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Physical & Chemical properties

Water solubility

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Endpoint:
water solubility
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2012-12-12 to 2013-01-14
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 105 (Water Solubility)
Deviations:
yes
Remarks:
See "Principles of method if other than guideline"
Principles of method if other than guideline:
- The test was conducted under exclusion of atmospheric carbon dioxide and atmospheric oxygen
- Two vessels were set up in a parallel design at 20 ± 1.0 °C, each solution was sampled repeatedly over time instead of setting up multiple vessels and sampling solutions from a different vessel at each sampling date. This modification helps to minimize weighing errors as larger amounts are being handled.

Vanadium, oxalate complexes was handled under inert gas only to avoid any exposure to air. During the test performance, solutions containing the test item were stirred slowly. The water was purged with argon (ca. half an hour) before preparing the test solutions.
GLP compliance:
yes (incl. QA statement)
Remarks:
signed, 2011-02-07
Type of method:
flask method
Key result
Water solubility:
145.1 g/L
Conc. based on:
test mat. (dissolved fraction)
Loading of aqueous phase:
200 g/L
Incubation duration:
>= 1 - <= 3 d
Temp.:
20 °C
pH:
1.9
Remarks on result:
other: mean dissolved concentration: 145.1 ± 11.4 g/L, calculated based on a vanadium content of 24.8 %.
Water solubility:
35.98 g/L
Conc. based on:
element (dissolved fraction)
Remarks:
Vanadium
Loading of aqueous phase:
200 g/L
Incubation duration:
>= 1 - <= 3 d
Temp.:
20 °C
pH:
1.9
Remarks on result:
other: mean dissolved concentration: 35.98 ± 2.83 g V/L
Details on results:
Observations
During the study, undissolved test material was observed in solution and especially on the bottom of the flasks. After filtration, the solution was clear.
 
Temperature
Thermo Data Logger EL-USB-TC: The mean temperature was 20.4 ± 0.4 °C.
 
Monitoring oxygen concentration
During the experimental performance of the test, the oxygen concentration in the acrylic glass box was measured with a MICRO IV oxygen sensor prior the test and directly before and after each sampling. The oxygen concentration remained around 0 %. 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 to 1.9. Measured pH of method blanks ranged from 5.5 to 6.0.The temperature measured by the pH meter did not remain at 20.0 ± 1.0 °C (but measured by the Thermo Data Logger it did). The pH meter is calibrated every workweek and verified every working day; however a calibration of the temperature was not performed since a thermo data logger was applied during the test. Thus, respective temperature measurements may not be as accurate.
 
Turbidity
Due to a limited sampling volume, turbidity was measured just once (after filtration) to verify that only dissolved vanadium concentrations would get measured.
 
Dissolved vanadium concentrations
Vanadium levels of method blanks sampled at day 1 were below the limit of detection (LOD = 0.232 µg V/L). Vanadium concentrations of method blanks from day 2 and 3 were above the LOQ (LOQ = 0.695 µg V/L) but far below concentrations in diluted actual samples.
The pH of the test solution was much lower at the higher loading of the main test, and the lower solution pH may have enhanced the dissolution. However, an insoluble residue was observed in the test vessels after 3 days. The consistent V concentrations and the observed precipitation seem to indicate that a solubility equilibrium had been reached.
Vanadium concentrations remained constant during the first three days of testing as defined by the study guideline OECD 105 and Regulation 440/2008/EC A.6.

Method validation summary

validation parameter

results

comment

selectivity

similar data with at least two different wavelengths for ICPOES method

no interferences due to test media observed

linearity

applied calibration functions were linear

correlation coefficient at least 0.999325

limits of detection (LOD)

0.232 – 0.375 μg V/L

 

limits of quantification (LOQ)

0.695 – 1.12 μg V/L

 

V concentrations in method blanks

day 1: below LOD (< 0.695 μg V /L), day 2 & 3: above LOQ (> 0.695 μg V/L) but below conc. In diluted test solutions

