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Physical & Chemical properties

Water solubility

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Endpoint:
transformation / dissolution of metals and inorganic metal compounds
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:
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 2011-02-07
Type of method:
flask method
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
30.06 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
24 h
Test conditions:
21.3 °C, pH 7.7
Remarks on result:
other: mean dissolved concentration: 30.06 ± 4.77 µg V/L
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
47.5 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
7 d
Test conditions:
21.6 °C, pH 7.9
Remarks on result:
other: mean dissolved concentration: 47.50 ± 7.5 µg V/L
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
72.4 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
28 d
Test conditions:
21.7 °C, pH 7.9
Remarks on result:
other: mean dissolved concentration: 72.40 ± 9.07 µg V/L
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
28.6 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
24 h
Test conditions:
21.3 °C, pH 6.1
Remarks on result:
other: mean dissolved concentration: 28.60 ± 6.66 µg V/L
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
37.06 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
7 d
Test conditions:
21.2 °C, pH 6.1
Remarks on result:
other: mean dissolved concentration: 37.06 ± 3.99 µg V/L
Key result
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
61.57 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
28 d
Test conditions:
21.4 °C, pH 6.2
Remarks on result:
other: mean dissolved concentration: 61.57 ± 3.48 µg V/L
Details on results:
Temperature
The temperature of the thermostatically controlled room was recorded with an EL-USB data logger. The mean temperatures were 21.2 ± 0.7 °C during the 28-d test with 1 mg/L loading and 21.3 ± 0.7 C during the 7-d test with 100 mg/L loading. Therefore, the mean temperatures are in agreement with the OECD guidance document 29.

Solution pH and oxygen concentrations
In solutions containing 1 and 100 mg/L of the test item and in respective method blanks at pH 8 and 6, pH ranged from 7.7 – 8.0 and 5.9 – 6.2, respectively.
Oxygen levels of all test solutions (all loadings) 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
Due to EDTA stabilisation of samples for HPLC-ICP-MS measurements, samples were at least diluted by a factor of 3.
Dissolved vanadium concentrations in method blanks from the test with 1 mg/L loading were at least below the LOQ of the specific measurement series. Vanadium concentrations of method blanks from the test with 100 mg/L loading were always below the respective LOD.
In addition to measuring vanadium speciation of solutions containing the test item, one method blank sample per media and sampling time was analysed by HPLC-ICP-MS to verify that the transformation/dissolution media, the eluent for the HPLC-analysis and the EDTA-solution needed for stabilising V speciation did not contain any vanadium. The concentrations of V species in these blanks were below the respective LOQs (LOQ: 6.1 μg/L for V (IV) and 6.0 μg/L for V (V)).
The highest LOD of ICP-OES measurements was 15.2 μg V /L with corresponding LOQs of 50.8 μg V /L. The LODs / LOQs of HPLC-ICP-MS measurements were 2.0 μg/L / 6.1 μg/L for V (IV) and 2.0 μg/L / 6.0 μg/L for V (V), respectively. The values in parentheses were obtained by multiplying the measured concentrations with dilution factor of at least 3 (dilution with EDTA to stabilize species.)
The OECD Series 29 requires a limit of 20% and 10% for the between-vessel and the within-vessel variation, respectively.
The observed variations within and between test vessels with a loading of 1 and 100 mg/L at pH 6 and pH 8 are in compliance with the test guideline after 7 and 28 days.

Mass balance
Vanadium recoveries for the test with 1 mg/L ranged from of 83.6 to 110 %. Rinsing of filters from the test with 100 mg/L loading was not necessary because vanadium was fully recovered; recoveries ranged from 101 to 103 %.

Method validation summary (ICP-OES)

validation parameter

results

Comment

selectivity

similar data with two different V wavelengths for ICP-OES method

no interferences observed

linearity

applied calibration functions were linear

correlation factor at least 0.99957

limit of detection

1.77 - 15.24 μg V/L

limit of quantification

5.90 - 50.78 μg V/L

V concentrations in method blanks

Test with 1 mg/L loading:
below respective LOD, except for 4 samples with V concentrations below respective LOQ

