Fatty acids, tall-oil, manganese salts

Water solubility

Link to relevant study record(s)

Reference

Endpoint:

water solubility

Type of information:

experimental study

Adequacy of study:

key study

Study period:

2018-02-13 to 2019-04-16

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:

Three vessels were set up in a parallel design, each vessel was sampled several times instead of sampling one vessel at every point in time/ exclusion of O2 and CO2, under inert gas (argon)

Qualifier:

according to guideline

Guideline:

EU Method A.6 (Water Solubility)

Version / remarks:

2008

Deviations:

yes

Remarks:

Three vessels were set up in a parallel design, each vessel was sampled several times instead of sampling one vessel at every point in time/ exclusion of O2 and CO2, under inert gas (argon)

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:

Appearance: highly viscous, sticky, brown
Storage conditions: Keep in a dry and well-ventilated place in tightly sealed original container. Do not store in heat or direct sunlight.

Water solubility:

22.5 mg/L

Conc. based on:

element

Remarks:

Mn

Loading of aqueous phase:

800 mg/L

Incubation duration:

39 d

Temp.:

20.1 °C

pH:

>= 6.3 - <= 7.1

Remarks on result:

other: S.D.: ± 7.3 mg Mn/L

Key result

Water solubility:

265 mg/L

Conc. based on:

test mat. (dissolved fraction)

Loading of aqueous phase:

800 mg/L

Incubation duration:

39 d

Temp.:

20.1 °C

pH:

>= 6.3 - <= 7.1

Remarks on result:

other: S.D.: ± 86 mg/L

Remarks:

calculated based on a Mn content of 8.5%

Details on results:

Temperature:
The mean temperatures were 20.1 ± 0.2 °C (data logger 2) and 19.8 ± 0.1 °C (data logger 7). The maximum and minimum temperature was 19.7 °C and 22.0 °C, respectively. An increasing temperature for a short time (i.e., one hour) is considered to be not critical and had no influence on the result of the water solubility of the test substance. Moreover, the mean temperature was within the limits.

pH values
The pH of test item solutions was in the range of 6.3 – 7.1, whereas the pH of method blanks was in the range of 5.9 - 7.3.

Turbidity
The turbidity in samples from test was always < 1 NTU indicating that filtered test item solutions did not contain any undissolved material after filtering.
Turbidity measurements were not performed on days 37, 38 and 39 due to insufficient test solution.
This is not critical and does not influence the result of the determination of the water solubility for the test item.

Analytical measurements
Manganese concentrations in method blanks were analysed / calculated if at least one sample per sampling day was >LOQ. Hence, the background concentrations (< 1 µg/L) are far below concentrations in actual samples (at least > 5 mg/L) a background correction was not necessary.
The increase of concentrations from day 15 to end of testing (day 39) was less than 15 %. Thus, the validity criteria as foreseen in OECD 105 and Regulation 440/2008/EC A.6 were fulfilled.
However, an easy rise of the manganese concentration was observed till end of testing. Nevertheless, after 15 sampling points (39 days) the residual volume in test vessels did not allow any further samplings.

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

Calibration [µg/L] – lowest and highest calibration point	Chosen wavelength	LOD [µg Mn/L]	LOQ [µg Mn /L]	Correlation coefficient	Sum of quality assurance samples	Recovery of quality assurance samples [%]
February 19, 2018; measurement of samples from 1^stpreliminary test under non GLP conditions
1.0 – 1000 (total of 13 calibration points, 13 used + blank)	259.372	0.035	0.106	0.999947	20	100
February 25, 2019; measurement of samples from 2^ndpreliminary test
1.0 – 1000 (total of 13 calibration points, 13 used + blank)	260.568	0.166	0.498	0.999982	8	100

ICP-OES Recovery/validation data manganese of measurement series

Element Mn	Recovery [%]	SD [%]	n (total)	n (valid)
February 19, 2018 (1st preliminary test under non GLP conditions)
Roth 75 µg/L	105	1	4	4
TMDA-70.2 nominal value 312 µg/L Diluted 10-fold nominal value 31.2 µg/L	102	2	4	4
Recalibration standard 250 µg/L	101	1	4	4
TMDA-70.2 nominal value 312 µg/L	109	1	4	4
Roth 750 µg/L	102	1	4	4
February 25, 2019 (2^ndpreliminary test)
Recalibration standard 25 µg/L	100	<1	2	2
Roth 50 µg/L	99.2	0.5	2	2
Recalibration standard 250 µg/L	98.7	0.1	2	2
Roth 500 µg/L	95.4	0.7	2	2