 

accuracy, precision & repeatability

mean recovery for TMDA-70 (312 μg V/L): 99.8 ± 0.8 % (n = 9)

concentration range of diluted samples

accuracy and precision

recovery for recalibration standard (750 μg V/L): 98.5 ± 0.9 % (n = 3)

concentration range of diluted samples

accuracy and precision

recovery for recalibration standard (500 μg V/L): 102 % (n = 1)

concentration range of diluted samples

accuracy and precision

mean recovery for Merck XXI standard (500 μg V/L): 98.0 ± 0.4 % (n = 3)

low concentration range

accuracy and precision

mean recovery for Merck XXI standard (100 μg V/L): 101 ± 1 % (n = 4)

low concentration range

accuracy and precision

mean recovery for CPI Quality Control standard (300 μg V/L): 102± 1 % (n = 2)

low concentration range

accuracy and precision

mean recovery for CPI Quality Control standard (250 μg V/L): 98.1 ± 0.3 % (n = 4)

concentration range of diluted samples

trueness

recovery of fortified samples: 97.5 – 99.5 %

 

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

test day [d]

V conc. of samples vessel A [g/L]

mean V conc. ± SD vessel A [g/L]

V conc. of samples vessel B [g/L]

mean V conc. ± SD vessel B [g/L]

mean V conc. ± SD [g/L]

variation between samplings [%]

1

34.87

33.85 ± 1.44

39.87

37.27 ± 3.68

35.56 ± 3.01

 

32.84

34.67

2

34.24

34.15 ± 0.13

39.00

39.54 ± 0.75

36.84 ± 3.14

3.6

34.06

40.07

3

39.89

36.57 ± 4.70

34.34

34.48 ± 0.20

35.53 ± 2.97

-3.6

33.24

34.62

 

 Measured vanadium concentrations in method blanks

test day [d]

V conc. blank A [µg/L]

V conc. blank B [µg/L]

LOD
[µg V/L]

LOQ
[µg V/L]

1

< LOD

< LOD

0.232

0.695

< LOD

< LOD

2

2.858

2.615

2.859

2.667

3

2.445

1.066

2.646

4.952

Vanadium concentrations remained constant during the first three days of testing, i.e. vanadium concentrations varied by less than 15 % between sampling points. Therefore, the acceptability criteria of the study guideline OECD 105 and Regulation 440/2008/EC A.6 could be regarded as fulfilled.

The mean dissolved vanadium concentrations of solutions sampled from day 1 until day 3 were calculated.

Mean dissolved V concentrations day 1 – day 3:

Vessel A: 34.86 ± 10.4 g/L

Vessel B: 37.10 ± 11.4 g/L

The amount of vanadium, oxalate complexes dissolved was calculated based on the vanadium content of the test substance as follows:

 = mean of measured V concentration * 100 % / 24.8 % [V content of test item]

 

mean calculated vanadium, oxalate complexes dissolved day 1 – day 3:

Vessel A: 140.6 ±10.4 g/L

Vessel B: 149.6 ±11.4 g/L

Conclusions:
Under the conditions of this test (under exclusion of CO2 and O2, under inert argon gas; flask method; loading of 200 g/L), a solubility equilibrium was reached during the first three days of testing. The mean measured amount of dissolved V from day 1 until day 3 at 20.0 ± 1.0 °C is 35.98 ± 2.83 g V/L (determined as dissolved V, separated by filtration from undissolved test item). This corresponds to a water solubility of vanadium, oxalate complexes of 145.1 ± 11.4 g/L at pH 1.9, calculated based on a vanadium content of 24.8 %. Hence, divanadium pentaoxide may considered as moderately soluble (100-1000 mg/L).
Endpoint:
transformation / dissolution of metals and inorganic metal compounds
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2012-08-29 to 2013-08-28
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
Version / remarks:
2001
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.:
239 µg/L
Element analysed:
Vanadium
Loading of aqueous phase:
1 mg/L
Incubation duration:
24 h
Test conditions:
21.2 °C, pH 7.9
Remarks on result:
other: mean of three measurements, SD: ± 4.5 µg V/L
Type of test:
full transformation/dissolution test - metals and sparingly soluble metal compounds
Mean dissolved conc.:
231 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 of three measurements, SD: ± 0.9 μg V/L
Details on results:
Temperature: the mean temperature was 21.4 ± 0.3 °C.

pH: The measured pH in solutions containing the test item ranged from 7.7 – 7.9 at target pH 8 and from 5.9 – 6.3 at target pH 6 and in method blanks from 7.7 – 7.9 and from 5.7 – 6.3, respectively.