Test with 100 mg/L loading:
below respective LOD, i.e. < 5.15 μg V/L

accuracy and precision, reproducibility

mean recovery for CRM TMDA-70 (312 µg V/L):
106 ± 3 % (n = 7)

concentration range of diluted samples from test with 100 mg/L

accuracy and precision, reproducibility

mean recovery for CRM TMDA-70 (156 µg V/L, dilution factor 2):
100 ± 2 % (n = 5)

concentration range of diluted samples from test with 100 mg/L

accuracy and precision, reproducibility

mean recovery for CRM TMDA-70 (31.2 µg V/L, dilution factor 10):
102 ± 6 % (n = 19)

concentration range of diluted samples from test with 1 mg/L

accuracy and precision, reproducibility

mean recovery for Merck XXI (500 µg V/L):
97.7 ± 3.6 % (n = 5)

for high concentration range

accuracy and precision, reproducibility

mean recovery for Merck XXI (100 µg V/L):
98.1 ± 0.8 % (n = 2)

for medium concentration range

accuracy and precision, reproducibility

mean recovery for Merck XXI (50 µg V/L):
102 ± 4 % (n = 9)

for low concentration range

accuracy and precision, reproducibility

mean recovery for Merck XXI (25 µg V/L):
100 ± 4 % (n = 10)

for low concentration range

accuracy and precision

mean recovery for recalibration (500 µg V/L):
97.3 ± 1.0 % (n = 2)

for high concentration range

accuracy and precision

mean recovery for recalibration (250 µg V/L):
95.8 ± 0.3 % (n = 2)

for medium concentration range

accuracy and precision, reproducibility

mean recovery for recalibration (100 µg V/L):
101 ± 5 % (n = 19)

for medium concentration range

accuracy and precision, reproducibility

mean recovery for recalibration (50 µg V/L):
98.5 ± 2.6 % (n = 10)

for low concentration range

accuracy and precision

mean recovery for multielement standard from CPI (250 µg V/L):
97.9 ± 2.2 % (n = 3)

for medium concentration range

trueness

Test with 1 mg/L loading:

fortification of samples:
99.8 – 102.5 % (n = 4)

Test with 100 mg/L loading:fortification of samples:
100.7– 101.7 % (n = 3)

Method validation summary (HPLC-ICP-MS)

validation parameter

results

Comment

selectivity

ICP-MS (51V) selective for vanadium; chromatographic peaks verified by V(IV) and V(V) standards

no interferences observed

linearity

applied calibration functions were linear

correlation factor at least 0.995

limit of detection

V(IV): 2.0 μg/L

V(V): 2.0 μg/L

 

limit of quantification

V(IV): 6.1 μg/L

V(V): 6.0 μg/L

 

V concentration in method blanks

At least below LOQs for V(IV)

 

accuracy and precision

mean recovery for recalibration standards (500 μg/L V(IV) and 500 μg/L V(V)):
V(IV): 87.3. ± 7.4 % (n = 3) V(V): 94.3 ± 8.2 % (n = 3)

concentration range of samples
(QA/QC requirements 100 ± 25 %)

accuracy and precision, reproducibility

mean recovery for recalibration standards (250 μg/L V(IV) and 250 μg/L V(V)):
V(IV): 90.2 ± 6.6 % (n = 5) V(V): 87.6 ± 7.7 % (n = 5)

concentration range of samples
(QA/QC requirements 100 ± 25 %)

accuracy and precision, reproducibility

mean recovery for recalibration standards (50 μg/L V(IV) and 50 μg/L V(V)):

V(IV): 98.4 ± 9.8 % (n = 32) V(V): 99.1 ± 10.0 % (n = 32)

 

concentration range of samples
(QA/QC requirements 100 ± 25 %)

trueness

total V (by ICP-OES) compared to sum of V(IV) and V(V) (by HPLC-ICP-MS):

Test with loading of 1 mg/L at pH 6: mean recoveries are in the range of 91.1 % to 118.8 %

Test with loading of 1 mg/L at pH 8:mean recoveries are in the range of 86.6 % to 109.2 %

Test with loading of 100 mg/L at pH 8:mean recoveries are in the range of 81.2 % to 102.8 %

Quality requirements are 100 ± 25 % due to comparison of two methods with very different uncertainties

 

Under the described conditions of this test with vanadium dioxide at a loading of 1 mg/L, dissolved vanadium concentrations after 672 h (28 d) were 72.40 ± 9.07 µg/L and 61.57 ± 3.12 µg/L at pH 8 and pH 6, respectively. Thus, the transformation/dissolution of VO2 was highest at pH 8. The dissolved vanadium concentration at a loading of 100 mg/L at pH 8 was 3.329 ± 0.110 mg/L after 7 days. Over the course of the test, predominantly pentavalent vanadium species were detectable.

