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Endpoint:
adsorption / desorption, other
Remarks:
Batch Equilibrium Method
Type of information:
experimental study
Adequacy of study:
key study
Study period:
2018-02-21 to 2018-10-05
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Justification for type of information:
requested from ECHA final decision on substance evaluation
Qualifier:
according to
Guideline:
OECD Guideline 106 (Adsorption - Desorption Using a Batch Equilibrium Method)
Version / remarks:
2000
Deviations:
yes
Remarks:
method validation for tier 3: The test item concentrations in the soils were determined in all concentration levels followed by calculating the mass balance.
Qualifier:
according to
Guideline:
EU Method C.18 (Adsorption / Desorption Using a Batch Equilibrium Method)
Version / remarks:
2008
Deviations:
no
GLP compliance:
yes (incl. certificate)
Type of method:
batch equilibrium method
Media:
soil
Specific details on test material used for the study:
Name: HH-2014-548
Batch number: AE 188/17
Expiry date: 2019-06-29
purity: 100% (UVCB)
Radiolabelling:
no
Remarks:
it was not possible to obtain a stable radiolabelled substance with needed purity (details see at the attached document)
Test temperature:
20 +- 2 °C (test temperature reached a max. of 22.8 °C during tier 1 and 2)
Analytical monitoring:
yes
Remarks:
in aqueous phase by LC-MS
Details on sampling:
The soil suspensions will be centrifuged after agitation to separate the phases, followed by analysing the concentration of the analytes in aqueous phase by LC-MS. Centrifugation conditions are determined depending on soil / solution ratio and soil type and will be documented in the raw data and given in the report. If necessary, test vessel adsorption will be determined by LC-MS after extraction of the test vessels with an appropriate solvent. For analysis of the soil, the aqueous phase will be decanted and the soil will be extracted. If the mass balance is ≥ 90 % during tier 1 the soil will not be extracted in tier 2 and tier 3 since an indirect method can be used. Details of sample preparation are documented in the raw data and given in the report.
- Concentrations:
2 mg test item /L (concentration used for adsorption kinetics)
1 mg test item /L
0.2 mg test item /L
0.1 mg test item /L
0.02 mg test item /L
- Sampling interval:
Tier 1: 24h
Tier 2: 0.25h, 0.5h, 1h for all soils
2h, 4h, 6h, 24h for soils LUFA 2.2 and 2.4
Desorption kinetics: 2h, 4h, 24h and 72h
Adsorption isotherms: 1h
- Sample storage before analysis: 25 mL acetonitrile containing 2 % formic acid were added to the wet soil. The vessel was shaken for 60 min. The suspensions were centrifuged at 4000 rpm for 5 min. The extraction was repeated twice with 25 mL acetonitrile containing 2 % formic acid (3rd extraction step with shaking overnight). The extracts were transferred quantitatively into a 100 ml. measuring flask and filled
up with acetonitrile containing 2 % formic acid. Blank extract was used for dilutions to calibration range, if necessary. During tier 1 the wet soil was transferred to a new centrifugation tube prior to extraction using 15mL 0.01 M CaCl2-solution. The suspensions were centrifuged at 4000 rpm for 5 min. For the extraction of the test vessel 20 mL acetonitrile/0.01 M CaCl2-solution (50/50 containing 1 % formic acid) was added and the test vessel was shaken for 1 hour.
Matrix no.:
#1
Matrix type:
other: silty sand
% Clay:
3.1
% Silt:
12.2
% Sand:
84.7
% Org. carbon:
0.71
