Aluminum magnesium vanadium oxide

Water solubility

Link to relevant study record(s)

Reference

Reference 1

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2011

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: Comparable to guideline study with acceptable restrictions

Qualifier:

according to guideline

Guideline:

OECD Guideline 105 (Water Solubility)

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Type of method:

flask method

Water solubility:

< 0.1 mg/L

Conc. based on:

element (dissolved fraction)

Remarks:

several elements have been measured

Loading of aqueous phase:

0.1 g/L

Incubation duration:

4 d

Remarks on result:

other: temperature and pH was not given

Results of solubility pre-tests

Added volume of water (mL)	0.1	0.5	1	2	10	100	1000
Dissolution	/	/	/	/	/	/	/

 

None of the prepared solutions, including the 10.8 mg/L (nominal) solution was clear. In all cases a suspension was obtained.

Results of ICP measurements of a saturated solution

The concentrations in the saturated solution (103.6 mg/L nominal), measured by the sponsor, are presented in the following table:

Element	Concentration (ppm)
Al	<1
Ca	3
Ce	<1
Cu	<1
Fe	<1
Gd	<1
K	<1
La	<1
Mg	1
Na	<1
Nd	<1
P	<1
Pr	<1
Sum of rare earth	0
SO4	<1
Si	<1
Sm	<1
Y	<1

 

Only traces of Calcium and Magnesium could be detected, all other elements were below the detection limit of 1 ppm. Therefore the solubility of the test substance can be stated as lower than 0.1 mg/L.

Reference 2

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

Experimental starting date: 18 Jul 2013, experimental completion date: 21 Aug 2013

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: GLP-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:

Landesamt für Umwelt, Wasserwirtschaft und Gewerbeaufsicht, Kaiser-Friedrich-Straße 7, 55116 Mainz, Germany

Type of method:

other: ICP-OES

Water solubility:

5 µg/L

Conc. based on:

element (dissolved fraction)

Remarks:

Aluminium

Loading of aqueous phase:

0.1 mg/L

Incubation duration:

>= 21 - <= 28 d

Temp.:

22 °C

pH:

8

Remarks on result:

other: the concentration of Al at loading rate 0.1 mg/L (test item), 28 days

Water solubility:

44.7 µg/L

Conc. based on:

element (dissolved fraction)

Remarks:

Aluminium

Loading of aqueous phase:

1 mg/L

Incubation duration:

>= 21 - <= 28 d

Temp.:

22 °C

pH:

8

Remarks on result:

other: the concentration of Al at loading rate 1 mg/L (test item), 28 days

Water solubility:

< 1 µg/L

Conc. based on:

element (dissolved fraction)

Remarks:

Vanadium

Loading of aqueous phase:

0.1 mg/L

Incubation duration:

>= 7 - <= 28 d

Temp.:

22 °C

pH:

8

Remarks on result:

other: the concentration of V at loading rate 0.1 mg/L (test item), 28 days

Water solubility:

6 µg/L

Conc. based on:

element (dissolved fraction)

Remarks:

Vanadium

Loading of aqueous phase:

1 mg/L

Incubation duration:

>= 7 - <= 28 d

Temp.:

22 °C

pH:

8

Remarks on result:

other: the concentration of V at loading rate 1 mg/L (test item), 28 days

The preliminary study was performed with 100 mg/L test item (nominal) at three different pH values (6.09, 7.07 and 8.0, nominal) over a period of 24 hours. The highest concentrations of Vanadium and Aluminium were measured at pH 8 (125 μg/L V) and (315 μg/L Al), respectively. Therefore, after consultation with the sponsor, pH 8.0 was chosen for the main study based on the measured amounts of Al and V.

 

The main study was performed with two different loading concentrations of the test item (0.1 and 1 mg/L, three replicates each) over a period of 28 days. The temperature lay in the range 20.0 – 22.8 °C. On days 2, 14 and 21, pH adjustment was performed

after sampling as the values in all flasks before adjustment lay at the limit of the range 8.0 ± 0.2 (7.8).

In the period of 0 – 14 days, the measurements of Aluminium in flasks 3 – 6 (0.1 mg/L test item, nominal) lay below the LOQ of Al (< 2.5 μg/L). On days 21 and 28, values lay at the LOQ of Al in the range 3.6 – 6.8 μg/L. In flasks 1 – 2 (blanks), the concentration of Al on days 21 and 28 was below LOQ of Al < 2.5 μg/L (1.7 μg/L, mean of days 21 and 28). The within- and between-vessel variation for the values in the flasks 3 – 6 (Al) was higher than 10 % and 20 %, respectively, as the measurements of Aluminium in this very low range were inexact and the risk of carryover for elements like Aluminium is high.

