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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:
23 Nov 2005 to 6 Jun 2008
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:
Adopted 11 April 2002
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA Subdivision N Pesticide Guideline 162-3 (Anaerobic Aquatic Metabolism)
Version / remarks:
18 October 1982
Deviations:
no
Qualifier:
according to guideline
Guideline:
EPA Subdivision N Pesticide Guideline 162-4 (Aerobic Aquatic Metabolism)
Version / remarks:
18 October 1982
Deviations:
no
GLP compliance:
yes (incl. QA statement)
Radiolabelling:
yes
Oxygen conditions:
aerobic/anaerobic
Inoculum or test system:
natural water / sediment
Details on source and properties of surface water:
Sampling details and properties of the water are provided in Table 1 and Table 2 in 'Any other information on materials and methods incl. tables'.
- Collection location: Natural pond, Rothenfluh, BL / Switzerland and Rhine river: Möhlin, AG / Switzerland
- Sampling: Water samples were taken from the same site and at the same time as the sediments, in depth of about 20 cm below the water surface.
- Preparation before use: For the strictly anaerobic study, the water was handled and transported carefully under nitrogen.
Details on source and properties of sediment:
Sampling details and properties of the sediment are provided in Table 1 and Table 2 in 'Any other information on materials and methods incl. tables'.
- Collection location: Natural pond, Rothenfluh, BL / Switzerland and Rhine river: Möhlin, AG / Switzerland
- Sampling: Sediment samples were taken from the aerobic and anaerobic zones of the surface water bodies (entire upper layer of the sediment of 2 or 5 cm to 10 cm thickness) for the aerobic and strictly anaerobic study part, respectively.
– Preparation before use: Before use, the sediments were wet-sieved through a 2 mm sieve. For the strictly anaerobic study, the two sediments were handled and transported carefully under nitrogen.
Duration of test (contact time):
>= 181 - <= 360 d
Initial conc.:
0.04 mg/L
Based on:
test mat.
Parameter followed for biodegradation estimation:
CO2 evolution
radiochem. meas.
Details on study design:
TEST SYSTEM
- Culturing apparatus: Cylindrical 1 L metabolism flasks (i.d. 10 cm), corresponding to a surface area of 78.5 cm2
- Water-sediment ratio: Sediment dry matter to water of 1:4 (Rhein ) to 1:6 (pond) (w/w)
- Method used to create aerobic conditions: The flow through gases for the systems was air for the aerobic systems
- Method used to create anaerobic conditions: The flow through gases for the systems was oxygen-free nitrogen for the anaerobic systems. Inlet air/oxygen free nitrogen was humidified by passage through water.
- Test performed in open system: The flasks were connected to an open gas flow-through system.
- Details of trap for CO2 and volatile organics: Ethylene glycol (organic volatiles) and two 2M NaOH (CO2). The effluent gases (20 - 30 mL/min) passed through a sodium hydroxide (2M) solution traps, to capture any mineralised carbon dioxide produced. As no radioactivity were trapped and due to its hydroscopic nature, the use of the ethylene glycol traps were terminated after the 69 DAT sampling for all remainder water-sediment systems.
- Preparation of stock solution: For the preparation of the stock solution the [Pyrazole-5-14C]-labelled test item was dissolved in 5 mL acetonitrile. The radioactivity content was determined by liquid scintillation counting (LSC). The final concentration of the test item in the stock solution was 5.6 mg/ 5 mL.
- Preparation of the application solution: For the application solution, 3.6 ml of the previous stock solution was placed into a 20 ml volumetric flask and was filled with acetonitrile. The radioactivity content was determined by LSC. The final concentration of the test item in the application solution was 4.4 mg / 20 mL.
- Application of 14C-test item to water-sediment systems: Each water-sediment vessel was removed from the flow-through system, immediately prior to application. For each flask, an aliquot of ca. 190 μl of the application solution was transferred by means of a syringe into the water phase just above the sediment surface of the water/sediment system. The amount of 0.043 mg of the test substance applied to each flask corresponded to direct over-spray at a field rate of 250 g/ha assuming a uniform distribution of the substance in the upper 30 cm water layer and was chosen for analytical reasons. During treatment of the anaerobic samples the flasks were flushed with nitrogen. The 0 DAT samples were not reconnected to the flow-through system as they were analysed immediately. For each sediment, two additional vessels were treated at an exaggerated rate equivalent to 1000 g/ha sprayed over a 30 cm deep water body. These water-sediment systems were for the structural elucidation of metabolite(s) if deemed necessary. Water-sediment systems designated for redox potential measurements were not treated.

TEST CONDITIONS
- Test temperature: 20 ± 1 °C
- Continuous darkness: Yes
(Aerobic)
- pH (water): 8.0 - 8.7 (river); 7.7-8.4 (pond)
- pH (sediment): 7.0 - 7.8 (river); 7.1-7.3 (pond)
(Anaerobic)
- pH (water): 8.9 - 9.2 (river); 8.5 - 9.2 (pond)
- pH (sediment): 7.6 - 8.4 (river); 7.3 - 8.0 (pond)

SAMPLING
Sampling frequency:
- Aerobic, non-sterile: Duplicate samples from each water/sediment type except for day 1: 0, 1, 3, 7, 14, 35, 70, 100 and 181 DAT
Untreated systems for biomass or plate count; 0 and 181 DAT
- Anaerobic, non-sterile Duplicate samples from each water/sediment type except for day 1: 0, 1, 3, 7, 14, 35, 70, 100, 181 and 360 DAT
Untreated systems for biomass or plate count; 0, 181 and 360 DAT
- Microbial biomas determination and plate counts: The samples for the determination of the microbial biomass were taken before treatment and at day 181. The aliquots for the plate counts from the anaerobic samples were taken after the application, at 181 days and at 360 days.
- Trapping solutions: Trapping solution associated with the vessels sampled were removed from the flow-through system and quantified by LSC.
- Sampling method used per analysis type: At each sampling interval, the allocated water-sediment vessel for each sediment was disconnected from the incubation system. Two complete aerobic and anaerobic systems were taken, with the exception of day 1, where one sample only was taken
- Sample storage before analysis: All samples were extracted on the day of sampling.
Compartment:
natural water / sediment
% Total extractable:
88.8
% Non extractable:
3.8
% CO2:
0.5
% Recovery:
93.1
Remarks on result:
other: River; Aerobic; Day 181
Compartment:
natural water / sediment
% Total extractable:
86.3
% Non extractable:
4
% CO2:
0.6
% Recovery:
90.9
Remarks on result:
other: Pond; Aerobic; Day 181
Compartment:
natural water / sediment
% Total extractable:
92.3
% Non extractable:
2.3
% CO2:
0.1
% Recovery:
94.7
Remarks on result:
other: River; Anaerobic; Day 360
Compartment:
natural water / sediment
% Total extractable:
91.2
% Non extractable:
1.7
% CO2:
0.1
% Recovery:
92.9
Remarks on result:
other: Pond; Anaerobic; Day 360
Parent/product:
parent
Compartment:
total system
% Degr.:
24.99
Parameter:
radiochem. meas.
Sampling time:
181 d
Remarks on result:
other: River; Aerobic
Parent/product:
parent
Compartment:
total system
% Degr.:
32.45
Parameter:
radiochem. meas.
Sampling time:
181 d
Remarks on result:
other: Pond; Aerobic
Parent/product:
parent
Compartment:
total system
% Degr.:
12.63
Parameter:
radiochem. meas.
Sampling time:
360 d
Remarks on result:
other: River; Anaerobic
Parent/product:
parent
Compartment:
total system
% Degr.:
16.22
Parameter:
radiochem. meas.
Sampling time:
360 d
Remarks on result:
other: Pond; Anaerobic
Key result
Compartment:
natural water / sediment: freshwater
DT50:
> 1 yr
Type:
(pseudo-)first order (= half-life)
Temp.:
20 °C
Remarks on result:
other: River; Pond; Aerobic; Anaerobic
Remarks:
Total system
Compartment:
natural water / sediment: freshwater
DT50:
2 d
Type:
(pseudo-)first order (= half-life)
Temp.:
20 °C
Remarks on result:
other: River; Aerobic
Remarks:
Water phase
Compartment:
natural water / sediment: freshwater
DT50:
2.6 d
Type:
(pseudo-)first order (= half-life)
Temp.:
20 °C
Remarks on result:
other: Pond; Aerobic
Remarks:
Water phase
Compartment:
natural water / sediment: freshwater
DT50:
8.8 d
Type:
(pseudo-)first order (= half-life)
Temp.:
20 °C
Remarks on result:
other: River; Anaerobic
Remarks:
Water phase
Compartment:
natural water / sediment: freshwater
DT50:
7.1 d
Type:
(pseudo-)first order (= half-life)
Temp.:
20 °C
Remarks on result:
other: Pond; Anaerobic
Remarks:
Water Phase
Other kinetic parameters:
first order rate constant
pseudo-first order rate constant
Transformation products:
not specified
Remarks:
M1, M4
Details on transformation products:
An overview of the results is provided in Table 7 – Table 10 in 'Any other information on results incl. tables'.
The test item was slowly degraded and two minor metabolites were identified as M1 and M4 in both water/sediment systems under aerobic and anaerobic conditions.

