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EC number: 810-418-2 | CAS number: 1703784-30-8
- Life Cycle description
- Uses advised against
- Endpoint summary
- Appearance / physical state / colour
- Melting point / freezing point
- Boiling point
- Density
- Particle size distribution (Granulometry)
- Vapour pressure
- Partition coefficient
- Water solubility
- Solubility in organic solvents / fat solubility
- Surface tension
- Flash point
- Auto flammability
- Flammability
- Explosiveness
- Oxidising properties
- Oxidation reduction potential
- Stability in organic solvents and identity of relevant degradation products
- Storage stability and reactivity towards container material
- Stability: thermal, sunlight, metals
- pH
- Dissociation constant
- Viscosity
- Additional physico-chemical information
- Additional physico-chemical properties of nanomaterials
- Nanomaterial agglomeration / aggregation
- Nanomaterial crystalline phase
- Nanomaterial crystallite and grain size
- Nanomaterial aspect ratio / shape
- Nanomaterial specific surface area
- Nanomaterial Zeta potential
- Nanomaterial surface chemistry
- Nanomaterial dustiness
- Nanomaterial porosity
- Nanomaterial pour density
- Nanomaterial photocatalytic activity
- Nanomaterial radical formation potential
- Nanomaterial catalytic activity
- Endpoint summary
- Stability
- Biodegradation
- Bioaccumulation
- Transport and distribution
- Environmental data
- Additional information on environmental fate and behaviour
- Ecotoxicological Summary
- Aquatic toxicity
- Endpoint summary
- Short-term toxicity to fish
- Long-term toxicity to fish
- Short-term toxicity to aquatic invertebrates
- Long-term toxicity to aquatic invertebrates
- Toxicity to aquatic algae and cyanobacteria
- Toxicity to aquatic plants other than algae
- Toxicity to microorganisms
- Endocrine disrupter testing in aquatic vertebrates – in vivo
- Toxicity to other aquatic organisms
- Sediment toxicity
- Terrestrial toxicity
- Biological effects monitoring
- Biotransformation and kinetics
- Additional ecotoxological information
- Toxicological Summary
- Toxicokinetics, metabolism and distribution
- Acute Toxicity
- Irritation / corrosion
- Sensitisation
- Repeated dose toxicity
- Genetic toxicity
- Carcinogenicity
- Toxicity to reproduction
- Specific investigations
- Exposure related observations in humans
- Toxic effects on livestock and pets
- Additional toxicological data
Adsorption / desorption
Administrative data
- Endpoint:
- adsorption / desorption, other
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 2019-06-24 to 2019-10-15
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
Data source
Reference
- Reference Type:
- study report
- Title:
- Unnamed
- Year:
- 2 019
- Report date:
- 2019
Materials and methods
Test guidelineopen allclose all
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 106 (Adsorption - Desorption Using a Batch Equilibrium Method)
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- other: Council Regulation (EC) No. 440/2008, Method C.18 (2008)
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Type of method:
- batch equilibrium method
- Media:
- soil
Test material
- Reference substance name:
- Reaction products of acrylonitrile and 2,2’-Iminodi(ethylamine), hydrogenated
- EC Number:
- 810-418-2
- Cas Number:
- 1703784-30-8
- IUPAC Name:
- Reaction products of acrylonitrile and 2,2’-Iminodi(ethylamine), hydrogenated
- Test material form:
- liquid
- Details on test material:
- Trade name Ortegol LA 2
CAS-No. 1703784-30-8
Batch number 2298695
Active substance/ 2-propenenitrile, reaction products with diethylenetriamine, hydrogenated
Purity 100% / mixture of different chain lengths and branched structures
Components / Aminopropyldiethylenetriamine APDETA / 6.2%
Content (certified) Bis-Aminopropyldiethylenetriamine BAPDETA / 64.3%
Tris- Aminopropyldiethylenetriamine TAPDETA / 24.0%
Appearance colorless - light yellowish liquid
Expiry date 2019-12-31
Recommended storage At room temperature, protected from light, under N2 in the tightly closed container in a dry, cool (room temperature), well-ventilated area
Constituent 1
- Radiolabelling:
- no
Study design
- Test temperature:
- Nominal: 20 - 25 °C
Batch equilibrium or other method
- Analytical monitoring:
- yes
- Details on sampling:
- Test Procedure
The study was performed in accordance to OECD-Guideline for Testing of Chemicals No. 106 (2000) and Council Regulation (EC) No. 440/2008, C.18 (2008).
Test vessels
Disposable centrifugation tubes (polypropylene) and disposable glass bottles
Concentration for adsorption experiments
50 mg test item /L
15.8 mg test item /L
5 mg test item /L (concentration used for adsorption / desorption kinetics)
1.58 mg test item /L
0.5 mg test item /L
Stock solutions
Stock solutions of 10 and 1 g/L of the test item in ultrapure water 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.
As aqueous stock solutions were used for spiking, max. 0.5 volume-% of these stock solutions were used in order to adjust the test concentrations. Afterwards, the samples were agitated.
Samples for analysis
The soil suspensions were centrifuged after agitation at 4000 rpm to separate the phases, followed by analysing the concentration of the test item in aqueous phase by LC-MS. For analysis of the soil, the aqueous phase was decanted and the soil was extracted. Extracts were also analysed by LC-MS.
Replicates
All samples were prepared in duplicate.
Sampling points
Tier 2: 0.5 h, 1 h, 2 h, 4 h
Tier 3: 2h, 24 h for desorption isotherms
CONTROLS
CaCl2-solution was conditioned as described above, followed by separation of the aqueous phase by centrifugation. Then the aqueous phase was fortified acc. to the concentrations used for the test item samples to verify the stability of the test item in the aqueous phase under test conditions. The samples were agitated as long as the test item sample with the longest agitation period. For adsorption isotherm, the lowest test item loading level was used as concentration for test item control replicates.
Replicates
Duplicates (tier 1 and tier 2)
BLANK
Blank samples were prepared for all soils as described for the test item samples but without fortification with the test item. The samples were agitated as long as the samples with the longest agitation period.
Dispersion treatment
Agitation
Sample Preparation Tier 1
Dilution medium
Acetonitrile containing 10 mM perfluoro heptanoic acid and 2% formic acid : 0.01 M CaCl2 solution conditioned with the respective soil ( 50 : 50 )
Standards
A stock solution of 10 g test item/L in ultrapure water was prepared. The solution was diluted to 7 calibration standards in the range of 20 to 200 µg test item/L with dilution medium.