 

Fl.	Content	Conc.on day 7 [µg/L]	Conc.on day 14 [µg/L]	Conc.on day 21 [µg/L]	Conc.on day 28 [µg/L]
1-2	-	< 1	< 1	< LOQ (1.5)	< LOQ (1.9)
3	0.1 mg/L	< 1	< 1	4.5	3.6
4	0.1 mg/L	< 1	< 1	4.0	5.8
5	0.1 mg/L	2.9	2.7	6.2	6.8
6	0.1 mg/L	1.9	< 1	4.8	4.6
Mean [µg/L]		-	-	4.8	5.2
RSD [%]		-	-	19.5 %	27.3 %
Measured Concentration of Aluminium, Mean (days 21, 28) [µg/L]					5.0
Standard deviation (days 21, 28, flasks 3 – 6) [µg/L]					1.13
Relative Standard Deviation (days 21, 28, flasks 3 – 6) [%]					22.5 %

 

The concentrations of Aluminium in flasks 7 – 10 increased over a period of seven days from 3.5 μg/L to 36.3 μg/L. On day 14, the concentration of Aluminium was slightly lower than on day 7, as 50 mL medium were added on day 7 after sampling (replenishing as demanded in guideline). The measured concentrations of Aluminium on days 21 and 28 in flasks 7 – 10 (1 mg/L, nominal) were nearly identical. Therefore, all values on days 21 and 28 were used in calculation of the mean. The within- and between-vessel variations for the values in the flasks 7 – 10 (21 and 28 d) were lower than 10 % and 20 %, respectively.

Fl.	Content	Conc.after 6 h [µg/L]	Conc.on day 1 [µg/L]	Conc.on day 2 [µg/L]	Conc.on day 7 [µg/L]	Conc.on day 14 [µg/L]	Conc.on day 21 [µg/L]	Conc.on day 28 [µg/L]
7	1 mg/L	2.1	9.2	16.7	32.6	27.0	40.8	40.8
8	1 mg/L	4.6	15.3	20.8	40.6	39.5	50.8	49.4
9	1 mg/L	4.0	9.8	17.3	35.0	33.5	43.6	42.1
10	1 mg/L	3.4	11.4	16.4	37.2	35.1	45.9	44.2
Mean [µg/L]		3.5	11.4	17.8	36.3	33.8	45.3	44.1
RSD [%]		31.2 %	24 %	11.4 %	9.4 %	15.4 %	9.3 %	8.6 %
Measured Concentration of Aluminium, Mean (days 21, 28) [µg/L]								44.7
Standard deviation (days 21, 28) [µg/L]								3.76
Relative Standard Deviation (days 21, 28) [%]								8.4 %

 

Therefore, the concentration of Aluminium was stated as:

 

5.0 µg/L Al at 20.0 – 22.8 °C = 5.0 * 10^-6kg/m³(SI units) for the nominal concentration of the test item 0.1 mg/L

44.7 µg/L Al = 44.7 * 10^-6kg/m³(SI units)for the nominal concentration of the test item 1 mg/L

 

For the nominal concentration 0.1 mg/L, the concentration of Vanadium lay below the lowest calibration level 1 µg/L.

The concentrations of Vanadium in the flasks 7 – 10 increased over a period of two days from 1.3 µg/L to 4.9 µg/L. The measured concentrations of Vanadium on days 7, 14, 21 and 28 in flasks 7 – 10 (1 mg/L, nominal) were nearly identical. Therefore, all values on days 7, 14, 21 and 28 were used in calculation of the mean. Both conditions for the RSD (< 10 % within-vessel and < 20 % between-vessel) were fulfilled for Vanadium in flasks 7 – 10.

