Manganese neodecanoate

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018-01-16 to 2018-02-23

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:

Two vessels were set up in a parallel design under argon, each vessel was sampled several times instead of sampling one single vessel at each point in time.

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

2008

Deviations:

yes

Remarks:

Two vessels were set up in a parallel design under argon, each vessel was sampled several times instead of sampling one single vessel at each point in time.

GLP compliance:

yes (incl. QA statement)

Remarks:

signed 2016-05-31

Type of method:

flask method

Specific details on test material used for the study:

Storage conditions: Room temperature tightly closed

Key result

Water solubility:

1.46 g/L

Conc. based on:

test mat. (dissolved fraction)

Loading of aqueous phase:

5.8 g/L

Incubation duration:

>= 39 - <= 41 d

Temp.:

20 °C

pH:

>= 6.4 - <= 6.6

Remarks on result:

other: S.D: ± 0.1 g/L

Remarks:

2nd test; result calculated based on a purity of 90 %

Water solubility:

1.63 g/L

Conc. based on:

test mat. (dissolved fraction)

Loading of aqueous phase:

5.8 g/L

Incubation duration:

>= 39 - <= 41 d

Temp.:

20 °C

pH:

>= 6.4 - <= 6.6

Remarks on result:

other: S.D: ± 0.12 g/L

Remarks:

2nd test; result calculated based on a purity of 100 %

Water solubility:

214 mg/L

Conc. based on:

element

Remarks:

Mn

Loading of aqueous phase:

5.8 g/L

Incubation duration:

>= 39 - <= 41 d

Temp.:

20 °C

pH:

>= 6.4 - <= 6.6

Remarks on result:

other: S.D: ± 15 mg/L

Remarks:

2nd test

Details on results:

Temperature and oxygen
- The mean temperature of the 1st test was 19.9 ± 0.7 °C and 20.1 ± 0.4 °C in the 2nd test.
- No oxygen was measurable

pH values
- samples: 1st test: 5.40 (37d) - 7.00 (1d), 2nd test: 6.5 (41d) - 6.7 (10d),
- blanks: 1st test: 6.45 (37d) - 7.54 (1d), 2nd test: 4.2 (10d) - 5.8 (41d)

Turbidity
- The turbidity in samples from test was always <1 NTU indicating that filtered solutions did not contain any undissolved material.

ICP-OES measurement for the element manganese with corresponding LOD/LOQ, correlation coefficient and sum of quality assurance samples and recovery

Calibration [µg/L] – lowest and highest calibration point	Chosen wavelength [nm]	LOD [µg/L]	LOQ [µg/L]	Correlation coefficient	Sum of quality assurance samples	Recovery of quality assurance samples [%]
(1^sttest) January 24, 2018; measurement of method blanks (days 1, 2, 3)
1 – 1000 (total of 13 calibration points, 13 used + blank)	257.610	0.088	0.265	0.999969	20	100
(1^sttest) January 29, 2018; measurement of samples (days 2, 3)
1 – 1000 (total of 13 calibration points, 13 used + blank)	257.610	0.024	0.073	0.999975	22	90.9
(1^sttest) February 01, 2018; measurement of samples (1d, 13d, 14) and method blanks (13 d, 14 d)
1 – 1000 (total of 13 calibration points, 13 used + blank)	257.610	0.192	0.575	0.999897	17	100
(1^sttest) February 15, 2018; measurement of samples and method blanks (days 28, 29)
1 – 1000 (total of 13 calibration points, 13 used + blank)	257.610	0.085	0.255	0.999973	13	100
(1^sttest) February 23, 2018; measurement of samples and method blanks (days 36, 37)
1 – 1000 (total of 13 calibration points, 13 used + blank)	257.610	0.077	0.231	0.999964	13	100
(2^ndtest) July 31, 2018; measurement of samples and method blanks (day 11)
25 – 1000 (total of 13 calibration points, 8 used + blank)	257.610	0.038	0.113	0.999985	21	100
(2^ndtest) August 01, 2018; measurement of method blanks (day 12)
1 – 1000 (total of 13 calibration points,13 used + blank)	257.610	0.041	0.122	0.999956	20	100
(2^ndtest) August 02, 2018; measurement of samples (days 12, 13) and method blanks (day 13)
1 – 1000 (total of 13 calibration points,13 used + blank)	257.610	0.046	0.137	0.999945	22	100
(2^ndtest) August 14, 2018; measurement of samples and method blanks (day 25)
1 – 1000 (total of 13 calibration points,13 used + blank)	260.568	0.041	0.124	0.999951	13	100
(2^ndtest) August 15, 2018; measurement of samples and method blanks (day 28)
1 – 1000 (total of 13 calibration points,13 used + blank)	260.568	0.073	0.218	0.999962	13	100
(2^ndtest) August 16, 2018; measurement of samples and method blanks (day 27)
1 – 1000 (total of 13 calibration points,13 used + blank)	260.568	0.148	0.444	0.999987	13	100
(2^ndtest) August 28, 2018; measurement of samples and method blanks (day 39)
1 – 1000 (total of 13 calibration points,13 used + blank)	257.610	0.028	0.085	0.999954	13	100
(2^ndtest) August 29, 2018; measurement of samples and method blanks (day 40)
2.5 – 1000 (total of 12 calibration points,13 used + blank)	259.372	0.052	0.155	0.999938	9	100
(2^ndtest) August 30, 2018; measurement of samples and method blanks (day 41)
1 – 1000 (total of 13 calibration points,13 used + blank)	259.372	0.060	0.180	0.999961	9	100