Aqueous phase
After centrifugation, an aliquot of each aqueous sample was stabilized by dilution with acetonitrile containing 10 mM perfluoro heptanoic acid and 2% formic acid (factor 2).
Soil extraction
The wet soil was used for extraction after decantation of the aqueous phase. The soil was extracted at 20 -25 °C. 30 mL methanol : ultrapure water (75 : 25 v/v) containing 0.3 mol/L sodium hydroxide were added to the wet soil. An ultrasonic bath was used for 10 min. The vessel was shaken for 60 min. The suspensions were centrifuged at 4000 rpm for 5 min. The extraction was repeated twice without the use of the ultrasonic bath. During the third extraction cycle the vessel was shaken for 30 min. The extracts were transferred quantitatively into a 100 mL measuring flask and filled up with methanol : ultrapure water (75 : 25 v/v) containing 0.3 mol/L sodium hydroxide.
Sample Preparation Tier 2 and Tier 3
Dilution medium
Acetonitrile : ultrapure water (90 : 10) containing 0.05%(v/v) heptafluorobutyric acid : 0.01 M CaCl2 solution conditioned with the respective soil (50 : 50)
Standards
A stock solution of 10 g test item/L in ultrapure water was prepared. The solution was diluted to 6 calibration standards in the range of 50 to 500 µg test item/L with dilution medium.
Aqueous phase
After centrifugation, an aliquot of each aqueous sample was stabilized by dilution with acetonitrile : ultrapure water (90 : 10) containing 0.05%(v/v) heptafluorobutyric acid (factor 2).
Soil extraction
See above for tier 1.
Matrix propertiesopen allclose all
- Matrix no.:
- #1
- Matrix type:
- other: silty sand
- % Clay:
- 4.1
- % Silt:
- 10.5
- % Sand:
- 85.4
- % Org. carbon:
- 0.718
- pH:
- 6.1
- CEC:
- 2.4 other: mval/100 g
- Matrix no.:
- #2
- Matrix type:
- loamy sand
- % Clay:
- 8.5
- % Silt:
- 11.3
- % Sand:
- 80.2
- % Org. carbon:
- 1.47
- pH:
- 6.8
- CEC:
- 7.6 other: mval/100 g
- Matrix no.:
- #3
- Matrix type:
- other: silty sand
- % Clay:
- 8.6
- % Silt:
- 29.3
- % Sand:
- 62.1
- % Org. carbon:
- 0.412
- pH:
- 6.9
- CEC:
- 4.9 other: mval/100 g
- Matrix no.:
- #4
- Matrix type:
- clay loam
- % Clay:
- 23.3
- % Silt:
- 38.6
- % Sand:
- 38.1
- % Org. carbon:
- 1.85
- pH:
- 7.4
- CEC:
- 22 other: mval/100 g
- Matrix no.:
- #5
- Matrix type:
- other: Dystric Cambisol
- % Clay:
- 17.6
- % Silt:
- 35
- % Sand:
- 47.4
- % Org. carbon:
- 3.12
- pH:
- 6.5
- CEC:
- 8.5 other: mval/100 g
- Details on matrix:
- Reason for the selection
These matrices are suitable for the conduction of the study because all parameters with impact on the adsorption / desorption behavior of a chemical substance were considered.
Tier 1 was conducted with LUFA soils 2.2 and 2.4.
Origin of soils
Landwirtschaftliche Untersuchungs- und Forschungsanstalt LUFA Speyer, Obere Langgasse 40, 67346 Speyer, Germany
European Commission Joint Research Centre, Institute for Reference Materials and Measurements IRMM, Retieseweg, B-2440 Geel, Belgium
Storage at test facility
Room temperature, in closed containers - Details on test conditions:
- CaCl2-solution:
Ultrapure water was used to prepare the CaCl2-solution (0.01 M).
Soil / Solution ratio
Tier 1: 1:10, 1:40 and 1:100
Tier 2 and Tier 3: 1:100
Agitation By horizontal shaker. Frequency was adjusted to avoid sedimentation of soil particles during treatment.
Test temperature
The temperature was mainly in the range of 20 to 25 °C during the course of the study. Deviation from this temperature range occurred only for brief periods (< 1h) with a temperature between 18 and 20 °C.The test temperature reached a minimum of 18.6 °C during the study for a short period. Regulation of the air conditioning was occasionally necessary for a couple of minutes. This caused that the temperature dropped.
This deviation is considered to have no negative impact on the integrity and quality of the study.