pH:
4.9
CEC:
4.3 meq/100 g soil d.w.
Matrix no.:
#2
Matrix type:
loamy sand
% Clay:
8.6
% Silt:
16.6
% Sand:
74.8
% Org. carbon:
1.61
pH:
5.4
CEC:
9.7 meq/100 g soil d.w.
Matrix no.:
#3
Matrix type:
other: silty sand
% Clay:
6.9
% Silt:
35.6
% Sand:
57.5
% Org. carbon:
0.67
pH:
5.9
CEC:
7.6 meq/100 g soil d.w.
Matrix no.:
#4
Matrix type:
clay loam
% Clay:
26.2
% Silt:
45.7
% Sand:
28.1
% Org. carbon:
1.99
pH:
7.4
CEC:
32.9 meq/100 g soil d.w.
Matrix no.:
#5
Matrix type:
loamy sand
% Clay:
10.8
% Silt:
34.7
% Sand:
54.5
% Org. carbon:
1.02
pH:
7.3
CEC:
17.7 meq/100 g soil d.w.
Details on matrix:
COLLECTION AND STORAGE
- Soil preparation (e.g.: 2 mm sieved; air dried etc.):Standard LUFA soils 2.1, 2.2, 2.3, 2.4 and 5M in contact to 0.01 M CaCl2-solution were used for this study. These matrices have varying adsorption capacities in relation to their content of organic matter, clay, pH and cation exchange capacity. All soils are air-dried and sieved to a maximum particle size of 2 mm by the distributor.
PROPERTIES
- Soil texture: Additionally, the actual content of organic matter, the content of clay, silt and sand and the cation exchange capacity were determined (externally, non-GLP).
- pH: pH values and Soil Dry Weights are given in Table 1 and 2 under 'Any other information on material and methods incl. tables'
Details on test conditions:
The soils will be weighed into the test vessels and an appropriate volume of 0.01 M CaCl2-solution will be added. After agitation overnight (12 h minimum), the samples will be used for adsorption experiments.
The soil samples will be conditioned as described above.
0.1 volume-% of the stock solutions, related to the volume of the aqueous phase in the soil suspensions will be added in order to adjust the test concentrations. Afterwards, the samples will be agitated.
Samples at adsorption equilibrium will be used for this purpose.
The test vessels will be centrifuged after completion of the adsorption experiments, weighed and the supernatant will be replaced by fresh 0.01 M CaCl2-solution. Then, the test vessels will be agitated again to investigate the desorption behavior of the test item.
The soil suspensions will be centrifuged after agitation to separate the phases, followed by analysing the concentration of the analytes in aqueous phase by LC-MS. Centrifugation conditions are determined depending on soil / solution ratio and soil type and will be documented in the raw data and given in the report. If necessary, test vessel adsorption will be determined by LC-MS after extraction of the test vessels with an appropriate solvent. For analysis of the soil, the aqueous phase will be decanted and the soil will be extracted. If the mass balance is ≥ 90 % during tier 1 the soil will not be extracted in tier 2 and tier 3 since an indirect method can be used. Details of sample preparation are documented in the raw data and given in the report.
All samples will be prepared in duplicate.
Sampling points will be fixed based on the results of tier 1 and described in a study plan amendment.
For the adsorption and desorption isotherms, the samples will be agitated according to the equilibration time determined during the adsorption and desorption kinetic experiments.
TEST CONDITIONS
- Buffer: 0.01 M CaCl2-solution
- pH: please refer to Table 1 ' any other information oin materials and methods incl. tables'
- Suspended solids concentration: please refer to Table 2 ' any other information oin materials and methods incl. tables'

