Tin antimony grey cassiterite

Water solubility

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

transformation / dissolution of metals and inorganic metal compounds

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2015-06-12 to 2015-09-28

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

GLP compliance:

yes (incl. QA statement)

Type of method:

other: transformation/ dissolution

Key result

Type of test:

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

Mean dissolved conc.:

0.389 µg/L

Element analysed:

Sn

Loading of aqueous phase:

1 mg/L

Incubation duration:

672 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 0.122 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

8.892 µg/L

Element analysed:

Sn

Loading of aqueous phase:

1 mg/L

Incubation duration:

672 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 2.670 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.329 µg/L

Element analysed:

Sb

Loading of aqueous phase:

1 mg/L

Incubation duration:

672 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 0.214 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.611 µg/L

Element analysed:

Sb

Loading of aqueous phase:

1 mg/L

Incubation duration:

672 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 0.041 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.131 µg/L

Element analysed:

V

Loading of aqueous phase:

1 mg/L

Incubation duration:

672 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 0.082 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.205 µg/L

Element analysed:

V

Loading of aqueous phase:

1 mg/L

Incubation duration:

672 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 0.013 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.566 µg/L

Element analysed:

Sn

Loading of aqueous phase:

1 mg/L

Incubation duration:

168 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD: ± 0.23 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

5.71 µg/L

Element analysed:

Sn

Loading of aqueous phase:

1 mg/L

Incubation duration:

168 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 2.39 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.214 µg/L

Element analysed:

Sb

Loading of aqueous phase:

1 mg/L

Incubation duration:

168 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.15 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.395 µg/L

Element analysed:

Sb

Loading of aqueous phase:

1 mg/L

Incubation duration:

168 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.03 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.093 µg/L

Element analysed:

V

Loading of aqueous phase:

1 mg/L

Incubation duration:

168 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.057 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

0.176 µg/L

Element analysed:

V

Loading of aqueous phase:

1 mg/L

Incubation duration:

168 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.009 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

1.59 µg/L

Element analysed:

Sn

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.218 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

0.254 µg/L

Element analysed:

Sn

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.067 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

0.099 µg/L

Element analysed:

Sb

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.015 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

0.059 µg/L

Element analysed:

Sb

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.032 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

0.059 µg/L

Element analysed:

V

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH 8, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.004 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

0.037 µg/L

Element analysed:

V

Loading of aqueous phase:

1 mg/L

Incubation duration:

24 h

Test conditions:

pH 6, agitation at 100 rpm, 21.5 ± 1.5 °C, 0.2 µm filtration

Remarks on result:

other: SD ± 0.017 µg/L

Details on results:

Temperature
The temperature of the thermostatically controlled room was recorded with a Testo 175-T2 data logger. The mean temperature was 20.4 ± 0.2 °C during the test with 1 mg/L loading at pH 8. The mean temperature during the test at pH6 was 20.4 ± 0.2 °C. Therefore, the mean temperature is in agreement with the OECD guidance document 29

Solution pH and oxygen concentrations
In solutions containing 1 mg/L of the test item at pH 6 and pH 8 as well as in method blanks (BW), the pHs in the range of 5.8 – 6.5 and 7.6 – 8.2, respectively.

Mass balance
The measured vanadium concentrations in samples from rinsed filters and vessels from pH 6 all were below LODs/LOQs (pH 6: 0.2033/0.6098). Therefore, the mass balance was not calculated for pH 6.
The measured concentrations for mass balance samples from pH 8 were above respective limits. However, the recovery of vanadium was 20.8 – 24.1%. This is clearly below 100 ± 15 %, indicating that aqua regia is not sufficient for a complete dissolution of the test item. The latter fact is expected for inorganic pigments.

Within-vessel variation and between-vessel variation
According to the guidance, “[…]it is reasonable to anticipate that for a constant loading of a substance, tested in a narrow particle size (e.g. 37 - 44 μm) and total surface area range, the within-vessel variation in transformation data should be less than 10 % and the between-vessel variation should be less than 20 %”.
The particle size distribution of each loading replicate may differ and thus resulting in different overall total surface areas per vessel. Since the exposed surface area is affecting the rate of transformation and dissolution of sparingly soluble metal compounds, increases in vessel variations may be observed in tests of materials with wider particle size distributions.
For the measured metals these variations are not always within the limits.
Background concentrations for antimony and vanadium at pH 6 and pH 8 were measured to be in the range of test item loaded samples. Therefore, the measured concentrations from test item loaded vessels at pH 6 and 8 were background (means) corrected. The background concentration of tin was below the LOD.