Oxygen: Oxygen levels in all test solutions 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:
In addition to measuring vanadium speciation in samples 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 ≤ the respective LOQ.
The observed variations within and between the test flasks are in compliance with the OECD Series 29, which requires a limit of 20 % and 10 % for the between-vessel and the within-vessel variation, respectively.
According to the guidance document “[…] the test can be stopped when three subsequent total dissolved metal concentration data points vary no more than 15%”. Since equilibrium was reached after 24 h, i.e. the dissolution of vanadium, oxalate complexes was complete and the vanadium speciation remained constant over the test with nearly all dissolved vanadium being in the pentavalent and highest oxidised form, the test was terminated after 24 hThe OECD Series 29 requires a limit of 20 % and 10 % for the between-vessel and the within-vessel variation, respectively.

Determination of mass balance
The test substance contains 24.8 v/v % vanadium. Measured V concentrations indicate the complete dissolution of the test item after 2h. The amount of test item was calculated as follows: measured dissolved V * 100 % / 24.8 % (percentage of V in test item). Therefore, a separate calculation of the mass balance is not necessary.

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 0.999854

limit of detection

samples and BWs: 12.3 μg V/L

sample fortification: 4.1 μg V/L

-

limit of quantification

samples and BWs: 41.1 μg V/L

sample fortification: 13.6 μg V/L

 -

V concentration in method blanks

< LOD (< 12.3 μg/L)

 -

accuracy and precision, repeatability

mean recovery of V in CRM TMDA-70

(312 μg V/L): 104.1 ± 2.5 % (n = 7)

concentration range of samples

accuracy and precision

mean recovery of V in Merck XXI

(250 μg V/L): 100.7 ± 2.7 % (n = 4)

concentration range of samples
accuracy and precision

mean recovery of V in recalibration standard

(100 μg V/L): 103.7 ± 4.7 % (n = 4)

low concentration range
accuracy and precision

mean recovery of V in recalibration standard

(250 μg V/L): 96.6 ± 1.7 % (n = 3)

concentration range
trueness

mean recovery of V in fortified

samples: 99.4 – 100.5 % (n = 6)

-

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 0.99957

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 concentrations in method blanks

At least below LOQs for V(IV) and V(V)

-

accuracy

mean recovery of V in recalibration standards (100 μg/L V(IV) and 100 μg/L V(V)):

81.2 ± 7.5% (n = 3) for V(IV)

87.9 ± 17.9 % (n = 3) for V(V)

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): recoveries are in the range of 92.2 % to 105.5 %

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

Measured total dissolved V and V(IV), V(V) concentrations for the loading of 1 mg/L

(target pH 8: 1, 2, 3; target pH 6: 4, 5, 6 – triplicate vessels per pH, duplicate samples per vessel)

sample

mean V conc. per vessel ± SD [μg/L]

mean V conc. all vessels ± SD [μg/L]

V(IV) conc. [μg/L]

V(V) conc. [μg/L]

mean Σ V(IV) + V(V) [μg/L]

recovery mean Σ V(IV) + V(V) related to mean V conc. all vessels [%]