Results and discussion
Adsorption coefficientopen allclose all
- Key result
- Sample No.:
- #1
- Type:
- Kd
- Value:
- 782 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.1 soil/solution ratio 1:100
- % Org. carbon:
- 0.718
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #1
- Type:
- Koc
- Value:
- 108 956 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.1 soil/solution ratio 1:100
- % Org. carbon:
- 0.718
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #2
- Type:
- Kd
- Value:
- 2 658 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.2 soil/solution ratio 1:100
- % Org. carbon:
- 1.47
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #2
- Type:
- Koc
- Value:
- 180 810 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.2 soil/solution ratio 1:100
- % Org. carbon:
- 1.47
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #3
- Type:
- Kd
- Value:
- 2 181 L/kg
- pH:
- 9.4
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.3 soil/solution ratio 1:100
- % Org. carbon:
- 0.412
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #3
- Type:
- Koc
- Value:
- 529 473 L/kg
- pH:
- 9.4
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.3 soil/solution ratio 1:100
- % Org. carbon:
- 0.412
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #4
- Type:
- Kd
- Value:
- 3 869 L/kg
- pH:
- 9.2
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.4 soil/solution ratio 1:100
- % Org. carbon:
- 1.85
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #4
- Type:
- log Koc
- Value:
- 209 160 L/kg
- pH:
- 9.2
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.4 soil/solution ratio 1:100
- % Org. carbon:
- 1.85
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #5
- Type:
- Kd
- Value:
- 2 193 L/kg
- pH:
- 7.6
- Temp.:
- 20 °C
- Matrix:
- Eurosoil 3 soil/solution ratio 1:100
- % Org. carbon:
- 3.12
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #5
- Type:
- Koc
- Value:
- 70 300 L/kg
- pH:
- 7.6
- Temp.:
- 20 °C
- Matrix:
- Eurosoil 3 soil/solution ratio 1:100
- % Org. carbon:
- 3.12
- Remarks on result:
- other: Bis-Aminopropyldiethylenetriamine BAPDETA
- Key result
- Sample No.:
- #1
- Type:
- Kd
- Value:
- 1 304 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.1 soil/solution ratio 1:100
- % Org. carbon:
- 0.718
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #1
- Type:
- Koc
- Value:
- 181 555 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.1 soil/solution ratio 1:100
- % Org. carbon:
- 0.718
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #2
- Type:
- Kd
- Value:
- 2 605 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.2 soil/solution ratio 1:100
- % Org. carbon:
- 1.47
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #2
- Type:
- Koc
- Value:
- 177 242 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.2 soil/solution ratio 1:100
- % Org. carbon:
- 1.47
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #3
- Type:
- Kd
- Value:
- 2 283 L/kg
- pH:
- 9.4
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.3 soil/solution ratio 1:100
- % Org. carbon:
- 0.412
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #3
- Type:
- Koc
- Value:
- 554 042 L/kg
- pH:
- 9.4
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.3 soil/solution ratio 1:100
- % Org. carbon:
- 0.412
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #4
- Type:
- Kd
- Value:
- 3 792 L/kg
- pH:
- 9.2
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.4 soil/solution ratio 1:100
- % Org. carbon:
- 1.85
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #4
- Type:
- Koc
- Value:
- 204 979 L/kg
- pH:
- 9.2
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.4 soil/solution ratio 1:100
- % Org. carbon:
- 1.85
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #5
- Type:
- Kd
- Value:
- 2 188 L/kg
- pH:
- 7.6
- Temp.:
- 20 °C
- Matrix:
- Eurosoil 3 soil/solution ratio 1:100
- % Org. carbon:
- 3.12
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #5
- Type:
- Koc
- Value:
- 70 131 L/kg
- pH:
- 7.6
- Temp.:
- 20 °C
- Matrix:
- Eurosoil 3 soil/solution ratio 1:100
- % Org. carbon:
- 3.12
- Remarks on result:
- other: Tris- Aminopropyldiethylenetriamine TAPDETA
- Key result
- Sample No.:
- #1
- Type:
- Kd
- Value:
- 75 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.1 soil/solution ratio 1:100
- % Org. carbon:
- 0.718
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #1
- Type:
- Koc
- Value:
- 10 477 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.1 soil/solution ratio 1:100
- % Org. carbon:
- 0.718
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #2
- Type:
- Kd
- Value:
- 1 068 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.2 soil/solution ratio 1:100
- % Org. carbon:
- 1.47
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #2
- Type:
- Koc
- Value:
- 72 663 L/kg
- pH:
- 8.7
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.2 soil/solution ratio 1:100
- % Org. carbon:
- 1.47
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #3
- Type:
- Kd
- Value:
- 1 612 L/kg
- pH:
- 9.4
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.3 soil/solution ratio 1:100
- % Org. carbon:
- 0.412
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #3
- Type:
- Koc
- Value:
- 391 310 L/kg
- pH:
- 9.4
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.3 soil/solution ratio 1:100
- % Org. carbon:
- 0.412
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #4
- Type:
- Kd
- Value:
- 3 470 L/kg
- pH:
- 9.2
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.4 soil/solution ratio 1:100
- % Org. carbon:
- 1.85
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #4
- Type:
- Koc
- Value:
- 187 593 L/kg
- pH:
- 9.2
- Temp.:
- 20 °C
- Matrix:
- LUFA 2.4 soil/solution ratio 1:100
- % Org. carbon:
- 1.85
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #5
- Type:
- Kd
- Value:
- 3 139 L/kg
- pH:
- 7.6
- Temp.:
- 20 °C
- Matrix:
- Eurosoil 3 soil/solution ratio 1:100
- % Org. carbon:
- 3.12
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
- Key result
- Sample No.:
- #5
- Type:
- Koc
- Value:
- 100 606 L/kg
- pH:
- 7.6
- Temp.:
- 20 °C
- Matrix:
- Eurosoil 3 soil/solution ratio 1:100
- % Org. carbon:
- 3.12
- Remarks on result:
- other: Aminopropyldiethylenetriamine APDETA
Any other information on results incl. tables
Results
Tier 1–Adsorption, Stability in the Test System and Test Vessel Adsorption
LUFA 2.4 was used for the first experiment for preliminary investigations on the adsorption behavior of the test item with soil / solution ratios of 1:10 and 1:40 at a concentration of 0.5 mg test item/L. Samples of the aqueous phase were taken after 4 h agitation. For both soil / solution ratios, the test item depletion in the aqueous phase was nearly quantitative(see table below). Because of the high adsorption, an additional experiment was conducted with a soil / solution of 1:100. For LUFA 2.2, the adsorption was determined only with a soil / solution ratio of 1:100. Although the test item concentration also decreased below the lowest calibration level, this soil / solution ratio was used for any further assessment, as it is the lowest technical feasible soil / solution ratio.
Tier 1: LUFA 2.2 andLUFA 2.4 – Adsorption Experiments
n = 2, aqueous phase was analysed
BAPDETA |
|||||
Soil Type |
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Adsorption |
LUFA 2.4 |
1:10 |
0.5 mg/L |
0.323 mg/L |
4 |
> 96 |
1:40 |
0.5 mg/L |
0.323 mg/L |
4 |
> 96 |
|
1:100 |
0.5 mg/L |
0.323 mg/L |
4 |
> 96 |
|
LUFA 2.2 |
1:100 |
0.5 mg/L |
0.323 mg/L |
4 |
> 96 |
TAPDETA |
|||||
Soil Type |
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Adsorption |
LUFA 2.4 |
1:10 |
0.5 mg/L |
0.121 mg/L |
4 |
> 96 |
1:40 |
0.5 mg/L |
0.121 mg/L |
4 |
> 96 |
|
1:100 |
0.5 mg/L |
0.121 mg/L |
4 |
95 |
|
LUFA 2.2 |
1:100 |
0.5 mg/L |
0.121 mg/L |
4 |
91 |
24 |
100 |
||||
APDETA |
|||||
Soil Type |
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Adsorption |
LUFA 2.4 |
1:10 |
0.5 mg/L |
0.0312 mg/L |
4 |
> 96 |
1:40 |
0.5 mg/L |
0.0312 mg/L |
4 |
> 96 |
|
1:100 |
0.5 mg/L |
0.0312 mg/L |
4 |
> 96 |
|
LUFA 2.2 |
1:100 |
0.5 mg/L |
0.0312 mg/L |
4 |
> 96 |
1 = measured concentrations were below the lowest calibration level 20 µg test item/L (LCL)
The test item control samples, samples with conditioned 0.01M CaCl2 solution but without soil, were stable over 24 h and 48 h, respectively, and verified the stability of the test item in the test system (without soil) (see table below). Test vessel adsorption was not observed, as the test item control samples did not show any decline of the test item.