TEST SYSTEM
- Type, size and further details on reaction vessel: 50 mL disposable centrifugation tubes
- Water filtered (i.e. yes/no; type of size of filter used, if any): no
- Soil/water ratio (if simulation test): Test volume: 40mL Tier 1: 1:40,1:10 and 1:5; Tier 2 and Tier 3: 1:10
- Number of reaction vessels/concentration: duplicates except Blank vessel for tier 2 testing (single)
- Measuring equipment: Equipment
Piston stroke pipettes, THERMO SClENTlFlC
Positive displacement pipettes, GILSON MEDlCAL
Centrifuge Megastar 3.0, VWR
Ultrasonic bath, BANDELIN
Multipette E3x, EPPENDORF
Top pan Balance, KERN
Analytical balance, SARTORlUS
pH-Meter, Lab 850, Si ANALYTlCS + HACH
Laboratory glassware
Data logger, TESTO
Shaker, EDMUND BUHLER
Syringe filter, Chromafil GF/RC-45/25, MACHEREY & NAGEL
Milli-Q system, Merck
PP 50 mL centrifugation tubes, VWR
Reagents
Calcium chloride ≥ 98 %, ROTH
Ultrapure water generated in house
Acetonitrile, HPLC-Plus ≥ 99.9 %, Merck
Formic Acid, ≥ 98 %, VWR
- Test performed in closed vessels due to significant volatility of test substance: no
- Test performed in open system: not reported
- Method of preparation of test solution:
Stock solutions
Stock solutions of 2, 1, 0.2, 0.1 and 0.02 g/L of the test item in acetonitrile were prepared.
Preparation of the soil samples (conditioning): The soils were weighed into the test vessels and an appropriate volume of 0.01 M CaCl2-solution was added.
After agitation overnight (12 h minimum), the samples were used for adsorption experiments.
Preparation of the samples for adsorption experiments
The soil samples were conditioned as described above. 0.1 volume-% (0.04 mL) of the stock solutions was added in order to adjust the test concentrations. Afterwards, the samples were agitated.
Preparation of the samples for desorption experiments
Samples at adsorption equilibrium were used for this purpose. After completion of the adsorption experiments the test vessels were centrifuged, weighed and the supernatant was replaced by fresh 0.01 M CaCl2-solution. Then the test vessels were agitated again to investigate the desorption behavior of the test item.
Computational methods:
- Adsorption and desorption coefficients (Kd): yes, as detailed in the study report
- Freundlich adsorption and desorption coefficients: yes, as detailed in the study report
- Adsorption coefficient per organic carbon (Koc): yes, as detailed in the study report
Key result
Sample No.:
#1
Type:
Koc
Remarks:
C40H73N3O
Value:
267 471 L/kg
pH:
5.9
Temp.:
22.8 °C
Matrix:
LUFA2.1
% Org. carbon:
0.718
Key result
Sample No.:
#2
Type:
Koc
Remarks:
C40H73N3O
Value:
136 414 L/kg
pH:
6.6
Temp.:
22.8 °C
Matrix:
LUFA2.2
% Org. carbon:
1.47
Key result
Sample No.:
#3
Type:
Koc
Remarks:
C40H73N3O
Value:
1 203 052 L/kg
pH:
6.8
Temp.:
22.8 °C
Matrix:
LUFA 2.3
% Org. carbon:
0.412
Key result
Sample No.:
#4
Type:
Koc
Remarks:
C40H73N3O
Value:
346 000 L/kg
pH:
7.4
Temp.:
22.8 °C
Matrix:
LUFA 2.4
% Org. carbon:
1.74
Key result
Sample No.:
#5
Type:
Koc
Remarks:
C40H73N3O
Value:
637 465 L/kg
pH:
7.5
Temp.:
22.8 °C
Matrix:
LUFA 5M
% Org. carbon:
0.916
Key result
Sample No.:
#1
Type:
Koc
Remarks:
C41H76N3O
Value:
278 741 L/kg
pH:
5.9
Temp.:
22.8 °C
Matrix:
LUFA 2.1
% Org. carbon:
0.718
Key result
Sample No.:
#2
Type:
Koc
Remarks:
C41H76N3O
Value:
140 238 L/kg
pH:
6.6
Temp.:
22.8 °C
Matrix:
LUFA 2.2
% Org. carbon:
1.47
Key result
Sample No.:
#3
Type:
Koc
Remarks:
C41H76N3O
Value:
1 183 242 L/kg
pH:
6.8
Temp.:
22.8 °C
Matrix:
LUFA 2.3
% Org. carbon:
0.412
Key result
Sample No.:
#4
Type:
Koc
Remarks:
C41H76N3O
Value:
320 551 L/kg
pH:
7.4
Temp.:
22.8 °C
Matrix:
LUFA 2.4
% Org. carbon:
1.74
Key result
Sample No.:
#5
Type:
Koc
Remarks:
C41H76N3O
Value:
573 756 L/kg
pH:
7.5
Temp.:
22.8 °C
Matrix:
LUFA 5M
% Org. carbon:
0.916
Key result
Sample No.:
#1
Type:
Kd
Remarks:
C40H73N3O
Value:
1 920 L/kg
pH:
5.9
Temp.:
22.8
Matrix:
LUFA 2.1
% Org. carbon:
0.718
Key result
Sample No.:
#2
Type:
Kd
Remarks:
C40H73N3O
Value:
2 005 L/kg
pH:
6.6
Temp.:
22.8 °C
Matrix:
LUFA 2.2
% Org. carbon:
1.47
Key result
Sample No.:
#3
Type:
Kd
Remarks:
C40H73N3O
Value:
4 957 L/kg
pH:
6.8
Temp.:
22.8 °C
Matrix:
LUFA 2.3
% Org. carbon:
0.412
Key result