- River system - aerobic incubation: In the aqueous phase the amount of test item decreased from 88.4 % to 1.7 % at day 181. The ratio of the anti isomer and syn isomer test item was kept during the whole study. Seventeen minor metabolites were detected in small amounts ≤ 2.3 % for the major one. Two of them (M4 and M1) were identified. In the sediment, the test item increased from 2.1% at day 0 to 84.1% at day 70 and decreased to 73.3% at the end of the study (mean value of two replicates). Seven minor metabolites were found in amounts ≤ 3.1 %. M1 and M4 were two of them. In the total system, the test item decreased from 90.5 % at day 0 to 75.0 % at day 181. Seventeen metabolites with amounts ≤ 3.9 % were found. M4, M1 and unknown metabolite 3 (U3) accounted for 3.4 %, 3.3 % and 3.8% in the total system (mean value).

- River system - anaerobic incubation: In the aqueous phase, the amount of test item decreased from 90.2 % to 4.2% at day 360 by dissipation into the sediment. Fifteen minor metabolites were detected (including M4, M1) in amounts ≤ 1.0%. In the sediment, the test item increased from 1.8% at day 0 to 83.2% at study termination, day 360. Nine minor metabolites were found (all under ≤ 1.5 % mean value). The amount of the test item in the total system did not decrease very significantly, from 92.1% at day 0 up to 95.3% at day 7 and decreased to 87.4% at day 360. The minor metabolites were ≤ 1.5 % mean value.

- Pond system - aerobic incubation: In the aqueous phase the amount of test item decreased from 90.4 % at day 0 to 1.2 % at day 181. Sixteen minor metabolites were detected in amounts ≤ 2.4 %. Two of them M4 and M1 were characterised. In the sediment, the test item increased from 1.8% at day 0 to 79.5% at day 70 and decreased to 66.4% at the end of the study (mean value of two replicates). Nine minor metabolites were found (≤ 3.5 %). The amount of the test item in the total system declined from 92.2 % at day 0 to 67.6 % at day 181. Sixteen metabolites were found ≤ 5.1 %. M4, M1 and U3 accounted for 4.2 %, 4.6 % and 4.4% in the total system at day 181 (mean value).

- Pond system – anaerobic incubation: In the aqueous phase, the amount of test item decreased from 89.6 % at day 0 to 2.2 % at day 360. Fifteen minor metabolites were detected in amounts ≤ 1.8 %. Two of them were M4 and M1. In the sediment, the test item increased from 1.8% at day 0 to 81.6 % at day 360. Seven minor metabolites were found (≤ 2.0 %). The amount of the test item in the total system declined from 91.4 % at day 0 to 83.8 % at day 360. Fifteen metabolites were found ≤ 2.3 %. M4 and M1 accounted at maximum for 0.8% and 0.3 % in the total system at day 360.
Evaporation of parent compound:
not specified
Volatile metabolites:
yes
Residues:
yes
Details on results:
An overview of the results is provided in Table 3 – Table 10 in 'Any other information on results incl. tables'.
- Microbial biomass and plate counts: Under aerobic conditions the microbial biomass remained relatively constant for the River system. During the study values ranged from 40.1 mg microbial carbon per 100 g dry sediment at post-handling, 39.4 mg at day 0 to 34.4 mg at 181 days. The corresponding values for the Pond system decreased from 170.4 mg (post handling) and 138.5 mg (day 0) to 89.0 mg at 181 days. Under anaerobic conditions the number of colony forming units (CFU) for River were 620000 per 1 g dry sediment at post-handling, 315000 at start of the test and 1345000 at termination. The values for Pond were 840000, 400000 and 1080000, respectively.

MASS BALANCE
The total radioactivity recovered was calculated by the sum of activity in the surface water, the sediment extracts, unextracted activity (from combustion) and that trapped as 14CO2 in the 2M sodium hydroxide trap. In all test systems the overall recovery ranged from 90.2 % to 98.5 % of the applied radioactivity (average of two replicates).

- River system- aerobic incubation: In the water layer the amount of radioactivity decreased from 88.4 % at day 0 to 7.6 % at day 181. The extractable radioactivity from the sediment increased from the start and reached a maximum of 86.5 % at 70 days, decreasing thereafter to 81.2 % at day 181. Correspondingly, non-extractables increased as the study progressed and reached a maximum of 3.8 % at day 181. Volatiles in the form of carbon dioxide steadily increased and reached 0.5 % at day 181. Organic volatiles were below limit of detection.

- River system - anaerobic incubation: The amount of radioactivity in the water layer decreased from 90.2 % at day 0 to 6.6 % at day 360. The extractable radioactivity from the sediment increased from the start reaching a maximum of 85.7 % at the end of the study, 360 days. Correspondingly, non-extractables increased as the study progressed and reached a maximum of 2.3 % at study end. Organic volatiles in the form of carbon dioxide were 0.1% at study end and other volatiles were below detection limit.

- Pond system - aerobic incubation: In the water layer the amount of radioactivity decreased continuously from 90.4 % at day 0 to 8.8 % at day 181. The extractable radioactivity from the sediment increased until day 70 (81.9 %) and decreased thereafter to 77.5 % at day 181. Non-extractables increased until study termination and reached 4.0 % at day 181. Volatiles in the form of carbon dioxide steadily increased and reached a maximum of 0.6 % at day 181. Organic volatiles were below limit of detection.

- Pond system - anaerobic incubation: In the water layer the amount of radioactivity decreased from 89.6 % at day 0 to 6.5 % at day 360. The extractable radioactivity from the sediment increased from the beginning to 84.7 % at 360 days. Non-extractables increased to 1.7% at the end of the study. Organic volatiles and volatiles in the form of carbon dioxide were below detection limit and 0.1%, respectively.

TEST CONDITIONS
- Aerobicity (or anaerobicity), moisture, temperature and other experimental conditions maintained throughout the study: Yes

Table 3. Distribution and Recovery of Radioactivity: River Aerobic Incubation

Incubation Time

Replicate / Mean

Aqueous Phase

Sediment Extracts

14CO2

Non- extractables

Recovery

days

 

% of applied radioactivity

 

0

a

88.6

2.3

n.p.

0.1

91.0

b

88.1

2.3

n.p.

0.1

90.6

mean

88.4

2.3

n.p.

0.1

90.8

 

1

a

54.1

37.8

0.0

0.8

92.7

 -

 -

 -

mean

54.1

37.8

0.0

0.8

92.7

 

3

a

30.8

60.2

0.0

0.4

91.4

b

32.1

58.6

0.0

0.4

91.2

mean

31.5

59.4

0.0

0.4

91.3

 

7

a

19.5

73.1

0.0

0.6

93.2

b

14.2

80.4

0.0

0.8

95.5

mean

16.9

76.7

0.0

0.7

94.3

 

14

a

18.8

70.5

0.0

1.0

90.4

b

16.9

72.8

0.0

1.0

90.6

mean

17.8

71.7

0.0

1.0

90.5

 

35

a

9.2

82.0

0.1

1.8

93.1

b

11.8

78.4

0.1

1.8

92.1

mean

10.5

80.2

0.1

1.8

92.6

 

70

a

7.6

85.9

0.2

2.5

96.2

b

5.3

87.2

0.1

2.4

95.0

mean

6.5

86.5

0.2

2.4

95.6

 

100

a

8.5

80.6

0.3

3.0

92.4

b

6.9

82.1

0.5

3.0

92.6

mean

7.7

81.4

0.4

3.0

92.5

 

181

a

6.5

82.8

0.4

3.6

93.3

b

8.7

79.6

0.6

4.0

92.8

mean

7.6

81.2

0.5

3.8

93.1

n.p. not performed

 

Table 4. Distribution and Recovery of Radioactivity: Pond Aerobic Incubation

Incubation Time

Replicate / Mean

Aqueous Phase

Sediment Extracts

14CO2

Non- extractables

Recovery

days

 

% of applied radioactivity

 

0

a

90.9

2.0

n.p.