Tier 1: LUFA 2.2 and LUFA 2.4 – Test Item Control Samples
n=2
BAPDETA |
|||||
Soil Type |
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Recovery Rate |
LUFA 2.4 |
1:10 |
0.5 mg/L |
0.323 mg/L |
24 |
101 |
1:40 |
0.5 mg/L |
0.323 mg/L |
24 |
104 |
|
1:100 |
0.5 mg/L |
0.323 mg/L |
48 |
93 |
|
LUFA 2.2 |
1:100 |
0.5 mg/L |
0.323 mg/L |
48 |
92 |
TAPDETA |
|||||
Soil Type |
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Recovery Rate |
LUFA 2.4 |
1:10 |
0.5 mg/L |
0.121 mg/L |
24 |
105 |
1:40 |
0.5 mg/L |
0.121 mg/L |
24 |
105 |
|
1:100 |
0.5 mg/L |
0.121 mg/L |
48 |
97 |
|
LUFA 2.2 |
1:100 |
0.5 mg/L |
0.121 mg/L |
48 |
100 |
APDETA |
|||||
Soil Type |
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Recovery Rate |
LUFA 2.4 |
1:10 |
0.5 mg/L |
0.0312 mg/L |
24 |
104 |
1:40 |
0.5 mg/L |
0.0312 mg/L |
24 |
104 |
|
1:100 |
0.5 mg/L |
0.0312 mg/L |
48 |
94 |
|
LUFA 2.2 |
1:100 |
0.5 mg/L |
0.0312 mg/L |
48 |
94 |
As an additional experiment, LUFA 2.2 was used with a soil / solution ratio of 1:100 and a test item concentration of 5 mg/L. The aqueous phase was measured at different sampling points. To proof, if the adsorption to soil is reasonable for the decline of the test item in the aqueous phase, additional replicates were spiked after sterilization with HgCl2. As the recovery rates for samples with and without sterilization were comparable (low), no biodegradation took place over the evaluated period of 1 h (see table below).
Tier 1: LUFA 2.2 – Adsorption Experiments
n = 2; aqueous phase was analysed; soil / solution ratio = 1:100
BAPDETA |
||||
Sample Type |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Adsorption |
without HgCl2 |
5 mg/L |
3.22 mg/L |
1 |
981 |
with HgCl2 |
5 mg/L |
3.22 mg/L |
1 |
97 |
TAPDETA |
||||
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Adsorption |
without HgCl2 |
5 mg/L |
1.20 mg/L |
1 |
991 |
with HgCl2 |
5 mg/L |
1.20 mg/L |
1 |
> 991 |
APDETA |
||||
Soil / Solution Ratio |
Applied concentration, test item [mg/L] |
Applied concentration, component [mg/L] |
Sampling point [h] |
Adsorption |
without HgCl2 |
5 mg/L |
0.310 mg/L |
1 |
88 |
with HgCl2 |
5 mg/L |
0.310 mg/L |
1 |
85 |
1 = measured concentrations for one replicate were below the lowest calibration level 20 µg test item/L (LCL)
Tier 1– Extraction from Soil /fresh Spikes
Various solvents and devices have been tested on freshly spiked soils. Positive results were obtained with an extraction solvent containing sodium hydroxide.
A summary of the tested extraction methods used is given in the following table.
The test item is highly adsorptive to soils. Even after extensive method development, no extraction was found to be quantitative.
Extraction using Methanol : water mixtures and sodium hydroxide was used for mass balance experiments.
Tier 1– Method Development Soil Extraction – Fresh Spikes
Applied test item: 100 µg to LUFA 2.4, n = 2
Extraction method |
Recovery rate BAPDETA [%] |
Recovery rate TAPDETA [%] |
Recovery rate APDETA [%] |
Methanol:water 80:20 + 2% formic acid, RT |
n.d. |
n.d. |
n.d. |
Methanol + 1% TFA, RT |
n.d. |
n.d. |
n.d. |
Acetonitrile + 12.5 mM PFHA + 1% FA, RT |
n.d. |
n.d. |
n.d. |
Methanol : 2-Propanol 50:50, ASE |
n.d. |
n.d. |
n.d. |
Methanol : water 50:50 + 0.2 mol/L NaOH, RT, 2 cycles 1 h |
42 |
53 |
39 |
Methanol : water 50:50 + 0.2 mol/L NaOH, RT, 2 cycles 1 h, 3rdcycles overnight |
48 |
61 |
49 |
Methanol : water 50:50 + 0.1 mol/L NaOH, ASE |
n.d. |
n.d. |
15 |
Methanol : water 50:50 + 0.2 mol/L NaOH, RT, 3 cycles 1 h |
37 |
37 |
34 |
Methanol : water 75:25 + 0.2 mol/L NaOH, RT, 3 cycles 1 h |
64 |
77 |
50 |
Methanol : water 75:25 + 0.3 mol/L NaOH, RT, 3 cycles 1 h |
86 |
90 |
67 |
Methanol : water 75:25 + 0.3 mol/L NaOH, RT, 2 cycles 1 h, 3rdcycle overnight |
61 |
80 |
55 |
n.d. = not detected
RT = room temperature
ASE = Accelerated solvent extractor
Tier 1– Mass Balance
Experiments regarding the mass balance were conducted during tier 1 with LUFA 2.2 and LUFA 2.4 with a concentration of 5 mg test item/L and sampling after 4 h adsorption. LUFA soil 2.4 was assumed to reflect the worst case scenario due to high amounts of cationic exchange capacity, organic carbon and clay. The extraction method at room temperature using methanol : water 75:25 containing 0.3 mol/L NaOH was used.