Sample No.:
#4
Type:
Kd
Remarks:
C40H73N3O
Value:
6 020 L/kg
pH:
7.4
Temp.:
22.8 °C
Matrix:
LUFA 2.4
% Org. carbon:
1.74
Key result
Sample No.:
#5
Type:
Kd
Remarks:
C40H73N3O
Value:
5 839 L/kg
pH:
7.5
Temp.:
22.8 °C
Matrix:
LUFA 5M
% Org. carbon:
0.916
Key result
Sample No.:
#1
Type:
Kd
Remarks:
C41H76N3O
Value:
2 001 L/kg
pH:
5.9
Temp.:
22.8 °C
Matrix:
LUFA 2.1
% Org. carbon:
0.718
Key result
Sample No.:
#2
Type:
Kd
Remarks:
C41H76N3O
Value:
2 062 L/kg
pH:
6.6
Temp.:
22.8 °C
Matrix:
LUFA 2.2
% Org. carbon:
1.47
Key result
Sample No.:
#3
Type:
Kd
Remarks:
C41H76N3O
Value:
4 875 L/kg
pH:
6.8
Temp.:
22.8 °C
Matrix:
LUFA 2.3
% Org. carbon:
0.412
Key result
Sample No.:
#4
Type:
Kd
Remarks:
C41H76N3O
Value:
5 578 L/kg
pH:
7.4
Temp.:
22.8 °C
Matrix:
LUFA 2.4
% Org. carbon:
1.74
Key result
Sample No.:
#5
Type:
Kd
Remarks:
C41H76N3O
Value:
5 256 L/kg
pH:
7.5
Temp.:
22.8 °C
Matrix:
LUFA 5M
% Org. carbon:
0.916
Adsorption and desorption constants:
Tier 1 - Adsorption
LUFA 2.2 and LUFA 2.4 soils were used for preliminary investigations on the adsorption behavior of the test item with soil I solution ratios of 1:5, 1:10 and 1:40 at a concentration of 2 mg test item/L. An adsorption of 2 99% was determined for the two analytes in both soils after 24 h.
Tier 1 - Test Vessel Adsorption
The test item adsorption to the test vessels in test item controls and soil suspensions was determined in tier 1 for the samples with the longest agitation period in polypropylene centrifugation tubes. Significant adsorption on test vessels was observed only for the control
samples but not for the samples containing soil.
Tier 1 - Extraction from Soil I Mass Balance
Recovery rates from 83% to 96% of the nominal concentration for the analytes were obtained using acetonitrile containing 2 % formic acid at ambient temperature. Significant adsorption on test vessels was observed only for the soil / solution ratio of 1:40. A soil / solution of 1:10 was chosen for tier 2 and tier 3.
Matrix Effects
Matrix effects of the analytical method have been investigated during tier 1 for the soils LUFA 2.2 and LUFA 2.4 and during tier 2 for the remaining soils. No matrix effects were observed for the samples of the aqueous phase. In contrast, a matrix effect was observed for extracts of some soils. For this reason, extracts of each soil were analysed with a matrix calibration.
Tier 2 - Adsorption Kinetics
The determination for adsorption kinetics was performed with a nominal test item concentration of 2 mg test item/L. A soil / solution ratio of 1:10 was used and concentrations of the test item were measured in aqueous phase at defined sampling points. The equilibrium was reached within 1 hour.
Tier 3 - Desorption Kinetics
The desorption behavior of the test item was determined after 1 h adsorption. The results show that the test item adsorption is not
reversible since the maximum desorption determined is 0.7 %.
Recovery of test material:
Recovery rates from 83% to 96% of the nominal concentration for the analytes were obtained.
Concentration of test substance at end of adsorption equilibration period:
For C40H73N3O (µg/ 40mL):
LUFA 2.1 79.3
LUFA 2.2 79.3
LUFA 2.3 79.5
LUFA 2.4 79.5
LUFA 5M 79.5
For C41H76N3O (µg/ 40mL):
LUFA 2.1 79.3
LUFA 2.2 79.3
LUFA 2.3 79.5
LUFA 2.4 79.5
LUFA 5M 79.5
Concentration of test substance at end of desorption equilibration period:
For C40H73N3O (µg/ 40mL):
LUFA 2.1 0.522
LUFA 2.2 0.336
LUFA 2.3 0.205
LUFA 2.4 0.118
LUFA 5M 0.0382
For C41H76N3O (µg/ 40mL):
LUFA 2.1 0.548
LUFA 2.2 0.369
LUFA 2.3 0.249
LUFA 2.4 0.166
LUFA 5M 0.109
Sample no.:
#1
Duration:
24 h
% Adsorption:
96
Remarks on result:
other: LUFA 2.2/C40H73N3O
Sample no.:
#2
Duration:
24 h
% Adsorption:
85
Remarks on result:
other: LUFA 2.4/C40H73N3O
Sample no.:
#1
Duration:
24 h
% Adsorption:
93
Remarks on result:
other: LUFA 2.2/C41H76N3O
Sample no.:
#2
Duration:
24 h
% Adsorption:
83
Remarks on result:
other: LUFA 2.4/C41H76N3O
Transformation products:
not measured
Details on results (Batch equilibrium method):
PRELIMINARY TEST
- Volume of CaCl2 solution: 40 mL
- Initial test substance concentration: 2 mg/L
- Test substance concentration in final solution: 1 and 0%