0.1

93.0

b

89.9

2.0

n.p.

0.1

92.0

mean

90.4

2.0

n.p.

0.1

92.5

 

1

a

52.2

38.5

0.0

0.4

91.0

 -

 -

 -

mean

52.2

38.5

0.0

0.4

91.0

 

3

a

35.1

54.6

0.0

0.4

90.1

b

34.0

57.0

0.0

0.5

91.6

mean

34.5

55.8

0.0

0.5

90.9

 

7

a

28.8

62.5

0.0

0.7

92.0

b

23.5

66.5

0.0

0.7

90.7

mean

26.2

64.5

0.0

0.7

91.4

 

14

a

17.2

72.1

0.0

1.2

90.6

b

17.7

71.4

0.0

1.1

90.2

mean

17.4

71.8

0.0

1.1

90.4

 

35

a

7.3

81.6

0.0

2.2

91.1

b

7.5

80.9

0.1

2.1

90.5

mean

7.4

81.2

0.0

2.1

90.8

 

70

a

7.5

82.8

0.6

2.8

93.7

b

7.8

81.0

0.8

3.4

93.0

mean

7.7

81.9

0.7

3.1

93.4

 

100

a

7.8

79.6

0.4

3.9

91.7

b

8.4

79.8

0.2

2.8

91.1

mean

8.1

79.7

0.3

3.4

91.5

 

181

a

8.9

78.1

0.6

3.9

91.5

b

8.7

76.9

0.7

4.1

90.6

mean

8.8

77.5

0.6

4.0

90.9

n.p.: not performed

 

Table 5. Distribution and Recovery of Radioactivity: River Anaerobic Incubation

Incubation Time

Replicate / Mean

Aqueous Phase

Sediment Extracts

14CO2

Non- extractables

Recovery

days

 

% of applied radioactivity

 

0

a

88.9

2.0

n.p.

0.2

91.1

b

91.6

2.0

n.p.

0.1

93.6

mean

90.2

2.0

n.p.

0.1

92.3

 

1

a

69.3

28.8

0.0

0.4

98.5

 -

 -

 -

 -

 -

 -

mean

69.3

28.8

0.0

0.4

98.5

 

3

a

59.9

31.8

0.0

0.2

91.9

b

59.1

32.0

0.0

0.2

91.3

mean

59.5

31.9

0.0

0.2

91.6

 

7

a

47.7

47.7

0.0

0.3

95.7

b

46.8

50.2

0.0

0.4

97.3

mean

47.2

48.9

0.0

0.3

96.5

 

14

a

25.0

64.4

0.0

0.7

90.1

b

30.8

59.6

0.0

0.6

91.0

mean

27.9

62.0

0.0

0.6

90.5

 

35

a

16.7

73.3

0.0

1.0

91.0

b

17.6

73.2

0.0

1.0

91.7

mean

17.1

73.2

0.0

1.0

91.3

 

70

a

11.6

81.8

0.0

1.2

94.6

b

13.0

80.0

0.0

0.9

93.9

mean

12.3

80.9

0.0

1.0

94.3

 

100

a

11.0

79.1

0.1

1.3

91.5

b

10.6

80.4

0.0

1.8

92.8

mean

10.8

79.8

0.0

1.6

92.1

 

181

a

8.7

82.5

0.1

1.7

92.9

b

8.2

81.1

0.1

1.9

91.3

mean

8.4

81.8

0.1

1.8

92.1

 

360

a

6.7

85.5

0.1

2.8

95.1

b

6.5

85.9

0.1

1.8

94.4

mean

6.6

85.7

0.1

2.3

94.7

n.p.: not performed

 

Table 6. Distribution and Recovery of Radioactivity: Pond Anaerobic Incubation

Incubation Time

Replicate / Mean

Aqueous Phase

Sediment Extracts

14CO2

Non- extractables

Recovery

days

 

% of applied radioactivity

 

0

a

89.6

2.0

n.p.

0.1

91.7

b

89.6

2.0

n.p.

0.1

91.6

mean

89.6

2.0

n.p.

0.1

91.7

 

1

a

67.4

28.8

0.0

0.3

96.5

 -

 -

 -

 -

 -

 -

mean

67.4

28.8

0.0

0.3

96.5

 

3

a

49.6

41.6

0.0

0.3

91.5

b

47.2

43.5

0.0

0.1

90.9

mean

48.4

42.6

0.0

0.2

91.2

 

7

a

38.9

54.6

0.0

0.5

94.0

b

41.2

53.3

0.0

0.4

94.9

mean

40.1

54.0

0.0

0.4

94.4

 

14

a

26.7

62.9

0.0

0.5

90.1

b

26.4

63.9

0.0

0.6

90.9

mean

26.5

63.4

0.0

0.6

90.5

 

35

a

15.1

74.0

0.0

1.0

90.2

b

18.2

71.1

0.0

0.9

90.2

mean

16.7

72.6

0.0

1.0

90.2

 

70

a

12.8

78.7

0.0

1.0

92.6

b

12.2

78.6

0.0

1.1

92.0

mean

12.5

78.7

0.0

1.1

92.3

 

100

a

10.6

80.6

0.0

1.3

92.6

b

10.4

79.8

0.1

1.2

91.5

mean

10.5

80.2

0.1

1.3

92.0

 

181

a

8.2

80.9

0.1

1.4

90.6

b

6.9

84.4

0.1

1.6

93.0

mean

7.5

82.6

0.1

1.5

91.8

 

360

a

6.3

84.0

0.1

1.6

92.0

b

6.7

85.4

0.1

1.7

93.8

mean

6.5

84.7

0.1

1.7

92.9

n.p.: not performed

 

Table 7. Distribution of 14C-test item and Metabolites in Aerobic Water/Sediment System at 20˚C (HPLC- Analysis) – River (% applied)

Incubation

Time

Compart-

ment

Repli

cate

Test item

Anti isomer

Syn isomer

U1

U2

U3

U4

U5

U6

U7

U8

U9

U10

U11

U12

U13

U14

U15

U16

Total

 

0

Water

A

88.61

6.75

81.86

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

88.61

Sediment

A

2.15

0.17

1.98

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

2.15

Total

A

90.76

6.92

83.84

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.76

Water

B

88.14

5.86

82.28

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

88.14

Sediment

B

2.14

0.15

1.99

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

2.14

Total

B

90.28

6.01

84.27

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.28

Water

mean

88.38

6.31

82.07

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

88.38

Sediment

mean

2.14

0.16

1.98

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

2.14

Total

mean

90.52

6.46

84.05

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.52

 

1

Water

A

47.71

3.75

43.96

1.66

1.43

0.40

<LD

0.89

<LD

<LD

1.21

<LD

<LD

<LD

<LD

0.76

<LD

<LD

<LD

54.06

Sediment

A

37.84

2.91

34.93

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

37.84

Total

A

85.55

6.66

78.89

1.66

1.43

0.40

<LD

0.89

<LD

<LD

1.21

<LD

<LD

<LD

<LD

0.76

<LD

<LD

<LD

91.90

 

