Slags, tin-smelting

Water solubility

Administrative data

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

04 June 2013

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Study was generated according to internationally accepted guideline (OECD 29).

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2014

Materials and methods

Test guideline

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:

yes

Remarks:

Within-vessel variation was not calculated for short term test. Reason for deviation: Relative standard deviation of two values is not significant. Impact on study: None

GLP compliance:

yes (incl. QA statement)

Type of method:

other: transformation/dissolution test

Test material

Test material information

Constituent 1

Reference substance name:

Slags, tin-smelting

EC Number:

273-736-5

EC Name:

Slags, tin-smelting

Cas Number:

69012-35-7

Molecular formula:

Since slags are characterised as inorganic UVCB substances, no exact molecular formula can be defined.

IUPAC Name:

bicyclo[1.1.1]diferroxane; oxo[(oxoalumanyl)oxy]alumane; oxocalcium; silanedione

Test material form:

solid: particulate/powder

Remarks:

migrated information: powder

Details on test material:

- Name of test material (as cited in study report): Slags, tin-smelting
- Molecular formula (if other than submission substance): not applicable
- Smiles notation (if other than submission substance): not applicable
- InChl (if other than submission substance): not applicable
- Structural formula attached as image file (if other than submission substance): not applicable
- Substance type: inorganic
- Physical state: solid
- Analytical purity: provided by sponsor in form of certificate of analysis
- Lot/batch No.: 2401213
- Expiration date of the lot/batch: 15 April 2015
- Storage condition of test material: room temperature

Results and discussion

Water solubility

Water solubility 1

Water solubility:

> 0 - <= 7.79 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Al (highest mean concentration in short-term test)

Water solubility 2

Water solubility:

0.67 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Ti (highest mean concentration in short-term test)

Water solubility 3

Water solubility:

> 0 - < 0.536 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Cr (highest mean concentration in short-term test)

Water solubility 4

Water solubility:

0.73 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Mn (highest mean concentration in short-term test)

Water solubility 5

Water solubility:

> 0 - <= 12.5 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Fe (highest mean concentration in short-term test)

Water solubility 6

Water solubility:

> 0.172 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Zr (highest mean concentration in short-term test)

Water solubility 7

Water solubility:

> 0 - <= 0.111 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Nb (highest mean concentration in short-term test)

Water solubility 8

Water solubility:

1 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Sn (highest mean concentration in short-term test)

Water solubility 9

Water solubility:

> 0 - < 0.26 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Ce (highest mean concentration in short-term test)

Water solubility 10

Water solubility:

> 0 - < 0.1 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Ta (highest mean concentration in short-term test)

Water solubility 11

Water solubility:

> 0 - <= 6 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: W (highest mean concentration in short-term test)

Water solubility 12

Water solubility:

> 0 - < 100 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Si (highest mean concentration in short-term test)

Water solubility 13

Water solubility:

> 0 - < 100 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Na (highest mean concentration in short-term test)

Water solubility 14

Water solubility:

> 0 - < 100 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Mg (highest mean concentration in short-term test)

Water solubility 15

Water solubility:

141 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: K (highest mean concentration in short-term test)

Water solubility 16

Water solubility:

560 µg/L

Temp.:

20 °C

pH:

6

Remarks on result:

other: Ca (highest mean concentration in short-term test)

Details on results:

PRELIMINARY TEST
pH that maximizes the Concentration:
Al, Ce, Cr, Fe, Mn, Nb, Si, Sn, Ta, Ti, W and Zr was not detected in buffer before addition of test item. Therefore no blank had to be subtracted from element concentration. If no element is detected before and after addition of test item, concentration will be reported as < lowest standard concentration.

The test was performed according to the description in the report obtaining the following results:

Table 1: Results preliminary test – concentration of aluminium after 24h shaking

pH Test Item Time of shaking Remarks Aluminium concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed 3.93
3.92

7 100.5 24 no solution observed 2.22
2.66

8 101.0 24 no solution observed 2.60
2.53
............................................................................................................................................................................................................
LOQ= Limit of quantification (6.7 µg/L Al)


Table 2: Results preliminary test – concentration of titanium after 24h shaking

pH Test Item Time of shaking Remarks Titanium concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed 0.319
1.06

7 100.5 24 no solution observed 0.182
n.d.