Recoveries of fortified samples

Recoveries of fortified samples vanadium (values were rounded, internal calculations were performed with more digits)

sample	Measured concentration [μg M/L]	calculated level after addition [μg M/L]	recovery [μg M/L] / [%]
1 mL of sample + 4 mL of 25 μg V/L
Mass balance sample a from vessel 1	1.467	20.293	20.116 / 99.1
0.5 mL of sample + 4.5 mL of 2.5 μg V/L
Mass balance sample filters from samples of vessel 4	<LOD	2.250	2.161 / 96.0
1 mL of sample + 2 mL of 5 μg V/L
Sample a from vessel 1 after 2h	0.032	3.344	3.665 / 109.6
Sample a from vessel 1 after 6h	0.041	3.347	3.808 / 113.8
Sample a from vessel 1 after 1 d	0.063	3.354	3.807 / 113.5
Sample a from vessel 1 after 4 d	0.121	3.374	3.700 / 109.7
Sample a from vessel 1 after 7 d	0.180	3.393	3.832 / 112.9
Sample a from vessel 1 after 14d	0.219	3.406	3.791 / 111.3
Sample a from vessel 1 after 21 d	0.245	3.415	3.817 / 111.8
Sample a from vessel 1 after 28 d	0.234	3.411	3.797 / 111.3
Sample a from vessel 4 after 2h	0.021	3.340	3.314 / 99.2
Sample a from vessel 4 after 6h	0.027	3.342	3.274 / 98.0
Sample a from vessel 4 after 1 d	0.047	3.349	3.303 / 98.6
Sample a from vessel 4 after 4 d	0.123	3.374	3.570 / 105.8
Sample a from vessel 4 after 7 d	0.113	3.371	3.510 / 104.1
Sample a from vessel 4 after 14 d	0.134	3.378	3.632 / 107.5
Sample a from vessel 4 after 21 d	0.159	3.386	3.711 / 109.1
Sample a from vessel 4 after 28 d	0.149	3.383	3.620 / 107.0

  

Recoveries of fortified samples tin (values were rounded, internal calculations were performed with more digits)

sample	Measured concentration [μg M/L]	calculated level after addition [μg M/L]	recovery [μg M/L] / [%]
1 mL of sample + 2 mL of 5 μg Sn/L
Sample a from vessel 1 after 2h	0.176	3.392	3.437 / 101.3
Sample a from vessel 1 after 6h	0.399	3.466	3.463 / 99.9
Sample a from vessel 1 after 1 d	1.457	3.819	3.901 / 102.2
Sample a from vessel 1 after 4 d	2.453	4.151	4.114 / 99.1
Sample a from vessel 1 after 7 d	2.993	4.331	4.338 / 100.2
Sample a from vessel 1 after 14 d	3.845	4.615	4.672 / 101.2
Sample a from vessel 1 after 21 d	4.497	4.832	4.895 / 101.3
Sample a from vessel 1 after 28 d	5.962	5.321	5.360 / 100.7
Sample a from vessel 4 after 2h	0.004	3.335	3.359 / 100.7
Sample a from vessel 4 after 6h	0.064	3.355	3.379 / 100.7
Sample a from vessel 4 after 1 d	0.248	3.416	3.477 / 101.8
Sample a from vessel 4 after 4 d	0.738	3.579	3.733 / 104.3
Sample a from vessel 4 after 7 d	0.510	3.503	3.668 / 104.7
Sample a from vessel 4 after 14 d	0.655	3.552	3.741 / 105.3
Sample a from vessel 4 after 21 d	0.613	3.538	3.578 / 101.1
Sample a from vessel 4 after 28 d	0.444	3.481	3.467 / 99.6

 

Recoveries of fortified samples antimony (values were rounded, internal calculations were performed with more digits)

