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Environmental fate & pathways

Biodegradation in water and sediment: simulation tests

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Reference
Endpoint:
biodegradation in water: sediment simulation testing
Type of information:
experimental study
Adequacy of study:
key study
Study period:
11 Jun 2011 – 17 Feb 2014
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
guideline study
Qualifier:
according to guideline
Guideline:
OECD Guideline 308 (Aerobic and Anaerobic Transformation in Aquatic Sediment Systems)
Version / remarks:
2002
Qualifier:
according to guideline
Guideline:
EPA OPPTS 835.4300 (Aerobic Aquatic Metabolism)
Version / remarks:
2008
Qualifier:
according to guideline
Guideline:
EPA OPPTS 835.4400 (Anaerobic Aquatic Metabolism)
Version / remarks:
2008
GLP compliance:
yes (incl. QA statement)
Radiolabelling:
yes
Oxygen conditions:
aerobic
Inoculum or test system:
natural water / sediment: freshwater
Details on source and properties of sediment:
- Details on collection (e.g. location, sampling depth, contamination history, procedure):
Water/Sediment system 1: Anglersee; Leverkusen/North Rhine-Westphalia/Germany; small, reclaimed gravel pit which is used for fishing only.
Water/Sediment system 2: Wiehltalsperre; close to Wiehl near Gummersbach/North Rhine-Westphalia/Germany; fresh water dam that is used for the preparation of drinking water, water and sediment collected from the forebay Nespen.
Water and sediment were taken in 1 to 2 m distance to the lakefronts and filled separately in plastic containers. Sediment was obtained from the upper sediment layer (5 – 10 cm thickness). No pesticides were used for previous 5 years at both locations.
- Storage conditions: At ambient conditions in the laboratory
- Storage length prior to use: Overnight until start of equilibration
- Textural classification (i.e. %sand/silt/clay): sand (Water/Sediment system Anglersee), silt loam (Water/Sediment system Wiehltalsperre)
- pH at time of collection: 7.1 (Anglersee), 6.5 (Wiehltalsperre)
- Organic carbon (mg/kg): 5400 (Anglersee), 70000 (Wiehltalsperre)
- Redox potential (mv) initial/final:171 (Anglersee), 126 (Wiehltalsperre)
- CEC (meq/100 g): 3.4 (Anglersee), 8.6 (Wiehltalsperre)
- Sediment samples sieved: Sieved to 2 mm mesh-size
Duration of test (contact time):
101 d
Initial conc.:
90 µg/L
Based on:
act. ingr.
Parameter followed for biodegradation estimation:
radiochem. meas.
test mat. analysis
Details on study design:
TEST CONDITIONS
- Volume of test solution/treatment: 400 μL of application solution were applied dropwise onto the water surface of the respective equilibrated test systems using a pipette.
- Test temperature: 20.0 °C
- pH: 6.7 (Anglersee), 4.7 (Wiehltalsperre)
- Continuous darkness: yes
- Other: The untreated test systems were equilibrated to study conditions for 12 days prior to application.

TEST SYSTEM
- Culturing apparatus: Special cylindrical glass containers (volume about 1000 mL, inner diameter about 10.5 cm, surface area about 86.6 cm2) were used as test vessels and each container was fitted with a glass stirrer for smoothly movement of the water layer.
- Number of culture flasks/concentration: 16
- Method used to create aerobic conditions: Stirrer and trap attachments were permeable for oxygen. As from DAT-0 to DAT-3 decreasing oxygen contents and redox potentials were observed in the water layer, the velocity of the shaker was increased from 60 rpm at DAT-0 to 65 rpm at DAT-3 and further to 70 rpm from DAT-7 onwards.
- Details of trap for CO2 and volatile organics if used: Every container had a trap attachment (permeable for oxygen) containing soda lime for absorption of carbon dioxide and a polyurethane (PU) foam plug for adsorption of volatile organic compounds.
- Other: For preparation of the test systems, wet sediment with a weight equivalent to a volume of 175 mL was filled into each test vessel and 520 mL of the corresponding water were added.