8 101.0 24 no solution observed < 0.1
0.110
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Ti)
LOQ= Limit of quantification (0.3 µg/L Ti)

Table 3: Results preliminary test – concentration of chromium after 24h shaking

pH Test Item Time of shaking Remarks Chromium concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed < 0.1
< 0.1

7 100.5 24 no solution observed < 0.1
< 0.1

8 101.0 24 no solution observed < 0.1
< 0.1
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Cr)
LOQ= Limit of quantification (0.3 µg/L Cr)


Table 4: Results preliminary test – concentration of manganese after 24h shaking

pH Test Item Time of shaking Remarks Manganese concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed 0.909
0.909

7 100.5 24 no solution observed 0.254
0.251

8 101.0 24 no solution observed 0.182
0.208
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Mn)
LOQ= Limit of quantification (0.3 µg/L Mn)


Table 5: Results preliminary test – concentration of iron after 24h shaking

pH Test Item Time of shaking Remarks Iron concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed 7.56
7.75

7 100.5 24 no solution observed < 2
3.00

8 101.0 24 no solution observed < 2
< 2
............................................................................................................................................................................................................
n.d.= not detectable (< 2 µg/L Fe)
LOQ= Limit of quantification (6.7 µg/L Fe)


Table 6: Results preliminary test – concentration of zirconium after 24h shaking

pH Test Item Time of shaking Remarks Zirconium concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed 0.196
< 0.1

7 100.5 24 no solution observed < 0.1
< 0.1

8 101.0 24 no solution observed < 0.1
< 0.1
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Zr)
LOQ= Limit of quantification (0.3 µg/L Zr)


Table 7: Results preliminary test – concentration of niobium after 24h shaking

pH Test Item Time of shaking Remarks Niobium concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed < 0.1
< 0.1

7 100.5 24 no solution observed < 0.1
< 0.1

8 101.0 24 no solution observed < 0.1
< 0.1
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Nb)
LOQ= Limit of quantification (0.3 µg/L Nb)


Table 8: Results preliminary test – concentration of tin after 24h shaking

pH Test Item Time of shaking Remarks Tin concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed 1.21
1.07

7 100.5 24 no solution observed 0.449
0.484

8 101.0 24 no solution observed 0.365
0.472
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Sn)
LOQ= Limit of quantification (0.3 µg/L Sn)


Table 9: Results preliminary test – concentration of cerium after 24h shaking

pH Test Item Time of shaking Remarks Cerium concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed < 0.1
< 0.1

7 100.5 24 no solution observed < 0.1
< 0.1

8 101.0 24 no solution observed < 0.1
< 0.1
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Ce)
LOQ= Limit of quantification (0.3 µg/L Ce)


Table 10: Results preliminary test – concentration of tantalum after 24h shaking

pH Test Item Time of shaking Remarks Tantalum concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed < 0.1
< 0.1

7 100.5 24 no solution observed < 0.1
< 0.1

8 101.0 24 no solution observed < 0.1
< 0.1
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 µg/L Ta)
LOQ= Limit of quantification (0.3 µg/L Ta)


Table 11: Results preliminary test – concentration of silicon after 24h shaking

pH Test Item Time of shaking Remarks Silicon concentration (µg/L)
added (mg/L) (h)
............................................................................................................................................................................................................
6 100.0 24 no solution observed < 0.1
< 0.1

7 100.5 24 no solution observed < 0.1
< 0.1

8 101.0 24 no solution observed < 0.1
< 0.1
............................................................................................................................................................................................................
n.d.= not detectable (< 0.1 mg/L Si)
LOQ= Limit of quantification (0.33 mg/L Si)


Table 12: Results preliminary test – concentration of sodium after 24h shaking

pH Test Item Time of shaking Remarks Found sodium concentration (mg/L) Found sodium conc. Sodium concentration
added (mg/L) (h) in buffer (mg/L) (mg/L), corrected [1]
.....................................................................................................................................................................................................................................................................................................................
6 100.0 24 no solution observed 1.58 1.59 < 0.1
1.59 < 0.1

7 100.5 24 no solution observed 3.42 3.38 < 0.1
3.39 < 0.1

8 101.0 24 no solution observed 18.0 17.7 0.3
17.8 0.1
......................................................................................................................................................................................................................................................................................................................
[1] corrected by blank concentration (buffer)
n.d.= not detectable (< 0.1 mg/L Na)
LOQ= Limit of quantification (0.33 mg/L Na)


Table 13: Results preliminary test – concentration of magnesium after 24h shaking

pH Test Item Time of shaking Remarks Found magnesium concentration Found magnesium conc. Magnesium concentration
added (mg/L) (h) (mg/L) in buffer (mg/L) (mg/L), corrected [1]
.......................................................................................................................................................................................................................................................................................................................
6 100.0 24 no solution observed 1.19 1.20 < 0.1
1.18 < 0.1

7 100.5 24 no solution observed 4.76 4.73 < 0.1
4.71 < 0.1

8 101.0 24 no solution observed 12.1 11.9 0.2
12.0 0.1
........................................................................................................................................................................................................................................................................................................................
[1] corrected by blank concentration (buffer)
n.d.= not detectable (< 0.1 mg/L Mg)
LOQ= Limit of quantification (0.33 mg/L Mg)