Fl.	Content	Conc.after 2 h [µg/L]	Conc.after 6 h [µg/L]	Conc.on day 1 [µg/L]	Conc.on day 2 [µg/L]	Conc.on day 7 [µg/L]	Conc.on day 14 [µg/L]	Conc.on day 21 [µg/L]	Conc.on day 28 [µg/L]
7	1 mg/L	1.3	2.3	4.0	4.8	6.1	6.1	5.9	6.0
8	1 mg/L	1.5	2.6	4.5	5.3	6.4	6.4	6.4	6.2
9	1 mg/L	1.2	2.3	4.0	4.7	5.5	5.5	5.5	5.5
10	1 mg/L	1.4	2.2	4.2	4.9	6.0	6.2	6.1	6.1
Mean [µg/L]		1.3	2.3	4.2	4.9	6.0	6.0	6.0	5.9
RSD [%]		10.9 %	7.7 %	5.1 %	5.9 %	6.6 %	6.8 %	6.4 %	4.9 %
Measured Concentration of Vanadium, Mean (days 7, 14, 21, 28) [µg/L]									6.0
Standard deviation (days 7, 14, 21, 28) [µg/L]									0.335
Relative Standard Deviation (days 7, 14, 21, 28) [%]									5.6 %

 

Therefore, the concentration of Vanadium was stated as:

 

< 1 µg/L V = 1 * 10^-6kg/m³(SI units) for the nominal concentration of the test item 0.1 mg/L

6.0 µg/L V = 6.0 * 10^-6kg/m³(SI units) for the nominal concentration of the test item 1 mg/L

Reference 3

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

disregarded due to major methodological deficiencies

Study period:

13 Jun 2012 - 20 Dec 2012

Reliability:

3 (not reliable)

Rationale for reliability incl. deficiencies:

other: Inconsistent results and partly standard deviations of measured concentration are not valide.

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:

: Test samples were not kept at a consistent temperature throughout the test period.

GLP compliance:

yes (incl. QA statement)

Remarks:

Landesamt für Umwelt, Wasserwirtschaft und Gewerbeaufsicht, Kaiser-Friedrich-Strasse 7, D-55116 Mainz, Germany

Water solubility:

38.1 µg/L

Temp.:

19.3 °C

pH:

8

Remarks on result:

other: Based on the detected aluminium concentration after 28 days and for the nominal concentration of 1 mg/L test item, temperature range 19.3- 22.1 °C

Water solubility:

5.4 µg/L

Temp.:

19.3 °C

pH:

8

Remarks on result:

other: Based on the detected vanadium concentration after 28 days and for the nominal concentration of 1 mg/L test item, temperature range 19.3- 22.1 °C

Results for Aluminium

The measured concentrations of Aluminium on days 7, 14, 21 and 28 are presented in the following table.

Concentration of Aluminium on Days 14, 21 and 28

Fl.	Content	Conc. Aluminium on day 7	Conc. Aluminium on day 14	Conc. Aluminium on day 21	Conc. Aluminium on day 28
		[µg/L]	[µg/L]	[µg/L]	[µg/L]
3	0.1 mg/L	10.9	13.2	10.4	7.7
4	0.1 mg/L	21.9	27.0	25.2	23.3
5	0.1 mg/L	26.6	31.8	29.0	33.6
6	1 mg/L	21.4	30.8	28.6	30.5
7	1 mg/L	27.4	38.0	39.6	40.6
8	1 mg/L	34.5	41.2	44.3	49.7
Measured Concentration of Aluminium on days 14, 21 and 28, Mean (flasks 3 – 5) [µg/L]					22.3
Standard deviation (Flasks 3 – 5) [µg/L]					9.564
Relative Standard Deviation (Flasks 3 – 5) [%]					43 %
Measured Concentration of Aluminium on days 14, 21 and 28 Mean (flasks 6 – 8) [µg/L]					38.1
Standard deviation (Flasks 6 – 8) [µg/L]					7.008
Relative Standard Deviation (Flasks 6 – 8 ) [%]					18 %

 

On day 7 the measured concentration of Aluminium in flasks 3 – 4 (0.1 mg/L test item, nominal) and 6 – 8 (1 mg/L test item, nominal) was 19.8 μg/L and 27.8 μg/L, respectively.

The measured concentration of Aluminium in flasks 6 – 8 (1 mg/L test item, nominal) on days 14, 21 and 28 was38.1 μg/L at 19.3 – 22.1°C = 3.81* 10-5 kg/m3 (SI units) (nominal load 1 mg/L, mean value of three individual vessels, seventeen values)

 

The results of the measured concentrations of Aluminium in the test item solutions with the nominal concentration 0.1 mg/L are not valid, as the relative standard deviation between vessels was higher than 20 % (43 %).

Results for Vanadium

The measured concentrations of Vanadium on days 7, 14, 21 and 28 are presented in the following table.