SAMPLING
- Sampling frequency: Duplicate samples were processed and analyzed 0, 3, 7, 14, 30, 50, 70 and 101 days after treatment (DAT).
- Sample storage before analysis:
The PU foam plugs were processed and analyzed within 1 day after sampling.
The soda lime traps were stored before processing at ambient temperature in the laboratory for a maximum period of 12 weeks.
For determination of dissolved carbon dioxide subsamples of water were made alkaline and stored before processing for a maximum period of 12 weeks.
Water and sediment extracts were stored in a freezer in the dark. The maximum sample storage period was 35 days.
The exhaustive extracted sediments were lyophilized and stored at ambient temperature in the laboratory.
Compartment:
natural water / sediment: freshwater
% Total extractable:
93.4
% Non extractable:
5.7
% CO2:
0.7
% Other volatiles:
< 0.1
% Recovery:
99.8
Remarks on result:
other:
Remarks:
Radioactivity distribution in the water/Sediment system Anglersee after 101 days
Compartment:
natural water / sediment: freshwater
% Total extractable:
46.7
% Non extractable:
48.1
% CO2:
1
% Other volatiles:
< 0.1
% Recovery:
95.8
Remarks on result:
other:
Remarks:
Radioactivity distribution in the water/Sediment system Wiehltalsperre after 101 days
Parent/product:
parent
Compartment:
total system
% Degr.:
0.7
Parameter:
radiochem. meas.
Sampling time:
101 d
Remarks on result:
other:
Remarks:
Mineralisation to 14CO2 after 101 days in the water/sediment system Anglersee
Parent/product:
parent
Compartment:
total system
% Degr.:
1
Parameter:
radiochem. meas.
Sampling time:
101 d
Remarks on result:
other:
Remarks:
Mineralisation to 14CO2 after 101 days in the water/sediment system Wiehltalsperre
Compartment:
natural water: freshwater
DT50:
24.2 d
Type:
other: Single first order (SFO)
Temp.:
20 °C
Remarks on result:
other:
Remarks:
Water/Sediment system: Anglersee
Compartment:
natural water: freshwater
DT50:
51.4 d
Type:
(pseudo-)first order (= half-life)
Temp.:
12 °C
Remarks on result:
other:
Remarks:
Calculated DT50 based on results at 20 °C in water/sediment system Anglersee
Compartment:
natural water / sediment: freshwater
DT50:
35.1 d
Type:
other: Single first order (SFO)
Temp.:
20 °C
Remarks on result:
other:
Remarks:
Water/Sediment system: Anglersee
Compartment:
natural water / sediment: freshwater
DT50:
74.5 d
Type:
(pseudo-)first order (= half-life)
Temp.:
12 °C
Remarks on result:
other:
Remarks:
Calculated DT50 based on results at 20 °C in water/sediment system Anglersee
Compartment:
natural water: freshwater
DT50:
6.3 d
Type:
other: Double first order in parallel (DFOP)
Temp.:
20 °C
Remarks on result:
other:
Remarks:
Water/Sediment system: Wiehltalsperre
Compartment:
natural water: freshwater
DT50:
13.4 d
Type:
(pseudo-)first order (= half-life)
Temp.:
12 °C
Remarks on result:
other:
Remarks:
Calculated DT50 based on results at 20 °C in water/sediment system Wiehltalsperre
Compartment:
natural water / sediment: freshwater
DT50:
20.8 d
Type:
other: Double first order in parallel (DFOP)
Temp.:
20 °C
Remarks on result:
other:
Remarks:
Water/Sediment system: Wiehltalsperre
Compartment:
natural water / sediment: freshwater
DT50:
44.2 d
Type:
(pseudo-)first order (= half-life)
Temp.:
12 °C
Remarks on result:
other:
Remarks:
Calculated DT50 based on results at 20 °C in water/sediment system Wiehltalsperre
Transformation products:
yes
No.:
#1
No.:
#2
No.:
#3
No.:
#4
Details on transformation products:
- Maximum occurrence of each transformation product: Four degradation products were identified with the following maximum amounts: AE 1392936 with 33.1% AR at DAT-101 in water/sediment system Anglersee, tefuryltrione-acetic-benzoic acid with 26.5% AR at DAT-70 in water/sediment system Anglersee, AE 0327513 with 27.1% AR at DAT-101 in water/sediment system Anglersee and tefuryltrione-isophthalic acid with 22.4% AR at DAT-101 in water/sediment system Wiehltalsperre.
Evaporation of parent compound:
no
Volatile metabolites:
no
Residues:
yes
Details on results:
TEST CONDITIONS
- Aerobicity (or anaerobicity), moisture, temperature and other experimental conditions maintained throughout the study: Yes