3

Water

A

28.18

1.76

26.42

0.67

0.53

0.27

<LD

0.38

<LD

<LD

0.49

<LD

<LD

<LD

<LD

<LD

<LD

0.24

<LD

30.77

Sediment

A

60.15

5.20

54.95

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

60.15

Total

A

88.33

6.96

81.37

0.67

0.53

0.27

<LD

0.38

<LD

<LD

0.49

<LD

<LD

<LD

<LD

<LD

<LD

0.24

<LD

90.92

Water

B

29.10

2.16

26.94

0.96

0.50

0.18

<LD

0.25

<LD

0.13

0.46

<LD

<LD

<LD

<LD

0.34

0.20

<LD

<LD

32.14

Sediment

B

58.59

5.24

53.36

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

58.59

Total

B

87.70

7.40

80.30

0.96

0.50

0.18

<LD

0.25

<LD

0.13

0.46

<LD

<LD

<LD

<LD

0.34

0.20

<LD

<LD

90.73

Water

mean

28.64

1.96

26.68

0.82

0.52

0.23

<LD

0.32

<LD

0.07

0.47

<LD

<LD

<LD

<LD

0.17

0.10

0.12

<LD

31.45

Sediment

mean

59.37

5.22

54.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

59.37

Total

mean

88.02

7.18

80.83

0.82

0.52

0.23

<LD

0.32

<LD

0.07

0.47

<LD

<LD

<LD

<LD

0.17

0.10

0.12

<LD

90.83

 

7

Water

A

16.86

1.20

15.67

0.59

0.39

0.18

<LD

0.53

0.09

0.19

0.25

<LD

<LD

<LD

<LD

0.29

<LD

0.12

<LD

19.49

Sediment

A

73.06

5.93

67.13

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

73.06

Total

A

89.92

7.13

82.79

0.59

0.39

0.18

<LD

0.53

0.09

0.19

0.25

<LD

<LD

<LD

<LD

0.29

<LD

0.12

<LD

92.55

Water

B

11.77

0.68

11.09

0.45

0.54

0.20

<LD

0.50

<LD

0.19

0.18

<LD

0.07

<LD

<LD

0.34

<LD

<LD

<LD

14.24

Sediment

B

80.41

9.54

70.86

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

80.41

Total

B

92.18

10.23

81.95

0.45

0.54

0.20

<LD

0.50

<LD

0.19

0.18

<LD

0.07

<LD

<LD

0.34

<LD

<LD

<LD

94.65

Water

mean

14.32

0.94

13.38

0.52

0.47

0.19

<LD

0.52

0.04

0.19

0.21

<LD

0.04

<LD

<LD

0.31

<LD

0.06

<LD

16.87

Sediment

mean

76.73

7.74

68.99

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

76.73

Total

mean

91.05

8.68

82.37

0.52

0.47

0.19

<LD

0.52

0.04

0.19

0.21

<LD

0.04

<LD

<LD

0.31

<LD

0.06

<LD

93.60

 

14

Water

A

16.58

0.78

15.80

0.76

0.35

0.21

<LD

0.05

0.05

0.08

0.06

<LD

<LD

<LD

<LD

0.31

0.20

0.12

<LD

18.76

Sediment

A

68.61

5.83

62.79

0.47

0.61

0.37

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.47

<LD

<LD

<LD

70.53

Total

A

85.20

6.61

78.59

1.22

0.96

0.58

<LD

0.05

0.05

0.08

0.06

<LD

<LD

<LD

<LD

0.78

0.20

0.12

<LD

89.29

Water

B

14.50

1.05

13.45

0.77

0.34

0.13

<LD

0.41

0.07

0.22

0.07

<LD

<LD

<LD

<LD

0.16

0.11

0.09

<LD

16.86

Sediment

B

71.48

5.72

65.76

0.58

0.33

0.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.25

<LD

<LD

<LD

72.79

Total

B

85.98

6.77

78.24

1.34

0.67

0.28

<LD

0.41

0.07

0.22

0.07

<LD

<LD

<LD

<LD

0.41

0.11

0.09

<LD

89.65

Water

mean

15.54

0.91

14.63

0.76

0.34

0.17

<LD

0.23

0.06

0.15

0.06

<LD

<LD

<LD

<LD

0.24

0.16

0.10

<LD

17.81

Sediment

mean

70.05

5.77

64.27

0.52

0.47

0.26

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.36

<LD

<LD

<LD

71.66

Total

mean

85.59

6.69

78.90

1.28

0.81

0.43

<LD

0.23

0.06

0.15

0.06

<LD

<LD

<LD

<LD

0.60

0.16

0.10

<LD

89.47

 

35

Water

A

4.76

0.33

4.42

1.49

0.84

0.35

<LD

0.06

0.49

0.15

0.32

<LD

0.19

0.22

0.08

<LD

0.19

0.06

<LD

9.18

Sediment

A

79.23

5.19

74.04

1.04

0.67

1.07

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

82.02

Total

A

83.99

5.52

78.47

2.53

1.52

1.42

<LD

0.06

0.49

0.15

0.32

<LD

0.19

0.22

0.08

<LD

0.19

0.06

<LD

91.21

Water

B

8.50

0.53

7.97

0.74

0.52

0.17

<LD

0.02

0.15

0.15

0.73

<LD

0.19

0.20

0.04

0.24

0.19

<LD

<LD

11.85

Sediment

B

76.55

6.88

69.67

0.48

0.65

0.69

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

78.37

Total

B

85.05

7.41

77.64

1.22

1.17

0.86

<LD

0.02

0.15

0.15

0.73

<LD

<LD

0.19

0.20

0.04

0.24

0.19

<LD

90.22

Water

mean

6.63

0.43

6.20

1.11

0.68

0.26

<LD

0.04

0.32

0.15

0.52

<LD

0.19

0.21

0.06

0.12

0.19

0.03

<LD

10.52

Sediment

mean

77.89

6.04

71.86

0.76

0.66

0.88

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

80.20

Total

mean

84.52

6.47

78.05

1.87

1.34

1.14

<LD

0.04

0.32

0.15

0.52

<LD

0.19

0.21

0.06

0.12

0.19

0.03

<LD

90.71

 

70

Water

A*

3.06

0.20

2.87

1.69

0.82

0.46

0.02

0.52

0.12

0.27

<LD

<LD

<LD

0.22

0.09

0.12

0.09

0.08

<LD

7.61

Sediment

A

84.11

6.20

77.90

0.61

<LD

1.19

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

85.91

Total

A

87.17

6.40

80.77

2.30

0.82

1.65

0.02

0.52

0.12

0.27

<LD

<LD

<LD

0.22

0.09

0.12

0.09

0.08

<LD

93.52

Water

B*

1.69

0.08

1.61

0.99

0.49

0.26

<LD

0.71

0.08

0.31

<LD

<LD

<LD

0.22

0.07

0.20

0.03

0.10

0.04

5.34

Sediment

B

84.14

7.55

76.59

0.25

0.56

1.69

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.53

<LD

<LD

<LD

87.18

Total

B

85.83

7.63

78.20

1.23

1.05

1.95

<LD

0.71

0.08

0.31

<LD

<LD

<LD

0.22

0.07

0.72

0.03

0.10

0.04

90.11

Water

Mean

2.38

0.14

2.24

1.34

0.65

0.36

0.01

0.61

0.10

0.29

<LD

<LD

<LD

0.22

0.08

0.16

0.06

0.09

0.02

6.47

Sediment

mean

84.12

6.88

77.25

0.43

0.28

1.44

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.27

<LD

<LD

<LD

86.54

Total

mean

86.50

7.02

79.48

1.77

0.93

1.80

0.01

0.61

0.10

0.29

<LD

<LD

<LD

0.22

0.08

0.42

0.06

0.09

0.02

93.02

 

100

Water

A

3.53

0.15

3.38

1.85

0.89

0.63

<LD

0.16

0.41

0.15

0.33

<LD

<LD

0.07

0.14

0.15

0.15

<LD

<LD

8.46

Sediment

A

79.51

5.28

74.23

0.44

<LD

0.38

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.31

<LD

80.63

Total

A

83.04

5.43

77.61

2.28

0.89

1.00

<LD

0.16

0.41

0.15

0.33

>LD

<LD

0.07

0.14

0.15

0.15

0.31

<LD

89.09

Water

B

2.90

0.15

2.76

1.55

1.07

0.19

<LD

0.23

0.15

0.07

0.21

<LD

<LD

0.21

0.06

0.14

0.13

<LD

<LD

6.91

Sediment

B

79.27

7.40

71.87

0.40

<LD

2.00

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.43

<LD

82.09

Total

B

82.17

7.55

74.63

1.95

1.07

2.18

<LD

0.23

0.15

0.07

0.21

<LD

<LD

0.21

0.06

0.14

0.13

0.43

<LD

89.00

Water

mean

3.22

0.15

3.07

1.70

0.98

0.41

<LD

0.19

0.28

0.11

0.27

<LD

<LD

0.14

0.10

0.14

0.14

<LD

<LD

7.68

Sediment

mean

79.39

6.34

73.05

0.42

<LD

1.19

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.37

<LD

81.36

Total

mean

82.61

6.49

76.12

2.12

0.98

1.59

<LD

0.19

0.28

0.11

0.27

<LD

<LD

0.14

0.10

0.14

0.14

0.37

<LD

89.05

 