Table 14: Results preliminary test – concentration of potassium after 24h shaking

pH Test Item Time of shaking Remarks Found potassium concentration Found potassium conc. Potassium concentration
added (mg/L) (h) (mg/L) in buffer (mg/L) (mg/L), corrected [1]
...........................................................................................................................................................................................................................................................................................................................
6 100.0 24 no solution observed 0.251 0.242 < 0.1
0.241 < 0.1

7 100.5 24 no solution observed 1.29 1.30 < 0.1
1.31 < 0.1

8 101.0 24 no solution observed 3.08 2.99 < 0.1
3.11 0.12
...........................................................................................................................................................................................................................................................................................................................
[1] corrected by blank concentration (buffer)
n.d.= not detectable (< 0.1 mg/L K)
LOQ= Limit of quantification (0.33 mg/L K)


Table 15: Results preliminary test – concentration of calcium after 24h shaking

pH Test Item Time of shaking Remarks Found calcium concentration F ound calcium conc. C alcium concentration
added (mg/L) (h) (mg/L) in buffer (mg/L) (mg/L), corrected [1]
...........................................................................................................................................................................................................................................................................................................................
6 100.0 24 no solution observed 0.251 0.242 < 0.1
0.241 < 0.1

7 100.5 24 no solution observed 1.29 1.30 < 0.1
1.31 < 0.1

8 101.0 24 no solution observed 3.08 2.99 < 0.1
3.11 0.12
...........................................................................................................................................................................................................................................................................................................................
[1] corrected by blank concentration (buffer)
n.d.= not detectable (< 0.1 mg/L Ca)
LOQ= Limit of quantification (0.33 mg/L Ca)

Tungsten could not be determined in preliminary test since no linear or another typical calibration curve was achieved.

Within the tested range from pH 6 to 8, the vessel at pH=6 showed a higher concentration than the others. Therefore the screening test was performed at pH=6.


pH Stability over a one Week Period:
The stability test for the buffered systems showed, that for the salt mixtures given in OECD Guidance Document 29 (pH 6, 7 and 8) and after an equilibration time of 24 hours, the pH values are within the expected range.
It was found that the gas phases need to be replaced, with every sampling time.
Results for the pH stability are shown in the table below:

Table 16: Results pH-stability

Time Temp. (°C) pH 6 Temp. (°C) pH 7 Temp. (°C) pH 8
........................................................................................................................................................................
2 h 22.8 6.2 22.4 6.9 22.5 7.8
6 h 22.2 5.9 21.7 7.1 21.1 7.9
24 h 21.9 6.2 21.5 6.8 21.8 7.9
48 h 22.5 6.1 23.1 6.8 23.2 7.8
168 h 22.5 6.2 22.3 7.2 22.2 7.8

Any other information on results incl. tables

Table 17: Results short-term test after 2h - 168 h shaking

Element	Sample time
	2h	6 h	24 h	48 h	168 h
	Mean conc. ± RSD (µg/L ± %)
Aluminium	≤ 1.78	≤ 1.33	≤ 1.66	≤ 2.80	≤ 7.79
	≤ 1.81	≤ 2.74	≤ 1.88	< 2.24	≤ 2.00
	≤ 2.77	≤ 4.00	≤ 2.34	≤ 2.32	≤ 5.23
Titanium	< 0.1	< 0.1	< 0.1	< 0.1	< 0.254
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	0.670	0.398	< 0.1	< 0.1	< 0.1
Chromium	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	< 0.1	< 0.1	< 0.1	< 0.1	≤ 0.536
	< 0.1	< 0.1	< 0.1	< 0.1	≤ 0.288
Manganese	≤ 0.114	< 0.103	≤ 0.1	< 0.139	< 0.1
	< 0.1	≤ 0.095	< 0.1	< 0.1	< 0.1
	< 0.185	0.300	< 0.1	0.511± 26.6	0.730±9.59
Iron	≤ 2.04	≤ 2.34	< 2.0	≤ 3.14	≤ 12.5
	< 2.0	< 2.0	< 2.0	< 2.0	≤ 1.45
	≤ 1.42	≤ 2.42	≤ 2.79	≤ 3.50	≤ 7.42
Zirconium	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	0.172	0.118	≤ 0.130	< 0.112	< 0.1
Niobium	≤ 0.102	< 0.1	< 0.1	< 0.1	< 0.1
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	≤ 0.111	< 0.1	< 0.1	< 0.1	< 0.1
Tin	< 0.1	0.110	< 0.1	≤ 0.122	< 0.260
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	1.00 ± 10.0	0.826 ± 9.69	0.541 ± 18.1	0.378	< 0.148
Cerium	< 0.1	< 0.1	< 0.1	< 0.130	< 0.260
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	< 0.1	< 0.1	< 0.1	< 0.1	0.178
Tantalum	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
	< 0.1	< 0.1	< 0.1	< 0.1	< 0.1
Tungsten	< 6.0	< 6.0	< 6.0	< 6.0	< 6.0
	< 6.0	< 6.0	< 6.0	< 6.0	< 6.0
	< 6.0	< 6.0	< 6.0	< 6.0	< 6.0
Silicon	< 100	< 100	< 100	< 100	< 100
	< 100	< 100	< 100	< 100	< 100
	< 100	< 100	< 100	< 100	< 100
Sodium	< 100; n.c; < 100	<100; <100; <100	<100; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; <100
	n.c. <100; < 100	<100; n.c.; <100	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; <100; <100
	< 100; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	<100; n.c.; n.c.
Magnesium	n.c.; n.c.; <100	<100; <100; <100	<100; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; <100
	n.c.; <100; <100	<100; <100; <100	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	<100; <100; <100
	<100; n.c.; <100	n.c.; <100; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	<100; <100; <100
Potassium	n.c.; n.c.; <100	n.c.; <100; <100	<100; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.
	<100; n.c.; n.c.	<100; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	<100; n.c.; n.c.
	<100; n.c.; n.c.	<100; n.c.; n.c.	n.c.; n.c.; n.c.	n.c.; n.c.; n.c.	141; n.c.; n.c.
Calcium	310; 230; 180	560; 320; <220	310; 470; n.c.	490; 540; 210	230; 290; n.c.
	300; 280; 190	200; <250; 200	350; 360; 150	470; 270; 180	220; 190; 160
	250; 150; 130	260; 310; 220	150; 230; n.c.	210; 310; 360	300; 470; 370
RSD = relative standard deviation; n.d. = not detectable (0.1 mg/L metal); n.c. = not calculable