The resulting recoveries obtained with this method are shown inTable 18. Due to technical problems, only the soil extracts could be analysed. As the adsorption is expected to be > 95% from results of former experiments, and the obtained recovery rates were below 85% (except for LUFA 2.4 replicate 2), the mass balances were found to be below 90%. Therefore, analyses of both phases, aqueous phase and soil phase had to be conducted during tier 2 and tier 3.
Tier 1:Mass Balance
Soil / solution ratio: 1:100, sampling after 4 h
Applied test item concentration = 5 mg/L
Soil Type |
Replicate |
Recovery Soil BAPDETA [%] |
Recovery Soil TAPDETA [%] |
Recovery Soil APDETA [%] |
LUFA 2.2 |
1 |
76 |
77 |
70 |
2 |
80 |
80 |
73 |
|
LUFA 2.4 |
1 |
78 |
82 |
74 |
2 |
87 |
94 |
85 |
Tier 2 – Adsorption Kinetics
The determination for adsorption kinetics was performed with a nominal test item concentration of 5 mg test item/L. A soil / solution ratio of 1:100 was used for all soils. The concentrations of the test item were measured in aqueous phase and soil extracts at defined sampling points. The sampling points were 0.5 h, 1 h, 2 h and 4 h. For each soil, the adsorption equilibrium was reached after 2 h of agitation. Mass balances after 4 h were between 62% and 93%. As test item stability was confirmed during tier 1, these recovery rates indicate very strong adsorption to the soils and the low extraction efficiency for the test item. Kd and KOC values were calculated from calculated amounts in the aqueous and the solid phase (direct method). The results for the different compounds are shown in the tables below.
In parallel, test item control samples verified the test item stability in the test system without soil. The results for the test item control samples are shown in the forth table below. Recovery rates were partly above 120%, probably due to solvation effects. Nevertheless, since the 4 h aged samples were in the range of 96% to 109% related to the initially measured concentration, the stability was confirmed.
Tier 2 - Adsorption Kinetics - BAPDETA
Equilibrium Time, Measured Amounts in Aqueous Phase and Soil Extracts, Kd and KOC
Applied concentration, test item: 5 mg/L
Applied concentration, BAPDETA: 3.22 mg/L
n = 2, teq= 2 h
Soil Type |
Vaq [mL] |
msoil [g] |
madsaq [µg] |
madssoil [µg] |
Ads [%] |
MB [%] |
OC [%] |
Kd [ml/g] |
KOC [ml/g] |
LUFA 2.1 |
100 |
0.969 |
30.1 |
228 |
91 |
80 |
0.718 |
782 |
108956 |
LUFA 2.2 |
100 |
0.928 |
12.5 |
224 |
97 |
73 |
1.47 |
2658 |
180810 |
LUFA 2.3 |
100 |
0.961 |
12.2 |
256 |
97 |
83 |
0.412 |
2181 |
529473 |
LUFA 2.4 |
100 |
0.887 |
7.92 |
272 |
98 |
87 |
1.85 |
3869 |
209160 |
Eurosoil 3 |
100 |
0.982 |
10.6 |
229 |
98 |
74 |
3.12 |
2193 |
70300 |
teq = time to reach adsorption equilibrium
mtest item = Applied amount, test item
Vaq = used volume of aqueous phase
msoil = used amount of soil (dry weight)
madsaq = amount of test item in the aqueous phase after adsorption equilibrium was reached (mean value of 2 h and 4 h sampling)
madssoil = amount of test item in the soil after 4 h of agitation
Ads = adsorption after 4 h of agitation, based on depletion of the compound from aqueous phase
MB = mass Balance after 4 h of agitation
%OC = percentage of organic carbon content in the soil
Tier 2- AdsorptionKinetics - TAPDETA
Equilibrium Time, Measured Amounts in Aqueous Phase and Soil Extracts, Kd and KOC
Applied concentration, test item: 5 mg/L
Applied concentration, TAPDETA: 1.20 mg/L
n = 2, teq= 2 h
Soil Type |
Vaq [mL] |
msoil [g] |
madsaq [µg] |
madssoil [µg] |
Ads [%] |
MB [%] |
OC [%] |
Kd [ml/g] |
KOC [ml/g] |
LUFA 2.1 |
100 |
0.969 |
8.28 |
105 |
94 |
93 |
0.718 |
1304 |
181555 |
LUFA 2.2 |
100 |
0.928 |
4.77 |
98 |
97 |
85 |
1.47 |
2605 |
177242 |
LUFA 2.3 |
100 |
0.961 |
4.74 |
104 |
97 |
90 |
0.412 |
2283 |
554042 |
LUFA 2.4 |
100 |
0.887 |
3.14 |
106 |
98 |
90 |
1.85 |
3792 |
204979 |
Eurosoil 3 |
100 |
0.982 |
4.58 |
98.4 |
98 |
84 |
3.12 |
2188 |
70131 |
Tier 2 - Adsorption Kinetics - APDETA
Equilibrium Time, Measured Amounts in Aqueous Phase and Soil Extracts, Kd and KOC values
Applied concentration, test item: 5 mg/L
Applied concentration, TAPDETA: 0.310 mg/L
n = 2, teq= 2 h
Soil Type |
Vaq [mL] |
msoil [g] |
madsaq [µg] |
madssoil [µg] |
Ads [%] |
MB [%] |
OC [%] |
Kd [ml/g] |
KOC [ml/g] |
LUFA 2.1 |
100 |
0.969 |
12.8 |
9.33 |
62 |
68 |
0.718 |
75 |
10477 |
LUFA 2.2 |
100 |
0.928 |
2.84 |
17.4 |
92 |
65 |
1.47 |
1068 |
72663 |
LUFA 2.3 |
100 |
0.961 |
1.38 |
21.3 |
96 |
73 |
0.412 |
1612 |
391310 |
LUFA 2.4 |
100 |
0.887 |
0.762 |
23.5 |
98 |
78 |
1.85 |
3470 |
187593 |
Eurosoil 3 |
100 |
0.982 |
0.602 |
18.6 |
98 |
62 |
3.12 |
3139 |
100606 |
teq = time to reach adsorption equilibrium
mtest item = Applied amount, test item
Vaq = used volume of aqueous phase
msoil = used amount of soil (dry weight)
madsaq = amount of test item in the aqueous phase after adsorption equilibrium was reached (mean value of 2 h and 4 h sampling)
madssoil = amount of test item in the soil after 4 h of agitation
Ads = adsorption after 4 h of agitation, based on depletion of the compound from aqueous phase
MB = mass Balance after 4 h of agitation
%OC = percentage of organic carbon content in the soil
Tier 2 - Adsorption Kinetics – Test Item Control Samples
Applied concentration, test item: 5 mg/L; n = 2
Soil Type |
Sampling Point |
Recovery Rate [%]1 |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
||
BAPDETA |
0 h |
116 |
127 |
113 |
126 |
123 |
4 h |
99 |
103 |
97 |
107 |
97 |
|
TAPDETA |
0 h |
136 |
140 |
125 |
133 |
134 |
4 h |
109 |
108 |
104 |
108 |
98 |
|
APDETA |
0 h |
92 |
87 |
102 |
122 |
95 |
4 h |
98 |
102 |
107 |
96 |
102 |
1) 0h: Recovery rate of the nominal concentration
4h: Recovery rate of the initially measured concentration
Tier 3– Desorption
Desorption of the test item was monitored after adsorption for 4 h. The aqueous phase was analysed at three different sampling points 1 h, 3 h and 24 h. The percent of desorption after 24 h and the values for Kdes and KdesOC are given in the following table. For LUFA 2.3 and LUFA 2.4, measured values were below the lowest calibration standard. For LUFA 2.2 and Eurosoil 3, the desorption was calculated to be 3% to 4%. For LUFA 2.1, significant desorption was observed for APDETA. Therefore, desorption was tested depending on applied concentration (desorption isotherm) for this soil.