181

Water

A

1.43

0.05

1.38

1.76

0.99

0.58

<LD

0.65

0.02

<LD

0.06

<LD

0.04

0.31

0.22

0.31

0.08

<LD

<LD

6.47

Sediment

A

76.06

5.68

70.38

1.03

2.03

3.03

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.65

<LD

<LD

<LD

82.79

Total

A

77.49

5.73

71.76

2.78

3.02

3.61

<LD

0.65

0.02

<LD

0.06

<LD

0.04

0.31

0.22

0.96

0.08

<LD

<LD

89.26

Water

B

1.94

0.12

1.82

2.32

1.23

0.80

<LD

0.72

<LD

<LD

0.21

<LD

<LD

0.57

0.37

0.36

0.19

<LD

<LD

8.70

Sediment

B

70.59

6.21

64.38

1.64

2.33

3.12

<LD

<LD

<LD

<LD

0.38

<LD

<LD

<LD

0.41

1.12

<LD

<LD

<LD

79.60

Total

B

72.53

6.33

66.20

3.96

3.56

3.92

<LD

0.72

<LD

<LD

0.59

<LD

<LD

0.57

0.78

1.48

0.19

<LD

<LD

88.30

Water

mean

1.69

0.08

1.60

2.04

1.11

0.69

<LD

0.69

0.01

<LD

0.14

<LD

0.02

0.44

0.29

0.34

0.14

<LD

<LD

7.59

Sediment

mean

73.32

5.94

67.38

1.33

2.18

3.08

<LD

<LD

<LD

<LD

0.19

<LD

<LD

<LD

0.21

0.88

<LD

<LD

<LD

81.19

Total

mean

75.01

6.03

68.98

3.37

3.29

3.77

<LD

0.69

0.01

<LD

0.32

<LD

0.02

0.44

0.50

1.22

0.14

<LD

<LD

88.78

U1 and U2 cochromatographed with M4 and M1; Test item is the sum of Anti and Syn isomers; LD= 0.01-0.10 %

*) For the paddy water at 70 days two additional degradation products U17 and U18 were found accounting for 0.03%, 0.03% applied in replicate A and 0.05, 0.10 % in replicate B.

 

Table 8. Distribution of 14C-test item and Metabolites in Anaerobic Water/Sediment System at 20˚C (HPLC- Analysis) – River (% applied)

Incubation

Time

Compart-

ment

Repli

cate

Test item

Anti isomer

Syn isomer

U1

U2

U3

U4

U5

U6

U7

U8

U9

U10

U11

U12

U13

U14

U15

U16

Total

 

0

Water

A

88.86

6.09

82.77

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

88.86

Sediment

A

1.88

0.15

1.72

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.88

Total

A

90.73

6.24

84.49

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.73

Water

B

91.57

6.94

84.63

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.57

Sediment

B

1.80

0.16

1.64

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.80

Total

B

93.37

7.10

86.26

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

93.37

Water

mean

90.21

6.51

83.70

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.21

Sediment

mean

1.84

0.16

1.68

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.84

Total

mean

92.05

6.67

85.38

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

92.05

 

1

Water

A

67.65

5.12

62.53

<LD

<LD

<LD

<LD

0.66

<LD

<LD

1.01

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

69.32

Sediment

A

28.78

2.28

26.50

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

28.78

Total

A

96.43

7.40

89.02

<LD

<LD

<LD

<LD

0.66

<LD

<LD

1.01

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

98.10

 

3

Water

A

59.23

4.77

54.46

<LD

<LD

<LD

<LD

0.37

<LD

<LD

0.32

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

59.92

Sediment

A

31.78

2.63

29.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

31.78

Total

A

91.01

7.40

83.61

<LD

<LD

<LD

<LD

0.37

<LD

<LD

0.32

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.70

Water

B

58.26

4.74

53.53

<LD

<LD

<LD

<LD

0.34

<LD

<LD

0.53

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

59.13

Sediment

B

31.97

2.88

29.09

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

31.97

Total

B

90.23

7.61

82.62

<LD

<LD

<LD

<LD

0.34

<LD

<LD

0.53

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.09

Water

mean

58.75

4.75

53.99

<LD

<LD

<LD

<LD

0.35

<LD

<LD

0.42

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

59.52

Sediment

mean

31.87

2.76

29.12

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

31.87

Total

mean

90.62

7.51

83.11

<LD

<LD

<LD

<LD

0.35

<LD

<LD

0.42

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.40

 

7

Water

A

46.48

3.90

42.58

0.15

0.21

0.15

<LD

<LD

0.38

<LD

<LD

<LD

0.12

<LD

<LD

<LD

<LD

0.18

<LD

47.68

Sediment

A

47.68

4.62

43.05

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

47.68

Total

A

94.16

8.52

85.64

0.15

0.21

0.15

<LD

<LD

0.38

<LD

<LD

<LD

0.12

<LD

<LD

<LD

<LD

0.18

<LD

95.36

Water

B

46.32

3.73

42.60

<LD

<LD

<LD

<LD

0.39

<LD

<LD

<LD

<LD

0.09

<LD

<LD

<LD

<LD

<LD

<LD

46.80

Sediment

B

50.15

3.86

46.29

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

50.15

Total

B

96.47

7.59

88.89

<LD

<LD

<LD

<LD

0.39

<LD

<LD

<LD

<LD

0.09

<LD

<LD

<LD

<LD

<LD

<LD

96.95

Water

mean

46.40

3.81

42.59

0.08

0.11

0.08

<LD

0.19

0.19

<LD

<LD

<LD

0.10

<LD

<LD

<LD

<LD

0.09

<LD

47.24

Sediment

mean

48.92

4.24

44.67

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

48.92

Total

mean

95.32

8.06

87.26

0.08

0.11

0.08

<LD

0.19

0.19

<LD

<LD

<LD

0.10

<LD

<LD

<LD

<LD

0.09

<LD

96.15

 

14

Water

A

23.04

1.42

21.62

0.19

0.22

0.15

<LD

0.45

0.10

0.15

0.20

<LD

<LD

<LD

<LD

0.23

0.15

0.17

<LD

25.03

Sediment

A

64.37

5.85

58.52

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

64.37

Total

A

87.41

7.27

80.14

0.19

0.22

0.15

<LD

0.45

0.10

0.15

0.20

<LD

<LD

<LD

<LD

0.23

0.15

0.17

<LD

89.40

Water

B

29.36

2.03

27.33

0.13

0.18

0.11

<LD

0.47

0.08

0.11

0.16

<LD

0.04

<LD

<LD

<LD

<LD

0.19

<LD

30.82

Sediment

B

59.57

4.18

55.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

59.57

Total

B

88.93

6.21

82.72

0.13

0.18

0.11

<LD

0.47

0.08

0.11

0.16

<LD

0.04

<LD

<LD

<LD

<LD

0.19

<LD

90.38

Water

mean

26.20

1.73

24.47

0.16

0.20

0.13

<LD

0.46

0.09

0.13

0.18

<LD

0.02

<LD

<LD

0.11

0.08

0.18

<LD

27.93

Sediment

mean

61.97

5.01

56.95

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

61.97

Total

mean

88.17

6.74

81.43

0.16

0.20

0.13

<LD

0.46

0.09

0.13

0.18

<LD

0.02

<LD

<LD

0.11

0.08

0.18

<LD

89.89

 