ICP-MS measurement series (March 08, 2019) with corresponding LOD/LOQ, correlation coefficient and sum of quality assurance samples and recovery

Calibration [µg/L] – lowest and highest calibration point	Chosen isotope	LOD [µg Mn/L]	LOQ [µg Mn/L]	Correlation coefficient	Sum of quality assurance samples	Recovery of quality assurance samples [%]
March 08, 2019; measurement of test samples and method blanks (days 1, 2, 3)
0.1 – 250 (total of 14 calibration points, 14 used + blank)	^55Mn in high helium mode	0.003	0.009	0.9999	33	100
March 22, 2019; measurement of test samples and method blanks (days 15, 16, 17)
0.25 – 500 (total of 14 calibration points, 14 used + blank)	^55Mn in no gas mode	0.003	0.008	1.000	33	100
March 29, 2019; measurement of test samples and method blanks (days 23, 24, 25)
1.0 – 500 (total of 11 calibration points, 11 used + blank)	^55Mn in high helium mode	0.005	0.015	0.9998	19	100
April 08, 2019; measurement of test samples and method blanks (days 30, 31, 32)
1.0 – 500 (total of 11 calibration points, 11 used + blank)	^55Mn in helium mode	0.005	0.016	1.000	19	100
April 16, 2019; measurement of test samples and method blanks (days 37, 38, 39)
1.0 – 500 (total of 11 calibration points, 11 used + blank)	^55Mn in helium mode	0.005	0.015	1.000	19	100

ICP-MS Recovery/validation data manganese of measurement series

Element Mn	Recovery [%]	SD [%]	n (total)	n (valid)
March 08, 2019
LabKings 0.75 µg/L	99.4	2.0	6	6
LabKings 7.5 µg/L	97.2	1.5	6	6
LabKings 75 µg/L	99.2	2.0	6	6
Recalibration standard 10 µg/L	104	2	6	6
Recalibration standard 100 µg/L	103	2	6	6
March 22, 2019
LabKings 2.5 µg/L	105	2	6	6
LabKings 25 µg/L	110	3	6	6
LabKings 250 µg/L	108	3	6	6
Recalibration standard 10 µg/L	109	3	6	6
Recalibration standard 100 µg/L	108	4	6	6
March 29, 2019
LabKings 25 µg/L	102	1	4	4
Recalibration standard 75 µg/L	100	1	4	4
TMDA-70.2 nominal value 312 µg/L - diluted 2-fold nominal value 156 µg/L	106	1	4	4
LabKings 250 µg/L	103	<1	4	4
April 08, 2019
LabKings 25 µg/L	104	2	4	4
Recalibration standard 75 µg/L	101	1	4	4
TMDA-70.2 nominal value 312 µg/L - diluted 2-fold nominal value 156 µg/L	105	1	4	4
LabKings 250 µg/L	103	2	4	4
April 16, 2019
LabKings 25 µg/L	106	1	4	4
Recalibration standard 75 µg/L	101	1	4	4
TMDA-70.2 nominal value 312 µg/L - diluted 2-fold nominal value 156 µg/L	107	1	4	4
LabKings 250 µg/L	108	2	4	4