Tier 3 - Desorption Kinetics
Recovery in Aqueous Phase, Kdes and KdesOC values
Applied concentration, test item: 5 mg/L
n = 2, tdes= 24 h
|
BAPDETA |
TAPDETA |
APDETA |
||||||
Soil Type |
Des [%] |
Kdes [ml/g] |
KdesOC [ml/g] |
Des [%] |
Kdes [ml/g] |
KdesOC [ml/g] |
Des [%] |
Kdes [ml/g] |
KdesOC [ml/g] |
LUFA 2.1 |
4 |
2 |
323 |
4 |
2 |
317 |
19 |
0 |
60 |
LUFA 2.2 |
3 |
4 |
263 |
3 |
4 |
246 |
4 |
2 |
168 |
LUFA 2.3 |
< LCL |
- |
- |
< LCL |
- |
- |
< LCL |
- |
- |
LUFA 2.4 |
< LCL |
- |
- |
< LCL |
- |
- |
< LCL |
- |
- |
Eurosoil 3 |
3 |
3 |
108 |
3 |
3 |
93 |
3 |
3 |
109 |
tdes = duration of desorption experiment, after 4 h adsorption
< LCL = measured values were below lowest calibration standard
Des = desorption after 24 h
Five concentrations 0.500, 1.58, 5.0, 15.8 and 50 mg test item/L were used for determination of the desorption isotherm. Desorption samples were prepared after 2 h adsorption and were taken after 24 h desorption. The measured concentrations did not show a linear correlation in the concentration range tested.
Tier 3– Adsorption Isotherms
The adsorption isotherm was determined with the concentrations of 0.500, 1.58, 5.0, 15.8 and 50 mg test item/L after an agitation time of 2 h hours. Soil extracts and aqueous phase were analysed. As the adsorption was high (> 90%, except for LUFA 2.1 APDETA) in tier 2, the measured concentration in the lower applied concentrations were expected to be below the lowest calibration level in the aqueous phase during adsorption isotherm analysis. However, the concentrations were unexpected high in some measurements, which is not plausible if a linear correlation between concentration and adsorption is assumed. But as the test item control samples with a nominal concentration of 0.500 mg test item /L showed good recoveries, spiking and analytical method were verified.
In addition, the measured test item concentration in higher concentrations did not show a linear correlation either. The mass balances, moreover, indicate a reduced extraction efficiency in higher concentrations.
The tables below show the calculated adsorption isotherms for each soil. If measured values were below the lowest calibration standards, these values were approximated from adsorption in tier 2. As 1/n of the linear Freundlich isotherm is expected to be in the range of 0.7 to < 1.0 and r2> 0.975 indicates the applicability of the linear isotherm, it is obvious that the Freundlich model is not valid for the test item PU-2018-821 in the tested concentration range.
Tier 3 - Freundlich AdsorptionIsotherms- BAPDETA
Applied test item concentrations K1 to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations BAPDETA K1 to K5:= 31.2, 10.2, 3.22, 1.02, 0.322 mg/L
n = 2
Soil Type |
msoil [g] |
Vaq [mL] |
r2 |
1/n |
MB [%] |
Control10 h [%] |
Control22 h [%] |
LUFA 2.1 |
0.969 |
100 |
0.45 |
0.24 |
59-147 |
83 |
105 |
LUFA 2.2 |
0.928 |
100 |
0.58 |
0.43 |
56-153 |
95 |
107 |
LUFA 2.3 |
0.961 |
100 |
0.45 |
0.32 |
90-139 |
99 |
100 |
LUFA 2.4 |
0.887 |
100 |
0.50 |
0.71 |
103-131 |
92 |
108 |
Eurosoil 3 |
0.982 |
100 |
0.74 |
0.62 |
69-142 |
98 |
102 |
msoil =
used amount of soil (dry weight) [g]
Vaq = Volume aqueous phase [mL]
n = regression constant
MB = mass balance, range of replicates mean value is given, for details see section 10.3
1 = recovery rate test item control from nominal, K5, mean value of two replicates
2 = recovery rate test item control from initial, K5, mean value of two replicates
Tier 3- Freundlich Adsorption Isotherms - TAPDETA
Applied test item concentrations K1 to K5 := 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations TAPDETA K1 to K5 := 12.0, 3.79, 1.20, 0.379, 0.120 mg/L
n = 2
Soil Type |
msoil [g] |
Vaq [mL] |
r2 |
1/n |
MB [%] |
Control10 h [%] |
Control12 h [%] |
LUFA 2.1 |
0.969 |
100 |
0.92 |
0.64 |
81-152 |
85 |
113 |
LUFA 2.2 |
0.928 |
100 |
0.91 |
0.57 |
100-132 |
110 |
110 |
LUFA 2.3 |
0.961 |
100 |
0.56 |
0.37 |
93-139 |
100 |
107 |
LUFA 2.4 |
0.887 |
100 |
0.49 |
0.70 |
102-120 |
95 |
111 |
Eurosoil 3 |
0.982 |
100 |
0.81 |
0.77 |
75-141 |
105 |
105 |
Tier 3 - Freundlich Adsorption Isotherms - APDETA
Applied test item concentrations K1 to K5 := 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations APDETA K1 to K5 := 3.10, 0.980, 0.310, 0.0980, 0.0310 mg/L
n = 2
Soil Type |
msoil [g] |
Vaq [mL] |
r2 |
1/n |
MB [%] |
Control10 h [%] |
Control22 h [%] |
LUFA 2.1 |
0.969 |
100 |
0.39 |
0.15 |
73-215 |
93 |
100 |
LUFA 2.2 |
0.928 |
100 |
0.021 |
0.052 |
44-110 |
87 |
109 |
LUFA 2.3 |
0.961 |
100 |
0.74 |
0.30 |
71-103 |
95 |
99 |
LUFA 2.4 |
0.887 |
100 |
0.60 |
0.50 |
44-80 |
98 |
102 |
Eurosoil 3 |
0.982 |
100 |
0.81 |
0.42 |
66-116 |
99 |
107 |
msoil = used amount of soil (dry weight) [g]
Vaq = Volume aqueous phase [mL]
n = regression constant
MB = mass balance, range of replicates mean value is given, for details see section 10.3
1 = recovery rate test item control from nominal, K5, mean value of two replicates
2 = recovery rate test item control from initial, K5, mean value of two replicates
It should be mentioned, that the linear concentration range is often limited for highly adsorptive test items. Whereas the soil is “overloaded” in higher concentration ranges, the decline of the test item in the aqueous phase leads to difficulties regarding the accuracy of the analytical method in low concentration ranges.