sample	Measured concentration [μg M/L]	calculated level after addition [μg M/L]	recovery [μg M/L] / [%]
1 mL of sample + 2 mL of 5 μg Sb/L
Sample a from vessel 1 after 2 h	0.010	3.337	3.587 / 107.5
Sample a from vessel 1 after 6 h	0.023	3.341	3.692 / 110.5
Sample a from vessel 1 after 1 d	0.087	3.362	3.705 / 110.2
Sample a from vessel 1 after 4 d	0.256	3.419	3.687 / 107.9
Sample a from vessel 1 after 7 d	0.373	3.458	3.810 / 110.2
Sample a from vessel 1 after 14 d	0.492	3.497	3.779 / 108.1
Sample a from vessel 1 after 21 d	0.647	3.549	3.855 / 108.6
Sample a from vessel 1 after 28 d	0.654	3.551	3.805 / 107.1
Sample a from vessel 4 after 2 h	0.003	3.334	3.503 / 105.1
Sample a from vessel 4 after 6 h	0.016	3.339	3.489 / 104.5
Sample a from vessel 4 after 1 d	0.062	3.354	3.518 / 104.9
Sample a from vessel 4 after 4 d	0.203	3.401	3.682 / 108.3
Sample a from vessel 4 after 7 d	0.238	3.413	3.681 / 107.9
Sample a from vessel 4 after 14 d	0.324	3.441	3.805 / 110.6
Sample a from vessel 4 after 21 d	0.449	3.483	3.818 / 97.7
Sample a from vessel 4 after 28 d	0.437	3.479	3.771 / 98.4

 

Method validation summary:

Validation parameter	results	Comment
selectivity	selective wavelength and isotopes for detection and evaluation of Sn, Sb and V
linearity	applied calibration functions were linear	correlation factor at least 0.9989
limit of detection	Sn: 0.0008 – 0.0046 µg/L Sb: 0.0007 – 0.0026 µg/L V: 0.0006 – 0.0062µg/L Mass balance: V: 0.0918 – 0.2033
limit of quantification	Sn: 0.0023 – 0.0139 µg/L Sb: 0.0021 – 0.0077 µg/L V: 0.0018 – 0.0186µg/L Mass balance: V: 0.2754 – 0.6098
accuracy and precision; repeatability	mean recovery for CRM TM-25.4: Sn: 103.1 ± 2.0 % (n = 28) Sb: 101.9 ± 3.5 % (n = 28) V: 104.3 ± 5.5 % (n = 28)	Diluted (5 fold) to 4.76 µg Sn/L 4.76 µg Sb/L 5.48 µg V/L
accuracy and precision; repeatability	mean recovery for CRM TMDA-53.3: Sn: 102.5 ± 3.0 % (n = 28) Sb: 98.8 ± 3.1 % (n = 28) V: 103.9 ± 4.9 % (n = 28)	Diluted (10 fold) to 1.84 µg Sn/L 1.68 µg Sb/L 31.4 µg V/L
accuracy and precision	mean recovery for CRM TMDA-53.3: Sn: 102.8 ± 3.2 % (n = 11) Sb: 101.0 ± 1.6 % (n = 11) V: 99.9 ± 1.7 % (n = 11)	Diluted (5 fold) to 3.68 µg Sn/L 3.36 µg Sb/L 62.8 µg V/L (only as information – out of calibration but valid)
accuracy and precision	mean recovery for CRM TMDA-53.3: mass balance pH6: V: 98.7 ± 3.3 % (n = 2) mass balance pH8: V: 103.4 ± 6.1 % (n = 4)	Diluted (10 fold) to 31.4 µg V/L
accuracy and precision	mean recovery for CRM TM-25.4: Sn: 101.4 ± 0.9 % (n = 11) Sb: 102.5 ± 1.4 % (n = 11) V: 100.1 ± 2.2 % (n = 11)	Diluted (10 fold) to 2.38 µg Sn/L 2.38 µg Sb/L 2.74 µg V/L
accuracy and precision	mean recovery for CRM TM-25.4: mass balance pH6: V: 101.5 ± 2.4 % (n = 2) mass balance pH 8: V: 97.9 ± 5.8 % (n = 4)	Diluted (5 fold) to 5.48 µg V/L
accuracy and precision	Mean recovery for recalibration standard: Sn: 99.1 ± 2.1 % (n = 18) Sb: 99.5 ± 4.2 % (n = 18) V: 106.1 ± 3.3 % (n = 18) mass balance pH6: V: 102.1 ± 2.8 % (n = 2) mass balance pH 8: V: 101.2 ± 5.6 % (n = 4)	Diluted to 5 µg Sn, Sb, V/L
accuracy and precision; repeatability	Mean recovery for recalibration standard: Sn: 98.8 ± 3.1 % (n = 22) Sb: 100.9 ± 2.5 % (n = 22) V: 98.5 ± 2.8 % (n = 22)	Diluted to 10 µg Sn, Sb, V/L
accuracy and precision; repeatability	Mean recovery for quality control standard QC: Sn: 96.5 ± 2.6 % (n = 22) Sb: 110.6 ± 3.2 % (n = 22) V: 97.0 ± 1.7 % (n = 22)	Diluted to 5 µg Sn, Sb, V/L
accuracy and precision	Mean recovery for quality control standard QC: V: 102.5 ± 3.9 % (n = 10)	Diluted to 10 µg V/L
accuracy and precision	Mean recovery for quality control standard QC1: mass balance pH6: V: 87.5 ± 1.4 % (n = 2)	Diluted to 10 µg Sn, Sb, V/L
trueness	recovery of fortified samples: Sn: 99.1 – 105.3 % (n = 16) Sb: 97.7 – 110.6 % (n = 16) V: 98.0 – 113.8 % (n = 16; only test samples)