MAIN TEST: PERFORMANCE
- Test material stability during adsorption/desorption phase: stable
- Experimental conditions maintained throughout the study: Yes
- Buffer/test substance interactions affecting sorption: No
- Buffer-catalyzed degradation of test substance: No

Table 3: Tier 1:Mass Balance LUFA 2.2 - C40H73N3O Compound, applied test item concentration: 2 mg/L, n=2

Soil / solution
ratio

Sampling point


[h]

Recovery rate from aqueous phase
[%]

Recovery rate from test vessel
[%]

Recovery rate from solid phase
[%]

Mass balance1)

[%]

1:40

24 I

1

4

-

-

24 II

1

5

-

1:10

24 I

1

0.4

103

96

24 II

1

0.4

88

1:5

24 I

0

0.3

87

89

24 II

0

0.2

89

Table 4: Tier 1:Mass Balance LUFA 2.2 - C41H76N3O Compound, applied test item concentration: 2 mg/L, n=2

Soil / solution
ratio

Sampling point


[h]

Recovery rate from aqueous phase
[%]

Recovery rate from test vessel
[%]

Recovery rate from solid phase
[%]

Mass balance1)

[%]

1:40

24 I

1

4

-

-

24 II

1

5

-

1:10

24 I

1

0.3

97

93

24 II

1

0.4

87

1:5

24 I

0

0.2

88

88

24 II

0

0.2

87

Table 5: Tier 1:Mass Balance LUFA 2.4 - C40H73N3O Compound, applied test item concentration: 2 mg/L, n=2

Soil / solution
ratio

Sampling point


[h]

Recovery rate from aqueous phase
[%]

Recovery rate from test vessel
[%]

Recovery rate from solid phase
[%]

Mass balance1)

[%]

1:40

24 I

1

3

-

-

24 II

1

3

-

1:10

24 I

0

0.2

81

85

24 II

0

0.3

87

1:5

24 I

0

0.1

84

85

24 II

0

0.1

85

Table 6: Tier 1:Mass Balance LUFA 2.4 – C41H76N3O Compound, applied test item concentration: 2 mg/L, n=2

Soil / solution
ratio

Sampling point


[h]

Recovery rate from aqueous phase
[%]

Recovery rate from test vessel
[%]

Recovery rate from solid phase
[%]

Mass balance1)

[%]

1:40

24 I

1

3

-

-

24 II

1

3

-

1:10

24 I

0

0.2

82

83

24 II

0

0.2

84

1:5

24 I

0

0.1

86

85

24 II

0

0.1

83

Table 7: Matrix effects – aqueous phase, applied test item concentration: 25 µg/L, n=2, Soil solution ratio 1:10

Soil

C40H73N3O

Compound

Recovery [%]

C41H76N3O

Compound

Recovery [%]

LUFA 2.1

101

99

LUFA 2.2

96

97

LUFA 2.3

103

101

LUFA 2.4

98

90

LUFA 5M

99

99

Table 8: Matrix effects – soil extract, applied test item concentration: 25 µg/L, n=2, Soil solution ratio 1:10

Soil

C40H73N3O

Compound

Recovery [%]

C41H76N3O

Compound

Recovery [%]

LUFA 2.1

90

77

LUFA 2.2

86

108

LUFA 2.3

85

76

LUFA 2.4

83

108

LUFA 5M

82

75

Table 9: Summarized Endpoints forHH-2014-548and the main components, Mobility according to McCall et al. (1980):KOC0 – 50 very high,KOC50 – 150 high,KOC150 – 500 medium,KOC500 – 2000 low,KOC2000 – 5000 slight,KOC> 5000 immobile

Soil

Soil / Solution Ratio

maq(eq)
[µg]

Kd
[mL/g]

KOC
[mL/g]

Kdes
[mL/g]