 

Recovery/validation data manganese

Element Mn	Recovery [%]	SD [%]	n (total)	n (valid)
January 24, 2018 (1^sttest)
TMDA-70.2 nominal value Mn: 312 µg/L	108	<1	4	4
Quality control standard (Roth) 7.5 µg/L	105	2	4	4
Quality control standard (Roth) 75 µg/L	104	2	4	4
Quality control standard (Roth) 750 µg/L	102	<1	4	4
Recalibration standard 100 µg/L	99.5	1.5	4	4
January 29, 2018 (1^sttest)
TMDA-70.2 nominal value Mn: 312 µg/L	107	1	4	4
Quality control standard (Roth) 7.5 µg/L	108	1	5	4
Quality control standard (Roth) 75 µg/L	104	1	5	4
Quality control standard (Roth) 750 µg/L	101	1	4	4
Recalibration standard 100 µg/L	102	1	4	4
February 01, 2018 (1^sttest)
TMDA-70.2 (dilution factor 2), nominal value Mn: 312 µg/L – diluted 156 µg/L	104	1	4	4
Quality control standard (Roth) 75 µg/L	105	2	4	4
Quality control standard (Roth) 750 µg/L	102	2	4	4
Recalibration standard 400 µg/L	105	2	4	4
February 15, 2018 (1^sttest)
TMDA-70.2 (dilution factor 2), nominal value Mn: 312 µg/L – diluted 156 µg/L	102	1	3	3
Quality control standard (Roth) 75 µg/L	102	<1	3	3
Quality control standard (Roth) 750 µg/L	99.8	0.7	3	3
Recalibration standard 500 µg/L	98.4	0.5	3	3
February 23, 2018 (1^sttest)
TMDA-70.2 (dilution factor 2), nominal value Mn: 312 µg/L – diluted 156 µg/L	105	2	3	3
Quality control standard (Roth) 75 µg/L	105	1	3	3
Quality control standard (Roth) 750 µg/L	101	<1	3	3
Recalibration standard 400 µg/L	103	1	3	3
July 31, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	101	2	5	5
Quality control standard (Roth) 100 µg/L	103	1	5	5
Quality control standard (Roth) 750 µg/L	98.2	0.2	5	5
Recalibration standard 500 µg/L	97.3	0.9	5	5
August 01, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	105	1	5	5
Quality control standard (Roth) 100 µg/L	103	1	5	5
Quality control standard (Roth) 750 µg/L	99.0	0.6	5	5
Recalibration standard 500 µg/L	98.5	1.1	5	5
August 02, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	102	1	5	5
Quality control standard (Roth) 100 µg/L	102	1	5	5
Quality control standard (Roth) 750 µg/L	99.2	2.2	5	5
Recalibration standard 500 µg/L	98.4	1.5	5	5
August 14, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	100	<1	3	3
Quality control standard (Roth) 100 µg/L	102	1	3	3
Quality control standard (Roth) 750 µg/L	99.3	0.5	3	3
Recalibration standard 500 µg/L	99.2	0.8	3	3
August 15, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	97.1	0.9	3	3
Quality control standard (Roth) 100 µg/L	102	<1	3	3
Quality control standard (Roth) 750 µg/L	98.9	0.9	3	3
Recalibration standard 500 µg/L	98.1	1.0	3	3
August 16, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	99.1	0.2	3	3
Quality control standard (Roth) 100 µg/L	103	1	3	3
Quality control standard (Roth) 750 µg/L	99.3	0.4	3	3
Recalibration standard 500 µg/L	99.0	1.0	3	3
August 28, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	100	2	3	3
Quality control standard (Roth) 100 µg/L	101	1	3	3
Quality control standard (Roth) 750 µg/L	98.5	0.5	3	3
Recalibration standard 500 µg/L	97.9	1.2	3	3
August 29, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	101	<1	2	2
Quality control standard (Roth) 100 µg/L	106	<1	2	2
Quality control standard (Roth) 750 µg/L	99.5	0.1	2	2
Recalibration standard 500 µg/L	97.8	0.1	2	2
August 30, 2018 (2^ndtest)
TMDA-70.2 1:2; nominal value Mn: 312 µg/L	101	<1	2	2
Quality control standard (Roth) 100 µg/L	103	<1	2	2
Quality control standard (Roth) 750 µg/L	99.5	0.3	2	2
Recalibration standard 500 µg/L	97.6	0.4	2	2