Conclusions:

According to the OECD Series on Testing and Assessment Number 29 (2001), dissolved mean Sn, Sb and V concentrations were determined in a transformation/dissolution test with a loading of 1 mg test item (tin antimony grey cassiterite)/L media (agitation at 100 rpm, 21.5 ± 1.5 °C) over 672 hours with samplings after 2 h, 6 h, 24 h, 96 h, 168 h, 332 h, 504 h and 672 h. At a pH of 6, mean Sn, Sb and V concentrations did not exceed 0.566 µg/L irrespective of the test duration (2-672h). Thus, the extent to which tin antimony grey cassiterite can produce soluble available ionic and other metal-bearing species in aqueous media at pH 6, is limited. At pH8, tin antimony grey cassiterite showed low potential to release Sb and V ions - both Sb and V concentrations did not exceed 0.611 µg/L in the aqueous phase irrespective of the test duration (2-672h). Tin concentrations at pH 8 were 1.59 ± 0.218 µg/L, 5.71 ± 2.39 µg/L and 8.89 ± 2.67 µg/L for test durations of 24, 168 and 672 h, respectively.

Reference 2

Endpoint:

transformation / dissolution of metals and inorganic metal compounds

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018-03-01 to 2018-03-13

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

GLP compliance:

yes (incl. QA statement)

Type of method:

flask method

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

3.13 µg/L

Element analysed:

V

Loading of aqueous phase:

100 mg/L

Incubation duration:

24 h

Test conditions:

pH 8, 0.2 µm filtration

Remarks on result:

other: SD ± 0.13 µg/L

Remarks:

LOD: 0.002 µg/L, LOQ: 0.005 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

4.51 µg/L

Element analysed:

V

Loading of aqueous phase:

100 mg/L

Incubation duration:

168 h

Test conditions:

pH 8, 0.2 µm filtration

Remarks on result:

other: SD ± 0.41 µg/L

Remarks:

LOD: 0.002 µg/L, LOQ: 0.005 µg/L

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

0.342 µg/L

Element analysed:

Sb

Loading of aqueous phase:

100 mg/L

Incubation duration:

24 h

Test conditions:

pH 8, 0.2 µm filtration

Remarks on result:

other: SD ± 0.042

Remarks:

LOD: 0.002 µg/L, LOQ: 0.006 µg/L, background corrected

Key result

Type of test:

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

Mean dissolved conc.:

2.57 µg/L

Element analysed:

Sb

Loading of aqueous phase:

100 mg/L

Incubation duration:

168 h

Test conditions:

pH 8, 0.2 µm filtration

Remarks on result:

other: SD ± 0.80

Remarks:

LOD: 0.002 µg/L, LOQ: 0.006 µg/L, background corrected

Type of test:

screening transformation/dissolution test - sparingly soluble metal compounds

Mean dissolved conc.:

1.27 µg/L

Element analysed:

Sn

Loading of aqueous phase:

100 mg/L

Incubation duration:

24 h

Test conditions:

pH 8, 0.2 µm filtration

Remarks on result:

other: SD ± 0.13

Remarks:

LOD: 0.005 µg/L, LOQ: 0.016 µg/L

Key result

Type of test:

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

Mean dissolved conc.:

8.26 µg/L

Element analysed:

Sn

Loading of aqueous phase:

100 mg/L

Incubation duration:

168 h

Test conditions:

pH 8, 0.2 µm filtration

Remarks on result:

other: SD ± 2.19

Remarks:

LOD: 0.002 µg/L, LOQ: 0.006 µg/L, background corrected

Details on results:

Temperature
The temperature of the thermostatically controlled room was recorded with a data logger. The mean temperatures were 21.2 ± 0.3 °C for the pH 8 Test. Therefore, the mean temperature is in agreement with the OECD guidance document 29.

Solution pH and oxygen concentrations
In solutions containing 100 mg/L of the test item at pH 8 as well as in method blanks (BW) the pH ranged from 7.86 to 7.95. Oxygen levels for test item loaded samples and method blanks ranged from 8.12 to 8.15 ppm and from 8.08 – 8.15, respectively.