ICP-MS Fortification of measurement series

Sample	Element	Measured concen-tration [µg/L]	Calculated level after addition [µg/L]	Recovery [µg/L] / [%]
March 08, 2019
Vessel 3 sample a 1d (dilution 100-fold) – 1 mL sample, 4 mL 250 µg/L standard	Mn	158	232	247 / 107
Vessel 5 sample a 2d (dilution 100-fold) – 1 mL sample, 4 mL 100 µg/L standard	Mn	132	106	106 / 99.4
Vessel 3 sample a 3d (dilution 100-fold) – 1 mL sample, 4 mL 75 µg/L standard	Mn	174	94.9	92.4 / 97.4
March 22, 2019
Vessel 3 sample a 15d (dilution 100-fold) – 1 mL sample, 4 mL 500 µg/L standard	Mn	198	440	439 / 99.9
Vessel 5 sample a 16d (dilution 100-fold) – 1 mL sample, 4 mL 500 µg/L standard	Mn	182	436	444 / 102
Vessel 4 sample a 17d (dilution 100-fold) – 1 mL sample, 4 mL 250 µg/L standard	Mn	85.4	217	225 / 103
March 29, 2019
Vessel 3 sample a 23d (dilution 100-fold) – 1 mL sample, 4 mL 500 µg/L standard	Mn	222	444	430 / 96.8
Vessel 4 sample a 24d (dilution 100-fold) – 1 mL sample, 4 mL 250 µg/L standard	Mn	89.6	218	218 / 99.9
Vessel 5 sample a 25d (dilution 100-fold) – 1 mL sample, 4 mL 100 μg/L standard	Mn	196	119	120 / 101
April 08, 2019
Vessel 3 sample a 23d (dilution 100-fold) – 1 mL sample, 4 mL 500 µg/L standard	Mn	235	447	465 / 104
Vessel 4 sample a 24d (dilution 100-fold) – 1 mL sample, 4 mL 250 µg/L standard	Mn	104	221	220 / 99.6
Vessel 5 sample a 25d (dilution 100-fold) – 1 mL sample, 4 mL 100 µg/L standard	Mn	235	127	129 / 102
April 16, 2019
Vessel 3 sample a 37d (dilution 100-fold) – 1 mL sample, 4 mL 500 µg/L standard	Mn	288	458	463 / 101
Vessel 4 sample a 38d (dilution 100-fold) – 1 mL sample, 4 mL 250 µg/L standard	Mn	126	225	224 / 99.4
Vessel 5 sample a 39d (dilution 100-fold) – 1 mL sample, 4 mL 100 µg/L standard	Mn	254	131	131 / 99.8

 

The water solubility of the test item is 265 mg/L ± 86 mg/L at day 39 based on a measured manganese concentration of 22.5 ± 7.3 mg Mn/L

Mean Mn concentrations
Vessel 3:                     28.9 ± 0.2 mg/L Mn
Vessel 4:                     13.3 ± < 0.1 mg/L Mn
Vessel 5:                      25.3 ± 0.2 mg/L Mn
Mean:                           22.5 ± 6.7 mg/L Mn

The mean Mn concentrations in replicate vessel 4 differ.

Based on a test item purity of 100 % and a mean manganese content of 8.5 % the water solubility ofthe test item is:

Mean of concentration x 100 % / 8.5 %

Vessel 3:                     340 ± 3 mg/L test item
Vessel 4:                     156 ± < 1 mg/L test item
Vessel 5:                      297 ± 2 mg/L test item
Mean:                           265 ± 86 mg/L test item

Conclusions:

Under the conditions of this test (under exclusion of CO2 and O2, under inert gas; flask method; loadings of ~800 mg/L test item in three replicates), a solubility equilibrium was not reached after day 39 of testing. The mean measured dissolved manganese concentration on day 39 at 20.1 ± 0.2 °C is 22.5 ± 7.3 mg/L.
This corresponds to a water solubility of dissolved Fatty acids, tall-oil, manganese salts of 265 ± 86 mg/L, calculated on a mean manganese content of 8.5 %.

Description of key information

Fatty acids, tall-oil, manganese salts has a water solubility of 265 ± 86 mg/L, calculated on a mean manganese content of 8.5 %.

Key value for chemical safety assessment

Water solubility:

265 mg/L

at the temperature of:

20 °C

Additional information

Under the conditions of this test (under exclusion of CO₂ and O₂, under inert gas; flask method; loadings of ~800 mg/L test item in three replicates), a solubility equilibrium was not reached after day 39 of testing. The mean measured dissolved manganese concentration on day 39 at 20.1 ± 0.2 °C is 22.5 ± 7.3 mg/L.

This corresponds to a water solubility of dissolved Fatty acids, tall-oil, manganese salts of 265 ± 86 mg/L, calculated on a mean manganese content of 8.5 %.

The dissolution of manganese from Fatty acids, tall-oil manganese salts after 2h in simulated gastric acid (pH 1.5) at 0.2 and 2 g/L loading is 2.2 and 1.2%, respectively, corresponding to 0.401 and 2.14 mg Mn/L.

The dissolution of Mn in simulated interstitial fluid (pH 7.4) at a loading of 2 g/L Fatty acids, tall-oil manganese salts is 0.16 and 1.5% after 24h and 168h, respectively, corresponding to 0.291 and 2.74 mg Mn/L.