 

Concentration of Vanadium on Days 14, 21 and 28

Fl.	Content	Conc. Vanadium on day 7	Conc. Vanadium on day 14	Conc. Vanadium on day 21	Conc. Vanadium on day 28
		[µg/L]	[µg/L]	[µg/L]	[µg/L]
3	0.1 mg/L	1.3	1.0	1.2	1.2
4	0.1 mg/L	2.9	2.9	3.0	2.9
5	0.1 mg/L	3.4	3.4	3.5	3.4
6	1 mg/L	4.5	5.3	5.1	4.9
7	1 mg/L	4.9	5.2	5.3	5.3
8	1 mg/L	5.8	5.8	6.1	6.1
Measured Concentration ofVanadiumon days 14, 21 and 28, Mean (flasks 3 – 5) [µg/L]					2.5
Standard deviation (Flasks 3 – 5) [µg/L]					1.049
Relative Standard Deviation (Flasks 3 – 5) [%]					42 %
Measured Concentration ofVanadiumon days 14, 21 and 28 Mean (flasks 6 – 8) [µg/L]					5.4
Standard deviation (Flasks 6 – 8) [µg/L]					0.436
Relative Standard Deviation (Flasks 6 – 8 ) [%]					8 %

 

On day 7 the measured concentration of Vanadium in flasks 3 – 4 (0.1 mg/L test item, nominal) and 6 – 8 (1 mg/L test item, nominal) was 2.5 μg/L and 5.0 μg/L, respectively. The measured concentration of Vanadium in flasks 6 – 8 (1 mg/L test item, nominal) on days 14, 21 and 28 was5.4 μg/L at 19.3 – 22.1°C = 5.4* 10-6 kg/m3 (SI units) (nominal load 1 mg/L, mean value of three individual vessels, eighteen values).

 

The results of the measured concentrations of Vanadium in the test item solutions with the nominal concentration 0.1 mg/L are not valid, as the relative standard deviation between vessels was higher than 20 % (42 %). Furthermore, the measurements of Vanadium at the LOQ (1 μg/L) are inexact.

Reference 4

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

supporting study

Study period:

07 - 16 Jan 2014

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: GLP-guideline study with reported deviation (main study was performed at pH=7, defined value)

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:

: main study was perforned at pH=7 (definded value)

Qualifier:

according to guideline

Guideline:

other: OECD Guidance Document No. 98 "Considerations Regarding Applicability on the Guidance of Transformation/Dissolution of Metals and Metal Compounds in Aqueous Media"

GLP compliance:

yes (incl. QA statement)

Remarks:

Landesamt für Umwelt, Wasserwirtschaft und Gewerbeaufsicht, Kaiser-Friedrich-Straße 7, 55116 Mainz, Germany

Type of method:

other: ICP-OES

Water solubility:

14.6 µg/L

Temp.:

20.5 °C

pH:

7

Remarks on result:

other: the concentration of Al at loading rate 1 mg/L (test item), day 7

Water solubility:

< 0.9 µg/L

Temp.:

20.7 °C

pH:

7

Remarks on result:

other: the concentration of Al at loading rate 0.1 mg/L (test item), day 7

Water solubility:

3.9

Temp.:

20.5

pH:

7

Remarks on result:

other: the concentration of V at loading rate 1 mg/L (test item), day 7

Water solubility:

< 1 µg/L

Temp.:

20.7 °C

pH:

7

Remarks on result:

other: the concentration of V at loading rate 0.1 mg/L (test item), day 7

Details on results:

The pH values in all flask lay within the demanded range 7.0 ± during the test.
The temperature lay in the range 20.2-21.1 °C.

 Analysis for Aluminium:

Flask #	Nominal load / [mg/L]	Conc. after 0 h [µg/L]	Conc. after 2 h [µg/L]	Conc. after 6 h [µg/L]	Conc. after 1 d [µg/L]	Conc. after 4 d [µg/L]	Conc. after 7 d [µg/L]
1	0	<1	<1	<1	<1	<1	<1
	0	<1	<1	<1	<1	<1	<1
2	0	<1	<1	<1	<1	<1	<1
	0	<1	<1	<1	<1	<1	<1
3	0.1	<1	<1	<1	<1	<1	<1
	0.1	<1	<1	<1	<1	<1	<1
4	0.1	<1	<1	<1	<1	<1	<1
	0.1	<1	<1	<1	<1	<1	<1
5	0.1	<1	<1	<1	<1	<1	<1
	0.1	<1	<1	<1	<1	<1	<1
6	1.0	<1	<1	<1	<1	11.0	15.1
	1.0	<1	<1	<1	<1	11.5	16.2
7	1.0	<1	<1	<1	<1	10.5	11.7
	1.0	<1	<1	<1	<1	10.6	12.8
8	1.0	<1	<1	<1	<1	11.6	15.6
	1.0	<1	<1	<1	<1	12.3	16.2
Mean [µg/L], flask 6-8						11.2	14.6
RSD						6.1%	14%

 

The concentration of Aluminium on day 7 was 14.6 µg/L for the nominal concentration the test item 1 mg/L. In flask 3-5 (0.1 mg/L nominal) the concentration of Aluminium was lower than the LOQ of Al ( 0.9 µg/L).