Manganese fortification

Sample	Element	Measured concentration [µg/L]	Calculated level after addition [µg/L]	Recovery [µg/L] / [%]
Fortification of measurement February 01, 2018 (1^sttest)
Vessel 1 sample a 14d (dilution factor 50) – 1 mL sample + 4 mL 100 µg/L standard	Mn	430	166	174 / 105
Fortification of measurement February 15, 2018 (1^sttest)
Vessel 2 sample a 28d (dilution factor 50) – 1 mL sample + 4 mL 100 µg/L standard	Mn	770	234	236 / 101
Fortification of measurement February 23, 2018 (1^sttest)
Vessel 2 sample a 36d (dilution factor 50) – 1 mL sample + 4 mL 100 µg/L standard	Mn	846	249	253 / 102
Fortification of measurement July 31, 2018 (2^ndtest)
Vessel 1 sample a 11d (dilution factor 5000) – 1 mL sample + 4 mL 500 µg/L standard	Mn	913	583	578 / 99.1
Fortification of measurement August 02, 2018 (2^ndtest)
Vessel 1 sample a 12d (dilution factor 200) – 1 mL sample + 4 mL 750 µg/L standard	Mn	485	697	697 / 100
Vessel 1 sample a 13d (dilution factor 10000) – 1 mL sample + 4 mL 250 µg/L standard	Mn	536	307	313 / 102
Fortification of measurement August 14, 2018 (2^ndtest)
Vessel 1 sample a 25d (dilution factor 200) – 1 mL sample + 4 mL 100 µg/L standard	Mn	791	238	237 / 99.6
Fortification of measurement August 15, 2018 (2^ndtest)
Vessel 1 sample a 26d (dilution factor 200) – 1 mL sample + 4 mL 750 µg/L standard	Mn	831	766	772 / 101
Fortification of measurement August 16, 2018 (2^ndtest)
Vessel 1 sample a 27d (dilution factor 500) – 1 mL sample + 4 mL 500 µg/L standard	Mn	414	483	489 / 101
Fortification of measurement August 28, 2018 (2^ndtest)
Vessel 1 sample a 39d (dilution factor 500) – 1 mL sample + 4 mL 250 µg/L standard	Mn	461	292	296 / 101
Fortification of measurement August 29, 2018 (2^ndtest)
Vessel 1 sample a 40d (dilution factor 500) – 1 mL sample + 4 mL 250 µg/L standard	Mn	460	292	300 / 103
Fortification of measurement August 30, 2018 (2^ndtest)
Vessel 1 sample a 41d (dilution factor 500) – 1 mL sample + 4 mL 750 µg/L standard	Mn	440	688	687 / 99.9

1st Test:

The pH value of solutions containing the test item started at 6.7 – 7.0 at day 1 and decreased over the sampling time to 5.4 – 5.5 (day 37). In contrast to the test vessels the pH value in method blanks was higher and in the range of 7.3 – 7.5 at day 1 and decreased over the sampling time to 6.5 – 6.6 (day 37). An influence of the test item on the pH cannot be excluded.

The determination of the water solubility of manganese neodecanoate is based on mean dissolved Mn concentrations of sampling days (36, 37 d) and a manganese content of 13.2 %.

The amount of dissolved manganese neodecanoate in the 1st test was calculated with a test item purity of 90 % according to test substance data sheet and 100 % as follows:

Mean Mn concentrations:       Vessel 1: 33.1 ± 0.4 mg/L, Vessel 2: 42.3 ± 0.5 mg/L, Mean: 37.7 ± 4.9 mg/L

Based on a test item purity of 90 % the water solubility of Manganese neodecanoate is:

Mean of concentration x 90 % / 13.2 %:       Vessel 1: 226 ± 3 mg/L, Vessel 2: 288 ± 3 mg/L, Mean: 257 ± 34 mg/L

Based on a test item purity of 100 % the water solubility of Manganese neodecanoate is:

Mean of concentration x 100 % / 13.2 %:       Vessel 1: 251 ± 3 mg/L, Vessel 2: 321 ± 4 mg/L, Mean: 286 ± 37 mg/L

However, the mean manganese concentration was analysed to 37.7 ± 4.9 mg/L Mn that is calculated to a water solubility for manganese neodecanoate of 286 ± 37 mg/L (sampling day 36 and 37; purity of 100 %) at 20 ± 1 °C. Based on the preliminary test a loading for the main test of 300 mg/L test item was chosen. Considering the loading (300 mg/L) and the test result (286 mg/L ± 37 mg/L) it became obvious that the loading chosen for the main test was too low.