KFOC

[µg1-1/n
(mL)1/ng-1]

1/n

Mobility according to McCall et al. based on KOC

Protonated oleic acid IQAC

LUFA 2.1

1:10

0.426

1920

267471

1566

173511

0.95

immobile

LUFA 2.2

1:10

0.426

2005

136414

2538

72343

0.99

immobile

LUFA 2.3

1:10

0.167

4957

1203052

4042

643987

1.0

immobile

LUFA 2.4

1:10

0.146

6020

346000

7425

107761

0.98

immobile

LUFA 5M

1:10

0.147

5839

637465

22597

656566

1.1

immobile

Methyl quaternized oleic acid IQAC

LUFA 2.1

1:10

0.409

2001

278741

1491

184184

0.96

immobile

LUFA 2.2

1:10

0.414

2062

140238

2307

70993

1.0

immobile

LUFA 2.3

1:10

0.170

4875

1183242

3323

529846

0.99

immobile

LUFA 2.4

1:10

0.157

5578

320551

5284

95875

0.96

immobile

LUFA 5M

1:10

0.164

5256

573756

7927

580722

1.1

immobile

HH-2014-548

LUFA 2.1

1:10

0.412

1986

276659

1505

182212

0.96

immobile

LUFA 2.2

1:10

0.416

2051

139531

2350

71242

1.0

immobile

LUFA 2.3

1:10

0.169

4890

1186903

3456

550937

0.99

immobile

LUFA 2.4

1:10

0.155

5660

325254

5680

98071

0.96

immobile

LUFA 5M

1:10

0.161

5364

585528

10638

594737

1.1

immobile

maq(eq)          = mass in the aqueous phase at adsorption equilibrium

Table 10: Freundlich Adsorption Isotherms forC40H73N3O Compound Applied test item concentrations: 2, 1, 0.2, 0.1, 0.02 mg/L

Volume of aqueous phase:40 mL

Soil Type

msoil[g]

r2

1/n

KFads

KFOC

LUFA 2.1

3.88

0.995

0.95

1246

173511

LUFA 2.2

3.71

0.998

0.99

1063

72343

LUFA 2.3

3.84

0.999

1.0

2653

643987

LUFA 2.4

3.62

0.999

0.98

1875

107761

LUFA 5M

3.70

0.999

1.1

6014

656566

Table 11: Freundlich Adsorption Isotherms forC41H76N3O Compound, Applied test item concentrations: 2, 1, 0.2, 0.1, 0.02 mg/L

Volume of aqueous phase:40 mL

Soil Type

msoil[g]

r2

1/n

KFads

KFOC

LUFA 2.1

3.88

0.995

0.96

1322

184184

LUFA 2.2

3.71

0.998

1.0

1044

70993

LUFA 2.3

3.84

0.997

0.99

2183

529846

LUFA 2.4

3.62

1.000

0.96

1668

95875

LUFA 5M

3.70

0.998

1.1

5319

580722

Validity criteria fulfilled:
yes
Conclusions:
Based on the results detected in the present study conducted according to OECD guideline 106 (2000), the test item showed a low desorption (0.05 to 0.7 %) during desorption kinetic experiments, thus, the expected desorption was too low for a reliable determination because the experimental error in the applied analytical methods would have been higher. The test item HH-2014-548 adsorbs to all tested soils with Koc values above 135000 and is therefore immobile in soiis according to McCall et al. The adsorption was not reversible.
Executive summary:

In a study conducted according to OECD guideline 106 (2000) five standard soils were incubated with the test item at concentrations of

2 mg test item /L (concentration used for adsorption kinetics), 1, 0.2, 0.1 and 0.02 mg test item /L for the following durations:

Tier 1: 24h

Tier 2: 0.25h, 0.5h, 1h for all soils

2h, 4h, 6h, 24h for soils LUFA 2.2 and 2.4

Desorption kinetics: 2h, 4h, 24h and 72h

Adsorption isotherms: 1h

Based on the obtained results the adsorption of the test item is nearly 100% in all soils and desorption is very low, thus, the test item HH-2014-548 adsorbs to all tested soils with Koc values above 135000 and is therefore immobile in soiis according to McCall et al. The adsorption was not reversible.