Mass balance
Total dissolved vanadium, tin and antimony concentrations in vessels, filters and syringes as measured by ICP-OES indicate an incomplete dissolution of the inorganic pigment IPC-2018-003 (Tin antimony grey cassiterite) in the aqueous media after addition of aqua regia to the sample vessels. For the determination of the mass balance two elements were chosen (V) for reporting the recovery. The recovery of vanadium was below 1% in all vessels, indicating that aqua regia is not sufficient for a complete dissolution of the test item. This was not unexpected since inorganic pigments are known for their low dissolution.

Within-vessel variation and between-vessel variation
According to the guidance, it is reasonable to anticipate that for a constant loading of a
substance, tested in a narrow particle size (e.g. 37 - 44 μm) and total surface area range, the within-vessel variation in transformation data should be less than 10% and the between-vessel variation should be less than 20 %. For these samples the observed variations of > 10 % (within-vessel) were all in the recommended range. The between vessel variation for Sb and Sn (7d), however, was not in the recommended range of < 20%.

Background corrections:
Reported values are background-corrected when feasible (method blank values > LOD, see below)

ICP-OES, mass balance samples

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

Limit of detection (LOD): 0.285 µg V /L

Limit of quantification (LOQ): 0.854 µg V/L

Correlation coefficients (r) within all measurement series: > 0.99986

Method validation summary

Mean recovery of fortified sample (n = 1): 101 %

Mean recoveries for certified reference material TM-26.4 (12.6 µg V/L, n = 4): 109 %

Mean recoveries for quality control standard (LabKings) (8 µg/L, n = 4): 102 %

Mean recoveries for recalibration standard (40 µg/L, n=4): 98.2 %

ICP-MS

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

Limit of detection (LOD): 0.002 µg V/L, 0.005 µg Sn/L, 0.002 µg Sb/L

Limit of quantification (LOQ): 0.005 µg V/L, 0.016 µg Sn/L, 0.006 µg Sb/L

Correlation coefficients (r) within all measurement series: > 0.9999

Method validation summary

Mean recovery of fortified sample (n = 1 per element):

V: 108%, Sn: 101%, Sb: 100%

Mean recoveries for certified reference material TM-26.4 (12.6 µg V/L, 5.78 µg Sn/L, 2.8 µg Sb/L, n = 4): 97.5 - 106 %

Mean recoveries for quality control standard (LabKings) (2 and 10 µg/L assessed with n=4 for each concentration):

V: 110-114 %, Sn: 104-108 %, Sb: 98.3-101 %

Mean recoveries for recalibration standard: 94-101 % (assessed with n=4 for each element)

Method blank means (pH 8)

V: All method blanks below LOD/LOQ

Sb: 0.009 ± 0.001 µg/L (24h); 0.010 ± 0.002 µg/L (7d)

Sn: All method blanks below LOD/LOQ (24h); 0.026 ± 0.02 µg/L (7d)

Conclusions:

According to the OECD Series on Testing and Assessment Number 29 (2001), dissolved mean Sn, Sb and V concentrations were determined at pH 8 in a transformation/dissolution test with a loading of 100 mg test item (tin antimony grey cassiterite) /L media (agitation at 100 rpm, 21.2 ± 0.3 °C) over 168 hours with samplings after 24 h and 168 h. After 24h in the test media at pH 8, the mean vanadium concentrations in the aqueous phase (separated by 0.2 µm filtration) were 3.13 ± 0.13 µg/L and increased to 4.51 ± 0.41 µg/L after 7 days of incubation. Antimony concentrations increased from 0.342 (24h, background corrected) to 2.57 µg/L (7 days). In addition, Tin concentrations of 1.27 ± 0.13 µg/L and 8.26 µg/L (background corrected) were determined after 24 h and 7 days, respectively.

Description of key information

The transformation/dissolution test (OECD Series on Testing and Assessment Number 29, 2001) of tin antimony grey casserite at a loading of 1 mg/L resulted in dissolved mean Sn, Sb and V concentrations after 672h of 0.389µg/L (Sn), 0.329µg/L (Sb) and 0.131µg/L (V) at pH6 and 8.895µg/L (Sn), 0.611µg/L (Sb) and 0.205 µg/L (V) at pH8.

The transformation/dissolution test (OECD Series on Testing and Assessment Number 29, 2001) of tin antimony grey casserite at a loading of 100 mg/L at pH8 resulted in dissolved mean Sn, Sb and V concentrations of 8.26 µg/L (Sn), 2.57µg/L (Sb) and 4.51µg/L (V).