MAJOR TRANSFORMATION PRODUCTS
- Range of maximum concentrations in % of the applied amount and day(s) of incubation when observed: Four degradation products were identified with the following maximum amounts: AE 1392936 with 33.1% AR at DAT-101 in water/sediment system Anglersee, tefuryltrione-acetic-benzoic acid with 26.5% AR at DAT-70 in water/sediment system Anglersee, AE 0327513 with 27.1% AR at DAT-101 in water/sediment system Anglersee and tefuryltrione-isophthalic acid with 22.4% AR at DAT-101 in water/sediment system Wiehltalsperre.

TOTAL UNIDENTIFIED RADIOACTIVITY (RANGE) OF APPLIED AMOUNT:
The total unidentified residues amounted to a maximum of 4.3% AR and no single component exceeded 4.0% AR at any sampling interval for both water/sediment systems.

EXTRACTABLE RESIDUES
- % of applied amount at day 0: Extractable residues in the sediment of water/sediment system Anglersee increased from 0.7% AR at DAT-0 to 28.2% AR at DAT-30 and declined then to 18.4% AR at DAT-101. Extractable residues in the sediment of water/sediment system Wiehltalsperre increased from 1.4% AR at DAT-0 to 23.0% AR at DAT-30 and declined then to 22.5% AR at DAT-101.

NON-EXTRACTABLE RESIDUES
- % of applied amount at day 0: Non-extractable residues (NER) in water/sediment system Anglersee increased from 0.5% AR at DAT-0 to 8.9% AR at DAT-30 and decreased to 5.7% AR at DAT-101. In water/sediment system Wiehltalsperre NER increased from 2.4% AR at DAT-0 to 54.5% AR at DAT-50 and decreased to 48.1% AR at DAT-101.

MINERALISATION
- % of applied radioactivity present as CO2 at end of study: The maximum amount of carbon dioxide at study end (DAT-101) was 0.7% AR in water/sediment system Anglersee and 1.0% AR in water/sediment system Wiehltalsperre.

VOLATILIZATION
- % of the applied radioactivity present as volatile organics at end of study: Formation of volatile organic compounds (VOC) was insignificant as demonstrated by values of < 0.1% AR at all sampling intervals for both water/sediment systems.
Validity criteria fulfilled:
not applicable

Description of key information

DT50 in freshwater sediment at 20 °C: 6.3 - 24.2 days (13.4 - 51.4 days, recalculated to 12 °C) in the water phase; 20.8 - 35.1 days (44.2 - 74.5 days, recalculated to 12 °C) in the total system, aerobic conditions (OECD 308)

Key value for chemical safety assessment

Half-life in freshwater:
51.4 d
at the temperature of:
12 °C
Half-life in freshwater sediment:
74.5 d
at the temperature of:
12 °C

Additional information

In a laboratory study, the route and rate of degradation of radiolabeled tefuryltrione was studied in two different water/sediment systems (sand, silt loam) under aerobic conditions in the dark for 101 days at 20.0 °C. The GLP study followed the OECD Guideline No. 308. After 101 days 0.7 and 1.0% of the applied radioactivity were mineralized to 14CO2. The half-life was 24.2 (sand system) and 6.3 (silt loam system) days (51.4 and 13.4 days, recalculated to 12 °C) in the water phase and 35.1 (sand system) and 20.8 (silt loam system) days (74.5 and 44.2 days, recalculated to 12 °C) in the total system.