35

Water

A

14.88

1.12

13.76

0.19

0.25

0.07

<LD

0.56

0.11

0.12

0.14

<LD

0.09

<LD

<LD

0.10

0.09

0.09

<LD

16.67

Sediment

A

73.27

5.50

67.78

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

73.27

Total

A

88.15

6.61

81.54

0.19

0.25

0.07

<LD

0.56

0.11

0.12

0.14

<LD

0.09

<LD

<LD

0.10

0.09

0.09

<LD

89.94

Water

B

16.15

1.13

15.02

0.09

0.10

0.05

<LD

0.05

0.56

0.15

0.09

<LD

0.09

<LD

<LD

0.10

0.05

0.09

<LD

17.59

Sediment

B

73.16

5.25

67.91

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

73.16

Total

B

89.31

6.38

82.93

0.09

0.10

0.05

<LD

0.05

0.56

0.15

0.09

<LD

0.09

<LD

<LD

0.10

0.05

0.09

<LD

90.75

Water

mean

15.51

1.12

14.39

0.14

0.17

0.06

<LD

0.30

0.33

0.14

0.12

<LD

0.09

<LD

<LD

0.10

0.07

0.09

<LD

17.13

Sediment

mean

73.22

5.37

67.84

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

73.22

Total

mean

88.73

6.50

82.23

0.14

0.17

0.06

<LD

0.30

0.33

0.14

0.12

<LD

0.09

<LD

<LD

0.10

0.07

0.09

<LD

90.34

 

70

Water

A

9.29

1.37

7.92

0.10

0.28

0.10

<LD

0.11

<LD

0.12

0.21

0.41

0.28

0.47

<LD

0.12

<LD

<LD

0.13

11.63

Sediment

A

74.01

6.46

67.55

0.83

1.52

0.40

<LD

<LD

<LD

0.45

0.88

0.97

1.04

<LD

<LD

0.59

<LD

1.10

<LD

81.80

Total

A

83.30

7.83

75.47

0.94

1.81

0.50

<LD

0.11

<LD

0.57

1.09

1.38

1.32

0.47

<LD

0.71

<LD

1.10

0.13

93.43

Water

B

11.51

1.37

10.14

<LD

<LD

<LD

<LD

<LD

0.68

0.29

0.22

<LD

<LD

0.28

<LD

<LD

<LD

<LD

<LD

12.98

Sediment

B

78.36

6.66

71.70

0.14

<LD

<LD

<LD

<LD

<LD

<LD

0.17

<LD

0.86

<LD

<LD

<LD

<LD

0.42

<LD

79.95

Total

B

89.87

8.03

81.84

0.14

<LD

<LD

<LD

<LD

0.68

0.29

0.39

<LD

0.86

0.28

<LD

<LD

<LD

0.42

<LD

92.93

Water

mean

10.40

1.37

9.03

0.05

0.14

0.05

<LD

0.06

0.34

0.20

0.21

0.21

0.14

0.38

<LD

0.06

<LD

<LD

0.06

12.30

Sediment

mean

76.19

6.56

69.62

0.49

0.76

0.20

<LD

<LD

<LD

0.22

0.52

0.49

0.95

<LD

<LD

0.29

<LD

0.76

<LD

80.88

Total

mean

86.58

7.93

78.65

0.54

0.90

0.25

<LD

0.06

0.34

0.43

0.74

0.69

1.09

0.38

<LD

0.36

<LD

0.76

0.06

93.18

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

100

Water

A

9.68

0.15

9.52

0.04

<LD

<LD

<LD

0.16

0.56

<LD

<LD

<LD

0.19

0.34

<LD

<LD

<LD

<LD

<LD

10.97

Sediment

A

79.14

7.01

72.13

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

79.14

Total

A

88.82

7.16

81.66

0.04

<LD

<LD

<LD

0.16

0.56

<LD

<LD

<LD

0.19

0.34

<LD

<LD

<LD

<LD

<LD

90.11

Water

B

8.65

0.63

8.02

0.22

0.16

<LD

<LD

0.81

0.12

<LD

0.07

<LD

0.15

0.15

0.04

0.13

<LD

0.10

<LD

10.60

Sediment

B

78.45

10.82

67.63

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.25

0.44

<LD

<LD

<LD

<LD

<LD

1.21

<LD

80.35

Total

B

87.10

11.44

75.65

0.22

0.16

<LD

<LD

0.81

0.12

<LD

0.32

0.44

0.15

0.15

0.04

0.13

<LD

1.31

<LD

90.96

Water

mean

9.16

0.39

8.77

0.13

0.08

<LD

<LD

0.48

0.34

<LD

0.04

<LD

0.17

0.25

0.02

0.07

<LD

0.05

<LD

10.78

Sediment

mean

78.80

8.91

69.88

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.12

0.22

<LD

<LD

<LD

<LD

<LD

0.61

<LD

79.75

Total

mean

87.96

9.30

78.65

0.13

0.08

<LD

<LD

0.48

0.34

<LD

0.16

0.22

0.17

0.25

0.02

0.07

<LD

0.66

<LD

90.53

 

181

Water

A

6.61

0.46

6.15

0.10

0.25

<LD

<LD

0.96

<LD

<LD

0.24

0.19

0.31

<LD

<LD

<LD

<LD

<LD

<LD

8.65

Sediment

A

79.89

7.09

72.80

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.30

<LD

<LD

<LD

<LD

2.28

<LD

82.46

Total

A

86.50

7.55

78.95

0.10

0.25

<LD

<LD

0.96

<LD

<LD

0.24

0.19

0.60

<LD

<LD

<LD

<LD

2.28

<LD

91.11

Water

B

5.86

0.42

5.44

0.36

0.21

0.07

<LD

0.77

<LD

<LD

0.19

0.34

0.20

0.07

0.11

<LD

<LD

<LD

<LD

8.19

Sediment

B

79.94

6.38

73.56

<LD

<LD

0.41

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.74

<LD

81.09

Total

B

85.80

6.80

79.00

0.36

0.21

0.47

<LD

0.77

<LD

<LD

0.19

0.34

0.20

0.07

0.11

<LD

<LD

0.74

<LD

89.28

Water

mean

6.24

0.44

5.80

0.23

0.23

0.03

<LD

0.87

<LD

<LD

0.22

0.26

0.25

0.04

0.05

<LD

<LD

<LD

<LD

8.42

Sediment

mean

79.92

6.74

73.18

<LD

<LD

0.20

<LD

<LD

<LD

<LD

<LD

<LD

0.15

<LD

<LD

<LD

<LD

1.51

<LD

81.77

Total

mean

86.15

7.17

78.98

0.23

0.23

0.23

<LD

0.87

<LD

<LD

0.22

0.26

0.40

0.04

0.05

<LD

<LD

1.51

<LD

90.19

 

360

Water

A

4.24

0.40

3.84

0.48

0.37

0.16

<LD

0.62

0.13

0.12

0.08

<LD

0.08

0.06

0.11

0.09

0.07

0.07

<LD

6.68

Sediment

A

82.37

6.71

75.66

<LD

1.71

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.38

<LD

<LD

<LD

<LD

1.00

<LD

85.45

Total

A

86.61

7.10

79.50

0.48

2.08

0.16

<LD

0.62

0.13

0.12

0.08

<LD

0.45

0.06

0.11

0.09

0.07

1.06

<LD

92.13

Water

B

4.10

0.30

3.80

0.48

0.32

0.15

<LD

0.61

0.19

0.11

0.08

<LD

0.10

0.13

0.07

0.06

0.09

0.03

<LD

6.51

Sediment

B

84.03

7.06

76.97

0.49

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.14

<LD

<LD

<LD

1.25

<LD

<LD

85.90

Total

B

88.13

7.36

80.77

0.97

0.32

0.15

<LD

0.61

0.19

0.11

0.08

<LD

0.24

0.13

0.07

0.06

1.33

0.03

<LD

92.42

Water

mean

4.17

0.35

3.82

0.48

0.35

0.15

<LD

0.61

0.16

0.12

0.08

<LD

0.09

0.09

0.09

0.08

0.08

0.05

<LD

6.60

Sediment

mean

83.20

6.89

76.31

0.24

0.85

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.26

<LD

<LD

<LD

0.62

0.50

<LD

85.68

U1 and U2 cochromatographed with M4 and M1; Test item is the sum of Anti and Syn isomers; LD= 0.01-0.10 %

 

Table 9. Distribution of 14C-test item and Metabolites in Aerobic Water/Sediment System at 20˚C (HPLC- Analysis) – Pond (% applied)

Incubation

Time

Compart-

ment

Repli

cate

Test item

Anti isomer

Syn isomer

U1

U2

U3

U4

U5

U6

U7

U8

U9

U10

U11

U12

U13

U14

U15

U16

Total

 