Conclusions:
Under the described conditions of this test with vanadium dioxide at a loading of 1 mg/L, dissolved vanadium concentrations after 672 h (28 d) were 72.40 ± 9.07 μg/L and 61.57 ± 3.12 μg/L at pH 8 and pH 6, respectively. Thus, the transformation/dissolution of VO2 was highest at pH 8. The dissolved vanadium concentration at a loading of 100 mg/L at pH 8 was 3.329 ± 0.110 mg/L after 7 days. Over the course of the test, predominantly pentavalent vanadium species were detectable.
Endpoint:
water solubility
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:
OECD Guideline 105 (Water Solubility)
Version / remarks:
1995
Deviations:
yes
Remarks:
exclusion of CO2 and O2; two vessels were set up in a parallel design
Qualifier:
according to guideline
Guideline:
EU Method A.6 (Water Solubility)
Version / remarks:
2008
Deviations:
yes
Remarks:
exclusion of CO2 and O2; two vessels were set up in a parallel design
GLP compliance:
no
Type of method:
flask method
Key result
Water solubility:
39.27 mg/L
Conc. based on:
test mat.
Loading of aqueous phase:
1 750 mg/L
Incubation duration:
>= 34 - <= 34 d
Temp.:
20 °C
pH:
>= 4 - <= 4.4
Remarks on result:
other: mean dissolved concentration: ± 3.49 mg/L
Water solubility:
24.11 mg/L
Conc. based on:
element (dissolved fraction)
Remarks:
Vanadium
Loading of aqueous phase:
1 750 mg/L
Incubation duration:
>= 34 - <= 35 d
Temp.:
20 °C
pH:
>= 4 - <= 4.4
Remarks on result:
other: mean dissolved concentration: 24.11 ± 2.14 mg V/L
Details on results:
Observations
During the study, undissolved test material was observed in the test media and especially at the bottom and the flask walls. After filtration, the solution was clear. To verify the reliability of the filtration step and thus that only dissolved vanadium concentrations would get measured, turbidity was measured in a filtered sample directly after sampling.

Temperature
The mean temperature was 19.6 ± 0.1 °C.

Monitoring oxygen concentration
The measured oxygen concentration ranges from -1.1 % to -0.1 %. Slightly negative values, though impossible, are due to measurement uncertainties of the device at 0 % oxygen content.

Solution pH
Solution pH of samples containing the test item decreased during the test from 4.4 to 4.0 (mean) whereas the pH of method blanks decreased from 5.8 to 5.3 (mean).

Turbidity
The turbidity of solution samples was measured after filtering to verify that only dissolved vanadium concentrations would get measured. The turbidity was always <1 NTU, indicating that there was not any undissolved material after the filtration step.

Method validation summary

validation parameter results comment
selectivity similar data with at least three different wavelengths for ICP-OES method no interferences due to test media observed
linearity applied calibration functions were linear correlation coefficients ≥ 0.999948
limits of detection (LOD) 0.062 – 0.248 µg V/L

limits of quantification (LOQ)

0.186 – 0.744 µg V/L

V concentrations in

method blanks

< respective LOQs 

in two samples > respective LOQ but well below conc. in actual samples containing the test item (< 1 %).

-

accuracy and precision;

repeatability

mean recovery for TMDA-70 (312 µg V/L):

100.3 ± 1.1 (n = 8)

concentration range of diluted samples

accuracy and precision;

repeatability

mean recovery for Quality Control standard

(diluted to 100 µg V/L): 107.1 ±2.8 (n = 8)

concentration range of diluted samples

accuracy and precision;

repeatability

mean recovery for recalibration standard

(diluted to 250 µg V/L): 99.7 ±3.7 (n = 7)

concentration range of diluted samples
accuracy and precision

 mean recovery for recalibration standard

(diluted to 100 µg V/L): 98.1 ± 0.3 (n = 2)

concentration range of diluted samples

Quality assurance measurements

Dissolved vanadium concentrations in analysed method blanks were at least below the respective limits of quantification with the exception of two samples in which V concentrations exceeded the respective LOQ (i.e. method blank a, vessel 1 after 2 days: 0.7107 µg V/L and after 20 days: 7.0112 µg V/L). The elevated vanadium concentrations measured in these two samples of one method blank were, however, well below vanadium concentrations of solutions containing the test item (< 1 %) and do not affect the results of the water solubility study.

According to the quality assurance requirement, V recovery was in the range of ± 15 % of the certified values.