Applicant's summary and conclusion

Conclusions:

Interpretation of results (migrated information): other: Due to the water solubility of each of the metal constituents, slags, tin-smelting can be regarded as insoluble.
Due to the complex composition of slags, tin-smelting , determination of the water solubility was performed on the basis of the solubilities of the underlying metals. Concentrations of potassium and calcium have been determined to 141 µg/L and 560 µg/L, respectively, those of sodium, magnesium and silicon were below 100 µg/L and the concentrations of the remaining metals (Al, Ti, Cr, Mn, Fe, Zr, Nb, Sn, Ce, Ta, W) were well below 100 µg/L. Based on these results slags, tin-smelting is characterised as insoluble in water.

Executive summary:

The water solubility of Slags, tin-smelting was determined following OECD guideline 29.

A 24 hour pre-test was performed in aqueous solution at pH = 6, 7 and 8. The solution buffered at pH = 6 was found to be the media that maximised the solubility.

With this buffer a screening transformation/dissolution test was performed to determine the dissolved metal ion concentration in five test vessels with three samples each. Concentrations have been determined by ICP-MS. The test obtained the following results:

Table 1: Summary of dissolved elements in transformation/dissolution test

Element	m/z	Mean concentration of dissolved elements ± RSD (µg/L ± %)
Aluminium (Al)	27	≤ 6.64
Titanium (Ti)	47	≤ 0.182
Chromium (Cr)	53	≤ 0.113
Manganese (Mn)	55	≤ 0.800
Iron (Fe)	56	≤ 11.1
Zirconium (Zr)	90	≤ 0.126
Niobium (Nb)	93	≤ 0.118
Tin (Sn)	118	≤ 0.728 ± 33.2
Cerium (Ce)	140	≤ 0.293
Tantalum (Ta)	181	≤ 0.104
Tungsten (W)	182	≤ 8.07
Sodium (Na)	23	30
Magnesium (Mg)	24	30
Silicon (Si)	28	< 100
Potassium (K)	39	15
Calcium (Ca)	44	130

RSD = relative standard deviation

According to OECD Guidance Document 29, the seven day short term test was performed with loadings of 1, 10 and 100 mg/L at pH 6. The concentrations after 7 days are shown in Table 2.

Table 2: Summary of dissolved elements in short term test

Element	m/z	Highest mean concentration of dissolved elements ± RSD (µg/L ± %)
Aluminium (Al)	27	≤ 7.79
Titanium (Ti)	47	0.670
Chromium (Cr)	53	< 0.1
Manganese (Mn)	55	0.730 ± 9.59
Iron (Fe)	56	≤ 12.5
Zirconium (Zr)	90	0.172
Niobium (Nb)	93	≤ 0.111
Tin (Sn)	118	1.00 ± 10.0
Cerium (Ce)	140	< 0.260
Tantalum (Ta)	181	< 0.1
Tungsten (W)	182	< 6.0
Sodium (Na)	23	60
Magnesium (Mg)	24	40
Silicon (Si)	28	< 100
Potassium (K)	39	101
Calcium (Ca)	44	560

RSD = relative standard deviation