Some numerical results are listed in the following table:

Soil Soil / Solution 
Ratio Kd 
[mL/g] Koc 
[mL/g] logKoc Mobility according 
to McCall et al. 
based on Koc
LUFA 2.1 1:10 1986 276659 5.44 immobile
LUFA 2.2 1:10 2051 139531 5.14 immobile
LUFA 2.3 1:10 4890 1186903 6.07 immobile
LUFA 2.4 1:10 5660 325254 5.51 immobile
LUFA 5M 1:10 5364 585528 5.77 immobile
    arithmetic mean Koc 502775 5.59 arithmetic mean logKoc
Endpoint:
adsorption / desorption: screening
Type of information:
experimental study
Adequacy of study:
key study
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Guideline study according to EC C.19 (OECD 121)
Qualifier:
according to
Guideline:
EU Method C.19 (Estimation of the Adsorption Coefficient (KOC) on Soil and Sewage Sludge Using High Performance Liquid Chromatography (HPLC))
Qualifier:
according to
Guideline:
OECD Guideline 121 (Estimation of the Adsorption Coefficient (Koc) on Soil and on Sewage Sludge using High Performance Liquid Chromatography (HPLC))
GLP compliance:
yes (incl. certificate)
Type of method:
HPLC estimation method
Media:
other:
Radiolabelling:
no
Test temperature:
Column temperature = 35 °C ± 1 °C
Details on study design: HPLC method:
EQUIPMENT
- Apparatus: Acquity UPLC system (Waters. Milford, MA. U.S.A.)
- Type, material and dimension of analytical (guard) column: Hypersil BDS-CN, 100 x 2.1 mm i.d., dp = 3 µm (Thermo Fisher Scientific. Waltham, MA. U.S.A.)
- Detection system: Acquity UPLC TUV detector (Waters). ZQ 2000 mass spectrometer (Waters)

MOBILE PHASES
- Type: A - 55/45 (v/v), B - methanol
- pH: not specified
- Experiments with additives carried out on separate columns: no
- Solutes for dissolving test and reference substances: A - 55/45 (v/v)

DETERMINATION OF DEAD TIME
- Method: by means of homologous series / by inert substances which are not retained by the column: not reported

REFERENCE SUBSTANCES
- Identity:2,4-DDT

DETERMINATION OF RETENTION TIMES
- Quantity of test substance introduced in the column: 10 µl
- Quantity of reference substances: 10 µl

REPETITIONS
- Number of determinations:1
Type:
Koc
Value:
> 427 000
Temp.:
35 °C
Type:
log Koc
Value:
> 5.63
Temp.:
35 °C
Details on results (HPLC method):
The reference substance 2,4-DDT was detected and had a retention time of 2.9 minutes. The results demonstrated the validity of the analytical method on the day of analysis.
A gradient to 100% methanol was applied in order to elute the test substance components. Neither in the full scan mode nor in the MRM mode at m/z 628.5 test substance related compounds were detected. To demonstrate that the test substance was applied, the test solution was analysed in the bypass mode (i.e. without the analytical column). The test substance was detected in the dead volume of the system. It demonstrated that the test substance most Iikely interacted strongly with the analytical column and no eluting of the components occurred. Based on the results obtained it was concluded that the test substance has a Kc value of higher than the reference substance 2,4-DDT. It corresponds with Koc and log Koc value for the test
substance of > 427000 and > 5,63, respectively.

No test substance related compounds were detected during any of the HPLC trials. The test substance was detected when the solution was analyzed in by-pass mode (i.e. without analytical column). This indicates that the test substance interacted strongly with the analytical column and no eluting of the compounds occurred.

The reference substance was detected and had a retention time of 2.9 minutes.

Validity criteria fulfilled:
yes
Conclusions:
In a study according the EC C.19 guideline (OECD 121) the adsorption coefficient Koc of the test item was studied. It was found that the test item strongly interacted with the analytical column. The reference substance 2,4 -DDT was detected and had a retention time of 2.9 minutes. Based on the results obtained it was concluded that the test substance has a Koc value of higher than the reference substance 2,4-DDT. It corresponds with Koc and log Koc value for the test substance of > 427000 and > 5,63, respectively.
Executive summary:

In a study according the EC C.19 guideline (OECD 121) the adsorption coefficient Koc of the test item was studied. It was found that the test item strongly interacted with the analytical column. The reference substance 2,4 -DDT was detected and had a retention time of 2.9 minutes. Based on the results obtained it was concluded that the test substance has a Koc value of higher than the reference substance 2,4-DDT. It corresponds with Koc and log Koc value for the test substance of > 427000 and > 5,63, respectively.