0

Water

A

90.91

5.96

84.95

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.91

Sediment

A

1.78

0.13

1.65

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.78

Total

A

92.69

6.09

86.60

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

92.69

Water

B

89.85

7.30

82.56

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

89.85

Sediment

B

1.83

0.14

1.69

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.83

Total

B

91.68

7.44

84.25

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.68

Water

mean

90.38

6.63

83.75

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.38

Sediment

mean

1.81

0.13

1.67

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.81

Total

mean

92.19

6.76

85.42

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

92.19

 

1

Water

A

51.15

3.45

47.70

<LD

<LD

<LD

<LD

0.41

<LD

<LD

0.63

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

52.20

Sediment

A

38.48

3.37

35.11

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

38.48

Total

A

89.63

6.82

82.81

<LD

<LD

<LD

<LD

0.41

<LD

<LD

0.63

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.67

 

3

Water

A

32.92

2.51

30.42

0.28

0.28

0.29

<LD

0.41

<LD

<LD

0.53

<LD

<LD

<LD

<LD

0.38

<LD

<LD

<LD

35.09

Sediment

A

54.60

5.10

49.49

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

54.60

Total

A

87.52

7.61

79.91

0.28

0.28

0.29

<LD

0.41

<LD

<LD

0.53

<LD

<LD

<LD

<LD

0.38

<LD

<LD

<LD

89.69

Water

B

29.07

2.01

27.06

0.47

0.50

0.34

<LD

0.75

<LD

0.11

0.87

<LD

<LD

<LD

<LD

1.01

0.53

0.36

<LD

34.01

Sediment

B

57.05

4.84

52.20

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

57.05

Total

B

86.12

6.85

79.27

0.47

0.50

0.34

<LD

0.75

<LD

0.11

0.87

<LD

<LD

<LD

<LD

1.01

0.53

0.36

<LD

91.05

Water

mean

31.00

2.26

28.74

0.37

0.39

0.31

<LD

0.58

<LD

0.05

0.70

<LD

<LD

<LD

<LD

0.69

0.27

0.18

<LD

34.55

Sediment

mean

55.82

4.97

50.85

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

55.82

Total

mean

86.82

7.23

79.59

0.37

0.39

0.31

<LD

0.58

<LD

0.05

0.70

<LD

<LD

<LD

<LD

0.69

0.27

0.18

<LD

90.37

 

7

Water

A

26.19

2.07

24.12

0.23

0.29

0.30

<LD

0.65

<LD

0.26

0.20

<LD

<LD

<LD

<LD

0.32

0.18

0.17

<LD

28.80

Sediment

A

62.47

5.61

56.86

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

62.47

Total

A

88.67

7.68

80.99

0.23

0.29

0.30

<LD

0.65

<LD

0.26

0.20

<LD

<LD

<LD

<LD

0.32

0.18

0.17

<LD

91.27

Water

B

18.75

1.51

17.24

0.91

0.92

0.52

<LD

1.16

0.23

0.38

<LD

<LD

0.10

0.55

<LD

<LD

<LD

<LD

<LD

23.52

Sediment

B

66.52

3.05

63.47

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

66.52

Total

B

85.27

4.55

80.71

0.91

0.92

0.52

<LD

1.16

0.23

0.38

<LD

<LD

0.10

0.55

<LD

<LD

<LD

<LD

<LD

90.04

Water

mean

22.47

1.79

20.68

0.57

0.61

0.41

<LD

0.91

0.12

0.32

0.10

<LD

0.05

0.27

<LD

0.16

0.09

0.08

<LD

26.16

Sediment

mean

64.50

4.33

60.17

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

64.50

Total

mean

86.97

6.12

80.85

0.57

0.61

0.41

<LD

0.91

0.12

0.32

0.10

<LD

0.05

0.27

<LD

0.16

0.09

0.08

<LD

90.65

 

14

Water

A

14.77

0.89

13.87

0.54

0.43

0.24

<LD

0.45

0.01

0.17

0.15

<LD

0.06

<LD

<LD

0.14

0.18

0.10

<LD

17.23

Sediment

A

67.98

6.04

61.94

0.61

0.58

0.44

<LD

<LD

<LD

<LD

0.25

0.40

0.47

<LD

<LD

0.24

0.72

0.43

<LD

72.11

Total

A

82.75

6.93

75.82

1.15

1.01

0.68

<LD

0.45

0.01

0.17

0.40

0.40

0.53

<LD

<LD

0.38

0.90

0.53

<LD

89.35

Water

B

14.49

0.76

13.73

0.67

0.54

0.33

<LD

0.01

0.46

0.43

0.14

<LD

0.12

<LD

<LD

0.22

0.11

0.13

<LD

17.66

Sediment

B

68.49

6.29

62.20

0.49

0.69

0.56

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.56

0.32

0.32

<LD

71.44

Total

B

82.98

7.05

75.94

1.15

1.23

0.89

<LD

0.01

0.46

0.43

0.14

<LD

0.12

<LD

<LD

0.78

0.43

0.46

<LD

89.10

Water

mean

14.63

0.83

13.80

0.61

0.48

0.28

<LD

0.23

0.23

0.30

0.14

<LD

0.09

<LD

<LD

0.18

0.15

0.12

<LD

17.45

Sediment

mean

68.23

6.16

62.07

0.55

0.64

0.50

<LD

<LD

<LD

<LD

0.12

0.20

0.23

<LD

<LD

0.40

0.52

0.38

<LD

71.77

Total

mean

82.86

6.99

75.88

1.15

1.12

0.78

<LD

0.23

0.23

0.30

0.27

0.20

0.33

<LD

<LD

0.58

0.67

0.50

<LD

89.22

 

35

Water

A

3.65

0.23

3.43

0.95

0.49

0.42

<LD

0.31

0.52

0.22

0.12

<LD

0.21

0.21

0.07

0.06

0.10

0.03

<LD

7.35

Sediment

A

78.17

4.88

73.29

0.92

0.96

1.51

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

81.57

Total

A

81.83

5.11

76.72

1.87

1.45

1.90

<LD

0.31

0.52

0.22

0.12

<LD

0.21

0.21

0.07

0.06

0.10

0.03

<LD

88.91

Water

B

3.74

0.26

3.47

0.90

0.56

0.36

<LD

0.56

0.42

0.14

0.14

<LD

0.12

0.23

0.07

0.13

0.14

<LD

<LD

7.50

Sediment

B

78.13

6.75

71.38

0.86

0.95

0.95

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

80.89

Total

B

81.86

7.02

74.85

1.76

1.51

1.31

<LD

0.56

0.42

0.14

0.14

<LD

0.12

0.23

0.07

0.13

0.14

<LD

<LD

88.39

Water

mean

3.69

0.25

3.45

0.92

0.52

0.39

<LD

0.43

0.47

0.18

0.13

<LD

0.16

0.22

0.07

0.09

0.12

0.01

<LD

7.42

Sediment

mean

78.15

5.82

72.33

0.89

0.96

1.23

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

81.23

Total

mean

81.85

6.06

75.78

1.81

1.48

1.62

<LD

0.43

0.47

0.18

0.13

<LD

0.16

0.22

0.07

0.09

0.12

0.01

<LD

88.65

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

70

Water

A

2.25

0.16

2.09

1.36

0.99

0.53

<LD

0.06

0.66

0.16

0.46

<LD

0.19

0.34

0.21

0.13

0.09

0.07

0.06

7.54

Sediment

A

80.91

4.23

76.67

0.84

0.74

0.33

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

82.81

Total

A

83.15

4.39

78.76

2.20

1.73

0.87

<LD

0.06

0.66

0.16

0.46

<LD

0.19

0.34

0.21

0.13

0.09

0.07

0.06

90.35

Water

B

1.88

0.10

1.78

0.98

0.92

0.98

0.09

0.90

<LD

0.29

0.48

<LD

0.13

0.42

0.34

0.17

0.06

0.11

0.07

7.84

Sediment

B

78.01

3.69

74.32

0.40

0.85

0.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.59

<LD

<LD

81.00

Total

B

79.89

3.78

76.10

1.38

1.77

1.13

0.09

0.90

<LD

0.29

0.48

<LD

0.13

0.42

0.34

0.17

1.65

0.11

0.07

88.83

Water

mean

2.06

0.13

1.93

1.17

0.96

0.76

0.05

0.48

0.33

0.22

0.47

<LD

0.16

0.38

0.28

0.15

0.07

0.09

0.06

7.69

Sediment

mean

79.46

3.96

75.50

0.62

0.79

0.24

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.79

<LD

<LD

81.90

Total

mean

81.52

4.09

77.43

1.79

1.75

1.00

0.05

0.48

0.33

0.22

0.47

<LD

0.16

0.38

0.28

0.15

0.87

0.09

0.06

89.59

 

