - 0.006 µg Cr / L

Limit of detection (LOD) for measurements of 100 mg/L loading test: 0.042 µg Ti / L, 0.003 µg Cr / L

Limits of quantification (LOQ) within all measurement series: 0.023 - 0.123 μg Ti / L; 0.016 - 0.018 µg Cr / L

Limit of quantification (LOQ) for measurements of 100 mg/L loading test: 0.126 μg Ti / L, 0.01 µg / L Cr

Correlation coefficients (r) within all measurement series: > 0.9988

Mean recovery of fortified samples (n = 4): 97.4 - 103 % (Cr), 99.1 - 106 % (Ti)

Mean recovery of certified reference material TMDA-52.4 (lot no. 0615, Environment Canada): 105 - 106 % (n=11, Ti), 103 -105 % (n=11, Cr)

Mean recovery of certified reference material TM-26.4 (lot no. 1115, Environment Canada) for measurements of 100 mg/L loading test: 94.4 % (n=4, Ti), 111 % (n=4, Cr)

date

Chosen isotope and gas mode

LOD
[µg/L]

LOQ
[µg/L]

correlation coefficient

Sum of quality assurance samples

Recovery of quality assurance samples [%]

September 12, 2017; measurement of test samples (all sampling times) and method blank samples (all sampling times) – only pH 6; pH 8 only sampling points 24 h and 7 d

Cr:52Cr* [Helium gas mode]

Ti:47Ti* [Helium gas mode]

Cr: 0.005

Ti: 0.041

Cr: 0.016

Ti: 0.123

Cr: 0.9996

Ti: 0.9997

Cr: 47

Ti: 47

Cr: 97.9

Ti: 97.9

date

Chosen isotope and gas mode

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) – only pH 8

Cr:52Cr* [HiHelium gas mode]

Ti:47Ti [HiHelium gas mode]

Cr: 0.006

Ti: 0.008

Cr: 0.018

Ti: 0.023

Cr: 0.9988

Ti: 0.9988

Cr: 7

Ti: 7

Cr: 100

Ti: 100

Conclusions:
The transformation/dissolution test (OECD Series on Testing and Assessment Number 29, 2001) of inorganic pigment "Chromium, iron, titanium and zinc spinel and rutile" at a loading of 1 mg/L at pH 6 and 8, performed for 28d, resulted in maximum quantified Cr concentrations of 0.355 µg/L (pH = 6, 28d), maximum Fe concentrations of 0.532 µg/L (pH = 6, 28d), maximum Zn concentrations of 4.78 µg/L (pH = 8, 28d) as well as maximum Ti concentrations of 0.022 µg/L (background corrected, pH = 8, 28d). Thus, the extent to which "Chromium, iron, titanium and zinc spinel and rutile" can produce soluble available ionic and other metal-bearing species in aqueous media is limited. An additional test at pH 8 with 100 mg/L loading for 7 days revealed maximum soluble concentrations of 4.42 µg/L Cr, 23.3 µg/L Zn, < 0.463 µg/L Fe and < 0.042 µg/L Ti.

Description of key information

The transformation/dissolution test (OECD Series on Testing and Assessment Number 29, 2001) of chromium, iron, titanium and zinc spinel and rutile at a loading of 1 mg/L at pH 6 and pH 8 for 28 days resulted in maximum quantified Cr concentrations of 0.355 µg/L (pH = 6, 28d), maximum  Fe concentrations of 0.532 µg/L (pH = 6, 28d), maximum Zn concentrations of 4.78 µg/L (pH = 8, 28d) as well as maximum Ti concentrations of 0.022 µg/L (background corrected, pH = 8, 28d). Thus, the extent to which "Chromium, iron, titanium and zinc spinel and rutile" can produce soluble available ionic and other metal-bearing species in aqueous media is limited. An additional test at pH 8 with 100 mg/L loading for 7 days revealed maximum soluble concentrations of 4.42 µg/L Cr, 23.3 µg/L Zn, < 0.463 µg/L Fe and < 0.042 µg/L Ti.

Thus, chromium, iron, titanium and zinc spinel and rutile is poorly soluble in environmental media at pH6 and pH8.

Key value for chemical safety assessment

Additional information