Furthermore, no undissolved material was observed in test item loaded vessels. Hence, it was decided to repeat the study using a loading of 4 g/L.

2nd Test:

For the second test, 3.2 g of the test item had to be weighed into 800 mL (~ 4 g/L) of argon purged water (5.487 g and 3.987 g in vessel 1 and 2, respectively). The loadings differed (~ 25 %) since handling and weighing of the material using a polyethylene spatula were much complicated.

The pH value of method blank started at 4.2 – 5.2 at day 10 and increased over the sampling time to 4.3 – 5.8 (day 41). The low pH might be due to slight acidic residues after intensive cleaning. In contrast to the method blanks the pH values in test vessels were higher and in the range of 6.2 – 6.7 at day 10 and 6.5 – 6.6 at test end.

The calculated variations / changes between the sampling points were less than 15 % for the days 39, 40 and 41 and an increasing trend in concentrations cannot be observed. Thus, the validity criteria as foreseen in OECD 105 and Regulation 440/2008/EC A.6 were fulfilled.

Different to the 1st test, a residue was observed at the bottom of the test vessels. Moreover, the loading was much higher than the water solubility of manganese neodecanoate determined experimentally in the 2nd test. Hence, the 2nd test result is considered to be fully valid.

The determination of the water solubility of manganese neodecanoate is based on mean dissolved Mn concentrations of sampling days (39, 40, 41) and a manganese amount of 13.2 % in the test item.

The amount of dissolved manganese neodecanoate in the 2nd test was calculated with a test item purity of 90 % according to test substance data sheet and 100 % as follows:

Mean Mn concentrations:              Vessel 1: 228 ± 4 mg/L, Vessel 2: 201 ± 6 mg/L, Mean: 214 ± 15 mg/L

Based on a test item purity of 90 % the water solubility of Manganese neodecanoate is:

Mean of concentration x 90 % / 13.2 %:       Vessel 1: 1552 ± 27 mg/L, Vessel 2: 1372 ± 42 mg/L, Mean: 1462 ± 100 mg/L

Based on a test item purity of 100 % the water solubility of Manganese neodecanoate is:

Mean of concentration x 100 % / 13.2 %:       Vessel 1: 1725 ± 30 mg/L, Vessel 2: 1525 ± 47 mg/L, Mean: 1625 ± 111 mg/L

Conclusions:

1st test
Under the conditions of this test (under exclusion of CO2 and O2, under inert gas; flask method; loadings of 300 mg/L in vessel 1 and 2) complete dissolution of the test substance weighed into the test vessel was observed. The mean measured amount of dissolved manganese at 20 ± 1 °C is 37.7 ± 4.9 mg/L (determined as dissolved manganese, separated by filtration from undissolved test item). This corresponds to a water solubility of manganese neodecanoate of 286 ± 37 mg/L, calculated on a manganese content of 13.2 % and a test substance purity of 100 % (w/w).
These results indicate complete dissolution of the test item in the first test. Therefore, a second test with a higher loading (~4 g/L) has been conducted.

2nd test
Under the conditions of this test (under exclusion of CO2 and O2, under inert gas; flask method; loadings of 6.859 g/L and 4.742 g/L test substance in vessel 1 and 2), a solubility equilibrium was observed during testing. The mean measured amount of dissolved manganese at 20 ± 1 °C is 214 ± 15 mg/L (determined as dissolved manganese on day 39, 40, 41, separated by filtration from undissolved test item). This corresponds to a water solubility of manganese neodecanoate of 1.46 ± 0.1 g/L, calculated on a manganese content of 13.2 % and a test substance purity of 90 % (w/w).
Based on a test substance purity of 100 % (w/w), the water solubility of manganese neodecanoate is calculated to 1.63 ± 0.11 g/L.

Description of key information

Under the conditions of this test (under exclusion of CO2 and O2, under inert gas; flask method; loadings of 6.859 g/L and 4.742 g/L test substance in vessel 1 and 2), a solubility equilibrium was observed during testing. The mean measured amount of dissolved manganese at 20 ± 1 °C is 214 ± 15 mg/L (determined as dissolved manganese on day 39, 40, 41, separated by filtration from undissolved test item). This corresponds to a water solubility of manganese neodecanoate of 1.46 ± 0.1 g/L, calculated on a manganese content of 13.2 % and a test substance purity of 90 % (w/w).

Based on a test substance purity of 100 % (w/w), the water solubility of manganese neodecanoate is calculated to 1.63 ± 0.11 g/L.

Key value for chemical safety assessment

Water solubility:

1.46 g/L

at the temperature of:

20 °C