Measured vanadium concentrations in test samples (calculations were performed with more digits, values were rounded)

test day [d]

dilution factor

V conc. of samples vessel 1 [mg/L]

mean V conc.
± SD
vessel 1
[mg/L]

V conc. of samples vessel 2 [mg/L]

mean V conc.
± SD vessel 2
[mg/L]

mean V conc.
± SD
[mg/L]

relative difference between samplings [%]

1

100

9.62

9.62 ± <0.01

9.10

9.10 ± 0.01

9.36 ± 0.30

 

9.61

9.11

2

11.52

11.55 ± 0.06

11.02

11.07 ± 0.08

11.31 ± 0.29

20.87

11.59

11.12

9

18.13

18.17 ± 0.05

18.65

18.67 ± 0.04

18.42 ± 0.30

62.85

18.20

18.70

10

19.05

19.12 ± 0.11

20.21

20.28 ± 0.11

19.70 ± 0.68

6.97

19.20

20.36

11

20.57

20.56 ± 0.02

22.41

 22.42 ± 0.01

21.49 ± 1.07

9.05

20.54

22.43

20

23.62

23.76 ± 0.20

25.39

 25.35 ± 0.05

24.56 ± 0.93

14.29

23.90

25.32

21

24.41

24.35 ± 0.09

25.91

25.99 ± 0.11

25.17 ± 0.95

2.49

24.28

26.07

34

25.34

25.27 ± 0.10

23.41

23.30 ± 0.15

24.29 ± 1.14

-3.51

25.19

23.20

35

25.82

26.52 ± 1.00

21.61

21.34 ± 0.38

23.93 ± 3.06

-1.46

Measured vanadium concentrations in method blanks

test day [d]

V conc. blank 1 [µg/L]

V conc. blank 1 [µg/L]

LOD
[µg V/L]

LOQ
[µg V/L]

1

< LOD

< LOD

0.196

0.587

< LOD

< LOD

2

0.711

< LOD

0.196

0.587

< LOD

< LOD

0.248

0.744

9

< LOD

< LOD

0.248

0.744

< LOD

< LOD

10

< LOD

< LOD

< LOD

< LOD

11

< LOD

< LOQ (0.3632)

< LOD

< LOD

20

0.7107

< LOD

0.062

0.186

< LOD

< LOD

21

< LOD

< LOQ (0.1839)

< LOD

< LOD

34

< LOD

< LOD

0.183

0.549

< LOQ (0.2486)

< LOQ (0.2111)

35

< LOQ(0.2892)

< LOQ(0.1989)

< LOD

< LOQ(0.2548)


Conclusions:
Under the conditions of this test (under exclusion of CO2 and O2, under inert argon gas; flask method; loading of 1750 mg/L), a solubility equilibrium was reached on day 34 and day 35. The mean measured amount of dissolved vanadium on day 34 and day 35 at 20.0 ± 1.0 °C amounts to 24.11 ± 2.14 mg/L corresponding to a water solubility of dissolved vanadium dioxide of 39.27 ± 3.49 mg/L. The solution pH of samples containing the test item decreased during the test from to 4.4 to 4.0 (mean) whereas the pH of method blanks decreased from 5.8 to 5.4 (mean).
Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
supporting study
Study period:
2010-09-01 to 2011-10-28
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 105 (Water Solubility)
Version / remarks:
,1995
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA OPPTS 830.7840 (Water Solubility)
Deviations:
no
GLP compliance:
no
Type of method:
flask method
Water solubility:
345 mg/L
Temp.:
20 °C
pH:
>= 3 - <= 4.5
Details on results:
The soluble vanadium appeared to be continuing to increase after the 3 day. Therefore additional times of 7 and 9 days equilibration at 30 °C followed by 24 h at 20 °C were analyzed. These additional times met the criteria for < 15 % difference.
Conclusions:
Interpretation of results: moderately soluble (100-1000 mg/L)
The water solubility of vanadium dioxide is 345 mg/L at 20 °C and pH 3.

Description of key information

The water solubility of dissolved vanadium dioxide is 39.27 ± 3.49 mg/L (inert argon gas; flask method; loading of 1750 mg/L; 20.0 ± 1.0 °C; pH 4.4 to 4.0)

Key value for chemical safety assessment

Water solubility:
39.27 mg/L
at the temperature of:
20 °C

Additional information

Two water solubility studies (key and supporting studies) according to OECD 105 and a transformation/dissolution test according to OECD Series on Testing and Assessment No. 29 were conducted with vanadium dioxide.

The water solubility key study results in a water solubility of dissolved vanadium dioxide of 39.27 ± 3.49 mg/L (inert argon gas; flask method; loading of 1750 mg/L; 20.0 ± 1.0 °C; pH 4.4 to 4.0).

The transformation/dissolution testing initiated at loadings of 1 mg/L results in dissolved vanadium concentrations after 672 h (28 d) 72.4 ± 9.07 µg/L and 61.57 ± 3.12 µg/L at pH 8 and pH 6, respectively and of 100 mg/L at pH 8 in a dissolved vanadium concentration of 3.329 0.110 mg/L. The results are used for classification and labelling (ecotoxicity).

The water solubility supporting study results in a water solubility of 345 mg VO2/L at 20 °C.