Because the test item showed no linear Freudlich adsorption behaviour, additional distribution coefficients Kd and organic carbon normalized distribution coefficients KOC were calculated for all concentrations and all soils.
Individual Distribution Coefficients Kd - BAPDETA
Applied test item concentrations K1 to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations BAPDETA K1 to K5:= 31.2, 10.2, 3.22, 1.02, 0.322 mg/L
n = 2
ApplicationConcentration
|
Kd |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
|
K1 |
9 |
66 |
17 |
616 |
108 |
K2 |
51 |
755 |
262 |
10695 |
643 |
K3 |
221 |
3315 |
3151 |
4417 |
3048 |
K4 |
815 |
1303 |
1042 |
1197 |
857 |
K5 |
365 |
619 |
486 |
454 |
366 |
Individual Distribution Coefficients Kd - TAPDETA
Applied test item concentrations K1to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations TAPDETA K1to K5:= 12.0, 3.79, 1.20, 0.379, 0.120 mg/L
n = 2
ApplicationConcentration
|
Kd |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
|
K1 |
64 |
218 |
27 |
725 |
299 |
K2 |
197 |
954 |
351 |
13213 |
615 |
K3 |
325 |
3822 |
2761 |
5343 |
3177 |
K4 |
723 |
1133 |
746 |
1260 |
713 |
K5 |
326 |
4634 |
- |
469 |
351 |
Individual Distribution Coefficients Kd - APDETA
Applied test item concentrations K1to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations APDETA K1to K5:= 3.10, 0.980, 0.310, 0.0980, 0.0310 mg/L
n = 2
ApplicationConcentration
|
Kd |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
|
K1 |
8 |
4 |
17 |
104 |
38 |
K2 |
8 |
149 |
41 |
9230 |
546 |
K3 |
15 |
2773 |
2128 |
4100 |
3330 |
K4 |
786 |
3299 |
2321 |
1508 |
3491 |
K5 |
436 |
3847 |
2352 |
2351 |
3680 |
Individual Carbon Normalized Distribution Coefficients KOC - BAPDETA
Applied test item concentrations K1 to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations BAPDETA K1 to K5:= 31.2, 10.2, 3.22, 1.02, 0.322 mg/L
n = 2
ApplicationConcentration
|
KOC |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
|
K1 |
1190 |
4465 |
4194 |
33289 |
3446 |
K2 |
7142 |
51352 |
63618 |
578083 |
20596 |
K3 |
30823 |
225528 |
764764 |
238759 |
97678 |
K4 |
113548 |
88610 |
252811 |
64721 |
27479 |
K5 |
50784 |
42106 |
117898 |
24554 |
11723 |
Individual Carbon Normalized Distribution Coefficients KOC - TAPDETA
Applied test item concentrations K1 to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations TAPDETA K1 to K5:= 12.0, 3.79, 1.20, 0.379, 0.120 mg/L
n = 2
ApplicationConcentration
|
KOC |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
|
K1 |
8862 |
14855 |
6585 |
39215 |
9576 |
K2 |
27498 |
64881 |
85205 |
714216 |
19719 |
K3 |
45290 |
259997 |
670208 |
288821 |
101816 |
K4 |
100679 |
77055 |
181131 |
68105 |
22856 |
K5 |
45368 |
315206 |
- |
25349 |
11257 |
Individual Carbon Normalized Distribution Coefficients KOC - APDETA
Applied test item concentrations K1 to K5:= 50.0, 15.8, 5.00, 1.58, 0.500 mg/L
Applied concentrations APDETA K1 to K5:= 3.10, 0.980, 0.310, 0.0980, 0.0310 mg/L
n = 2
ApplicationConcentration
|
KOC |
||||
LUFA 2.1 |
LUFA 2.2 |
LUFA 2.3 |
LUFA 2.4 |
Eurosoil 3 |
|
K1 |
1158 |
245 |
4152 |
5627 |
1222 |
K2 |
1095 |
10154 |
9863 |
498900 |
17501 |
K3 |
2104 |
188624 |
516575 |
221606 |
106729 |
K4 |
109488 |
224401 |
563384 |
81538 |
111888 |
K5 |
60692 |
261686 |
570753 |
127083 |
117938 |
Applicant's summary and conclusion
- Validity criteria fulfilled:
- yes
- Executive summary:
Summary
General Information
The adsorption / desorption behavior of the test item PU-2018-821 (batch no. 2298695) was investigated in five different soils according to OECD guideline 106 and Council Regulation (EC) No. 440/2008, C.18 from 2019-06-24 to 2019-10-15 at Noack Laboratorien GmbH, 31157 Sarstedt, Germany.