Analysis for Vanadium

Flask #	Nominal load / [mg/L]	Conc. after 0 h [µg/L]	Conc. after 2 h [µg/L]	Conc. after 6 h [µg/L]	Conc. after 1 d [µg/L]	Conc. after 4 d [µg/L]	Conc. after 7 d [µg/L]
1	0	<1	<1	<1	<1	<1	<1
	0	<1	<1	<1	<1	<1	<1
2	0	<1	<1	<1	<1	<1	<1
	0	<1	<1	<1	<1	<1	<1
3	0.1	<1	<1	<1	<1	<1	<1
	0.1	<1	<1	<1	<1	<1	<1
4	0.1	<1	<1	<1	<1	<1	<1
	0.1	<1	<1	<1	<1	<1	<1
5	0.1	<1	<1	<1	<1	<1	<1
	0.1	<1	<1	<1	<1	<1	<1
6	1.0	<1	<1	1.3	1.9	2.9	3.9
	1.0	<1	<1	1.3	1.8	3.0	3.7
7	1.0	<1	<1	1.3	2.0	3.2	4.1
	1.0	<1	<1	1.2	2.1	3.5	4.0
8	1.0	<1	1.2	1.9	2.3	3.5	3.7
	1.0	<1	1.2	1.5	2.6	3.5	4.0
Mean [µg/L], flask 6-8	-		-	1.4	2.1	3.3	3.9
RSD				17%	14%	9%	3%

 

No linear dependency of the measured concentration against time was observed. For the nominal concentration 0.1 mg/L (flask 3-5), the concentration of Vanadium lay below the lowest calibration level (>1 µg/L).

The relative standard deviation of the values in the flask 8 (within vessels) was higher than 10% for Vanadium after 6 h. This was considered as uncritical as the measured values for Vanadium after 6 h were below of LOQ of V (<2.2 µg/L) 

Description of key information

The solubility of the substance is stated as < 0.1 mg/L in the water solubility test (OECD 105). 
Transformation/dissolution test:
5.0 µg/L Al and < 1 µg/L V at a nominal concentration of 0.1 mg/L test item, at 20-22.8 °C and pH 8; 28 days
44.7 µg/L Al and 6.0 µg/L V at a nominal concentration of 1 mg/L test item, at 20-22.8 °C and pH 8; 28 days
<0.9 µg/L Al and <1.0 µg/L V at a nominal concentration of 0.1 mg/L test item, at 20.2-21.1 °C and pH 7; 7 days
14.6 µg/L Al and 3.9 µg/L V at a nominal concentration of 1 mg/L test item, at 20.2-21.1 °C and pH 7; 7days

Additional information

The water solubility of the test substance was determined under flask conditions according to OECD guideline 105.

The first transformation/dissolution in aqueous media of Aluminium magnesium vanadium oxide was determined according to OECD SERIES ON TESTING AND ASSESSMENT No. 29 in 2012. Not all the validity criteria were met for the transformation /dissolution test. The results of the measured concentrations of aluminium and vanadium in the test item solutions with the nominal concentration 0.1 mg/L are not valid, as the relative standard deviation (RSD) between vessels was higher than 20% (43% and 42% respectively).

 

Therefore a repeated transformation /dissolution test according to the OECD SERIES ON TESTING AND ASSESSMENT No. 29 was performed in 2013. Only the RSDs within- and between-vessels were higher than 10% and 20% in the measurements of Al at the loading rate of 0.1 mg/L test item, in all the other measurements the RSDs within- and between- vessel were lower than 10% and 20%, respectively. Due to the low determination range (< 10 µg/L), the inexact measurements of Al was acceptable.

The supporting study from 2014 at pH=7 (definded value); 7 days shows that the concentrations of Aluminium and Vanadium, respectively are below the concentrations observed at pH 8 after 28 days in 2013 (2013a study).