1 2h

2 2h

3 2h

249.3 ± 1.3

259.0 ± 0.4

251.5 ± 2.1

253.3 ± 4.7

12.0

22.4

22.2

215.9

222.6

218.9

238.0

94.0

1 6h

2 6h

3 6h

244.5 ± 10.7

258.9 ± 0.5

251.7 ± 2.0

251.7 ± 8.1

8.6

7.7

7.9

218.8

233.3

222.8

233.0

92.6

1 24h

2 24h

3 24h

237.1 ± 0.1

244.7 ± 0.5

235.2 ± 0.2

239.0 ± 4.5

15.3

16.0

18.3

214.5

237.2

230.7

244.0

102.1

4 2h

5 2h

6 2h

246.3 ± 0.5

244.2 ± 0.9

245.2 ± 0.8

245.2 ± 1.1

23.6

117.9

28.2

198.5

126.5

206.2

233.6

95.3

4 6h

5 6h

6 6h

250.2 ± 0.8

248.9 ± 0.5

248.6 ± 0.8

249.2 ± 1.0

15.3

15.9

11.2

209.2

172.0

203.7

229.7

92.2

4 24h

5 24h

6 24h

231.8 ± 0.4

231.2 ± 1.0

230.2 ± 0.4

231.1 ± 0.9

18.1

26.6

22.1

197.6

225.9

240.9

243.8

105.5

Internal calculations were performed with more digits, values were rounded

LOD: Limit of detection (HPLC coupled to ICP-MS LOD V(IV) = 2.0 μg/L; LOD V(V) = 2.0 μg/L)

LOQ: Limit of quantification (HPLC coupled to ICP-MS LOQ V(IV) = 6.1 μg/L; LOQ V(V) = 6.0 μg/L)

SD: standard deviation

Conclusions:
Under the described conditions of this test with vanadium, oxalate complexes at a loading of 1 mg/L, dissolved vanadium concentrations after 24 h were 239.0 ± 4.5 μg/L and 231.1 ± 0.9 μg/L at pH 8 and pH 6, respectively. Measured concentrations indicate a complete dissolution of the test item in both media. Over the course of the test predominantly pentavalent vanadium species were detectable. The within and between vessel variation, the variation of mean V concentrations between sampling intervals as well as temperatures and oxygen levels meet the requirements of the OECD-Guidance document 29.
According to the guidance document (OECD-Guidance document 29) “[…] the test can be stopped when three subsequent total dissolved metal concentration data points vary no more than 15 %”. Since equilibrium was reached after 24 h, i.e. the dissolution of vanadium, oxalate complexes was complete and the vanadium speciation remained constant over the test with nearly all dissolved vanadium being in the pentavalent and highest oxidised form, the test was terminated after 24 h.

Description of key information

The water solubility of vanadium, oxalate complexes is 145.1 ± 11.4 g/L at pH 1.9 and 20 °C.

The transfomation/dissolution test with a loading of 1 mg/L indicated a complete dissolution of the test item in both media ( pH8 and 6) after 24 h.

Key value for chemical safety assessment

Water solubility:
145.1 g/L
at the temperature of:
20 °C

Additional information

Water solubility:

Under the conditions of this test (under exclusion of CO2 and O2, under inert argon gas; flask method; loading of 200 g/L), a solubility equilibrium was reached during the first three days of testing. The mean measured amount of dissolved V from day 1 until day 3 at 20.0 ± 1.0 °C is 35.98 ± 2.83 g V/L (determined as dissolved V, separated by filtration from undissolved test item). This corresponds to a water solubility of vanadium, oxalate complexes of 145.1 ± 11.4 g/L at pH 1.9, calculated based on a vanadium content of 24.8 %. Hence, divanadium pentaoxide may considered as moderately soluble (100-1000 mg/L).

Transformation /dissolution:

Under the described conditions of this test with vanadium, oxalate complexes at a loading of 1 mg/L, dissolved vanadium concentrations after 24 h were 239.0 ± 4.5 μg/L and 231.1 ± 0.9 μg/L at pH 8 and pH 6, respectively. Measured concentrations indicate a complete dissolution of the test item in both media. Over the course of the test predominantly pentavalent vanadium species were detectable. According to OECD-Guidance document 29 “[…] the test can be stopped when three subsequent total dissolved metal concentration data points vary no more than 15 %”. Since equilibrium was reached after 24 h, i.e. the dissolution of vanadium, oxalate complexes was complete and the vanadium speciation remained constant over the test with nearly all dissolved vanadium being in the pentavalent and highest oxidised form, the test was terminated after 24 h.