Distribution coefficients Kd and organic carbon normalized distribution coefficients KOC were determined with a single concentration. Furthermore, investigations about the adsorption as a function of the test item loading level (Freundlich adsorption isotherms) in the aqueous phase were performed. Three components of the test item, Aminopropyldiethylenetriamine (APDETA), Bis-aminopropyldiethylenetriamine (BAPDETA) and tris-aminopropyldiethylenetriamine (TAPDETA) were analysed by LC-MS/MS. With an overall yield of 94.5%, these components are suitable to investigate the adsorption/desorption behavior of the test item. Determined adsorption coefficients are given for the individual components as well as for the product itself, taking into account the respective amounts.
Relevant properties of the used soils are given in Table 1 below. Experiments for adsorption kinetics were conducted with a nominal test item concentration of 5 mg test item/L (K3). Additional concentrations of 50.0, 15.8, 5.00, 1.58, 0.500 mg/L (K1, K2, K3, K4, K5) were used for the determination of the Freundlich adsorption isotherms.
Table1: RelevantCharacteristics of Test Matrices
Soils
LUFA 2.1
LUFA 2.2
LUFA 2.3
LUFA 2.4
Eurosoil 3
batch
F2.1 2817
F2.2 4016
F2.3 4116
F2.4 2617
160718
Soil Type1)
Silty sand1)
Loamy sand1)
Silty sand1)
Clayey loam1)
Dystric Cambisol4)
pH (0.01 M CaCl2)3)
4.9
5.4
5.9
7.4
5.55)
Organic Carbon [%]2)
0.718
1.47
0.412
1.85
3.12
Clay (<0.002 mm) [%]2)
4.1
8.5
8.6
23.3
17.6
Silt (0.002-0.063 mm) [%]2)
10.5
11.3
29.3
38.6
35.0
Sand (0.063-2 mm) [%]2)
85.4
80.2
62.1
38.1
47.4
Cation Exchange Capacity [mval/100g]2)
2.4
7.6
4.9
22
8.5
1) according to German DIN
2) determined at Agrolab Agrar und Umwelt GmbH (non-GLP)
3) Analyses data sheet provided by LUFA
4) data taken from Gawlik and Muntau, Eurosoils II Laboratory and Reference Materials for Soil-related Studies, Environment Institute 1999
5) actual certified value on the corresponding soil certificate
Results Tier 1
During experiments in tier 1 test item control samples (the test item dissolved in soil eluates of LUFA 2.2 and LUFA 2.4) showed that the test item is stable in the aqueous phase and no indication for adsorption to the test vessel takes place. As matrix effects were observed during analyses, matrix-matched standards were prepared.
The parental mass balance for the test item was determined in the LUFA soils 2.2 and 2.4 with an application concentration of 5 mg/L, a soil / solution ratio of 1:100 and over an agitation time of 4 h. The parental mass balances were finally calculated by taking into account the test item recovery in the aqueous phase, the soil and residual test item in pore water. Mass balances below 90% were obtained. Therefore, the direct method was used throughout tier 2 and tier 3.
Results Tier 2 – Adsorption Kinetics
These experiments confirmed the results of tier 1. The test item was highly adsorptive and the adsorption equilibrium was determined after 2 h agitation. Results are shown in Table 2 below.
Table2: Summarized Endpoints for the Components of PU-2018-821
Mobility according to McCall et al. (1980):KOC 0 – 50 very high, KOC 50 – 150 high, KOC 150 – 500 medium, KOC 500 – 2000 low, KOC 2000 – 5000 slight, KOC > 5000 immobile; based on results of tier 2
Soil Type
Kd[mL/g]
KOC[mL/g]
Mobility according to McCall et al.
BAPDETA
LUFA 2.1
782
108956
immobile
LUFA 2.2
2658
180810
immobile
LUFA 2.3
2181
529473
immobile
LUFA 2.4
3869
209160
immobile
Eurosoil 3
2193
70300
immobile
TAPDETA
LUFA 2.1
1304
181555
immobile
LUFA 2.2
2605
177242
immobile
LUFA 2.3
2283
554042
immobile
LUFA 2.4
3792
204979
immobile
Eurosoil 3
2188
70131
immobile
APDETA
LUFA 2.1
75
10477
immobile
LUFA 2.2
1068
72663
immobile
LUFA 2.3
1612
391310
immobile
LUFA 2.4
3470
187593
immobile
Eurosoil 3
3139
100606
immobile
PU-2018-8211
LUFA 2.1
868
120933
immobile
LUFA 2.2
2540
172808
immobile
LUFA 2.3
2170
526648
immobile
LUFA 2.4
3823
206683
immobile
Eurosoil 3
2254
72245
immobile
1 = Weighted mean value of both analysed components, content of components taken into account
Results Tier 3
Results Tier 3 – Desorption Kinetics and Desorption Isotherms
Only in LUFA 2.1, significant desorption (for APDETA) was observed during desorption kinetics. Therefore, only this soil was used for desorption isotherm experiments. The determined desorption isotherm did not show a linear trend.
Results Tier 3 – Adsorption Isotherms
As the adsorption was high (> 90%, except for LUFA 2.1 APDETA) in tier 2, the measured concentration in the lower applied concentrations were expected to be below the lowest calibration level in the aqueous phase during adsorption isotherm analysis. However, the concentrations were unexpected high in some measurements, which is not plausible if a linear correlation between concentration and adsorption is assumed. But as the test item control samples with a nominal concentration of 0.500 mg test item /L showed good recoveries, spiking and analytical method were verified.
In addition, the measured test item concentration in higher concentrations did not show a linear correlation either. The mass balances, moreover, indicate a reduced extraction efficiency in higher concentrations. If measured values were below the lowest calibration standards, these values were approximated from adsorption in tier 2. As 1/n of the linear Freundlich isotherm is expected to be in the range of 0.7 to < 1.0 and r2 > 0.975 indicates the applicability of the linear isotherm, it is obvious that the Freundlich model is not valid for the test item PU-2018-821 in the tested concentration range.
Individual values for Kd and KOC were calculated for each soil and each concentration. But due to above described limitations for the applicability of the Freundlich model, it is recommended to use the results of tier 2 for risk assessment.
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