Endpoint:
adsorption / desorption
Remarks:
adsorption
Type of information:
calculation (if not (Q)SAR)
Remarks:
Migrated phrase: estimated by calculation
Adequacy of study:
supporting study
Reliability:
4 (not assignable)
Rationale for reliability incl. deficiencies:
other: no information available whether the calculation model is validated for the substance under investigation
Principles of method if other than guideline:
The soil sorption coefficient Koc of imidazolium compounds, 2-(C17 and C17-unsatd. alkyl)-1-[2-(C18 and C18-unsatd. amido)ethyl]-4,5-dihydro-1-methyl, Me sulfates was calculated using EPIWIN v3.20, PCKOCWIN v1.66.
Type of method:
other: calculation
Media:
soil
Type:
log Koc
Value:
10.95

The estimation of the soil sorption coefficient Koc via EPIWIN v3.20, PCKOCWIN v1.66 yielded a value of 8.97 x 10E10 (log Koc=10.953). The calculated Koc would indicate a very high soil sorption. Due to missing information about the applicability of the calculation model in respect to the substance under investigation the result and the conclusion thereoff should be treated with care.

Conclusions:
The soil sorption coefficient Koc of imidazolium compounds, 2-(C17 and C17-unsatd. alkyl)-1-[2-(C18 and C18-unsatd. amido)ethyl]-4,5-dihydro-1-methyl, Me sulfates was calculated using EPIWIN v3.20, PCKOCWIN v1.66. The estimation yielded a Koc=8.97 x 10E10 (log Koc=10.953). This value would indicate a very high soil sorption. Due to missing information about the applicability of the calculation model in respect to the substance under investigation the result and the conclusion thereoff should be treated with care.

Description of key information

Oleic-acid based IQAC, DMS quaternised will strongly interact with soils, sediment and suspended matter in natural environment. It is technically not feasible to determine a concrete soil sorption coefficient.

Key value for chemical safety assessment

Koc at 20 °C:
502 775

Additional information

In a study conducted according to OECD guideline 106 (2000) five standard soils were incubated with the test item at concentrations of 2 mg test item /L (concentration used for adsorption kinetics), 1, 0.2, 0.1 and 0.02 mg test item /L for the following durations:

Tier 1: 24h

Tier 2: 0.25h, 0.5h, 1h for all soils

2h, 4h, 6h, 24h for soils LUFA 2.2 and 2.4

Desorption kinetics: 2h, 4h, 24h and 72h

Adsorption isotherms: 1h

Based on the obtained results the adsorption of the test item is nearly 100% in all soils and desorption is very low, thus, the test item HH-2014-548 adsorbs to all tested soils with Koc values above 135000 and is therefore immobile in soiis according to McCall et al. The adsorption was not reversible.

Some numerical results are listed in the following table:

Soil Soil / Solution 
Ratio Kd 
[mL/g] Koc 
[mL/g] logKoc Mobility according 
to McCall et al. 
based on Koc
LUFA 2.1 1:10 1986 276659 5.44 immobile
LUFA 2.2 1:10 2051 139531 5.14 immobile
LUFA 2.3 1:10 4890 1186903 6.07 immobile
LUFA 2.4 1:10 5660 325254 5.51 immobile
LUFA 5M 1:10 5364 585528 5.77 immobile
    arithmetic mean Koc 502775 5.59 arithmetic mean logKoc

In a study according the EC C.19 guideline (OECD 121) the adsorption coefficient Koc of the test item was studied. It was found that the test item strongly interacted with the analytical column. The reference substance 2,4 -DDT was detected and had a retention time of 2.9 minutes. Based on the results obtained it was concluded that the test substance has a Koc value of higher than the reference substance 2,4-DDT. It corresponds with Koc and log Koc value for the test substance of > 427000 and > 5.63, respectively.A concrete soil sorption coefficient could not be determined as the test item was not eluted from the column. In the guideline, however, it is stated that the method may not work for surface active substances and the results confirm this. Therefore this study is not appropriate to determine the soil sorption coefficient.

The soil sorption coefficient was also calculated using EPIWINv3.20, PCKOCWIN v1.66, resulting in a very high soil sorption coefficient of 11. EPIWIN is not outlined to calculate properties of ionic substances, Therefore this value is not suitable fort he assessment.

Furthermore it is not opportune to determine a Koc from log Kow because the common Koc derivations are not valid for surface active substances (EU RAR 2009, see also REACH Reference guidance 7a, section R7.1.15).