100

Water

A

1.77

0.13

1.63

1.35

0.87

0.42

0.02

0.82

0.73

0.14

0.28

<LD

0.18

0.60

0.12

0.22

0.15

0.12

<LD

7.79

Sediment

A

77.57

6.20

71.37

0.24

0.67

0.81

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.29

<LD

79.59

Total

A

79.34

6.33

73.01

1.59

1.54

1.23

0.02

0.82

0.73

0.14

0.28

<LD

0.18

0.60

0.12

0.22

0.15

0.42

<LD

87.38

Water

B

2.17

0.16

2.01

1.91

1.00

0.64

<LD

0.20

0.20

0.15

0.73

0.13

0.28

0.37

0.13

0.22

0.15

0.07

<LD

8.36

Sediment

B

73.82

6.52

67.30

1.04

1.36

1.25

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.14

0.90

0.40

0.53

0.32

79.78

Total

B

76.00

6.68

69.31

2.95

2.35

1.90

0.00

0.20

0.20

0.15

0.73

0.13

0.28

0.37

0.28

1.12

0.55

0.60

0.32

88.13

Water

mean

1.97

0.15

1.82

1.63

0.93

0.53

0.01

0.51

0.47

0.14

0.51

0.07

0.23

0.48

0.13

0.22

0.15

0.10

<LD

8.08

Sediment

mean

75.70

6.36

69.34

0.64

1.01

1.03

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.07

0.45

0.20

0.41

0.16

79.68

Total

mean

77.67

6.51

71.16

2.27

1.95

1.56

0.01

0.51

0.47

0.14

0.51

0.07

0.23

0.48

0.20

0.67

0.35

0.51

0.16

87.76

 

181

Water

A

1.27

0.08

1.20

2.44

1.58

1.14

<LD

1.06

<LD

<LD

0.18

0.04

<LD

0.56

0.32

0.12

0.16

<LD

<LD

8.88

Sediment

A

67.94

6.03

61.91

1.89

3.54

2.92

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.83

<LD

<LD

<LD

78.13

Total

A

69.22

6.11

63.11

4.33

5.12

4.06

<LD

1.06

<LD

<LD

0.18

0.04

<LD

0.56

0.32

1.95

0.16

<LD

<LD

87.00

Water

B

1.05

0.06

0.99

2.27

1.43

1.39

<LD

1.08

<LD

<LD

0.13

<LD

<LD

0.45

0.35

0.31

0.20

<LD

<LD

8.67

Sediment

B

64.82

5.61

59.22

1.85

2.67

3.25

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.38

2.54

0.62

0.78

<LD

76.90

Total

B

65.87

5.67

60.21

4.12

4.10

4.64

<LD

1.08

<LD

<LD

0.13

<LD

<LD

0.45

0.73

2.85

0.82

0.78

<LD

85.57

Water

mean

1.16

0.07

1.09

2.36

1.51

1.27

<LD

1.07

<LD

<LD

0.15

0.02

<LD

0.50

0.34

0.22

0.18

<LD

<LD

8.77

Sediment

mean

66.38

5.82

60.56

1.87

3.10

3.09

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.19

2.18

0.31

0.39

<LD

77.51

Total

mean

67.55

5.89

61.66

4.22

4.61

4.35

<LD

1.07

<LD

<LD

0.15

0.02

<LD

0.50

0.53

2.40

0.49

0.39

<LD

86.28

U1 and U2 cochromatographed with M4 and M1; Test item is the sum of Anti and Syn isomers; LD= 0.01-0.10 %

 

Table 10. Distribution of 14C-test item and Metabolites in Anaerobic Water/Sediment System at 20˚C (HPLC- Analysis) – Pond (% applied)

Incubation

Time

Compart-

ment

Repli

cate

Test item

Anti isomer

Syn isomer

U1

U2

U3

U4

U5

U6

U7

U8

U9

U10

U11

U12

U13

U14

U15

U16

Total

 

0

Water

A

89.60

7.21

82.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

89.60

Sediment

A

1.82

0.14

1.68

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.82

Total

A

91.41

7.35

84.06

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.41

Water

B

89.56

7.65

81.92

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

89.56

Sediment

B

1.80

0.12

1.68

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.80

Total

B

91.37

7.77

83.60

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.37

Water

mean

89.58

7.43

82.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

89.58

Sediment

mean

1.81

0.13

1.68

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.81

Total

mean

91.39

7.56

83.83

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.39

 

1

Water

A

66.32

5.13

61.18

<LD

<LD

<LD

<LD

0.40

<LD

<LD

0.71

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

67.43

Sediment

A

28.75

2.02

26.73

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

28.75

Total

A

95.06

7.15

87.91

<LD

<LD

<LD

<LD

0.40

<LD

<LD

0.71

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

96.18

 

3

Water

A

48.80

3.71

45.09

<LD

<LD

<LD

<LD

0.34

<LD

<LD

0.45

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

49.59

Sediment

A

41.61

3.78

37.83

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

41.61

Total

A

90.41

7.49

82.92

<LD

<LD

<LD

<LD

0.34

<LD

<LD

0.45

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

91.20

Water

B

46.49

3.81

42.69

<LD

<LD

<LD

<LD

0.32

<LD

<LD

0.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

47.20

Sediment

B

43.52

3.57

39.95

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

43.52

Total

B

90.02

7.38

82.64

<LD

<LD

<LD

<LD

0.32

<LD

<LD

0.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.72

Water

mean

47.65

3.76

43.89

<LD

<LD

<LD

<LD

0.33

<LD

<LD

0.42

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

48.39

Sediment

mean

42.57

3.68

38.89

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

42.57

Total

mean

90.21

7.43

82.78

<LD

<LD

<LD

<LD

0.33

<LD

<LD

0.42

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

90.96

 

7

Water

A

37.34

2.58

34.76

<LD

0.33

0.26

<LD

0.76

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.17

<LD

38.87

Sediment

A

54.64

4.96

49.68

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

54.64

Total

A

91.99

7.54

84.44

<LD

0.33

0.26

<LD

0.76

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.17

<LD

93.52

Water

B

40.26

2.47

37.79

0.22

0.19

0.20

<LD

0.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.21

<LD

41.24

Sediment

B

53.26

5.34

47.92

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

53.26

Total

B

93.52

7.81

85.71

0.22

0.19

0.20

<LD

0.15

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.21

<LD

94.50

Water

mean

38.80

2.53

36.28

0.11

0.26

0.23

<LD

0.46

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.19

<LD

40.06

Sediment

mean

53.95

5.15

48.80

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

53.95

Total

mean

92.75

7.68

85.08

0.11

0.26

0.23

0.00

0.46

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.19

<LD

94.01

 

14

Water

A

24.95

1.95

23.00

0.13

0.26

0.20

<LD

0.50

<LD

<LD

0.40

<LD

<LD

<LD

<LD

<LD

<LD

0.22

<LD

26.65

Sediment

A

62.93

5.65

57.29

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

62.93

Total

A

87.88

7.59

80.29

0.13

0.26

0.20

<LD

0.50

<LD

<LD

0.40

<LD

<LD

<LD

<LD

<LD

<LD

0.22

<LD

89.59

Water

B

25.26

2.52

22.73

<LD

<LD

0.10

<LD

0.40

0.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.09

<LD

0.18

26.41

Sediment

B

63.87

3.13

60.74

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

63.87

Total

B

89.12

5.65

83.47

<LD

<LD

0.10

<LD

0.40

0.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.09

0.19

0.18

90.27

Water

mean

25.10

2.24

22.87

0.06

0.13

0.15

<LD

0.45

0.19

0.00

0.20

<LD

<LD

<LD

<LD

<LD

0.04

0.11

0.09

26.53

Sediment

mean

63.40

4.39

59.01

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.18

63.40

Total

mean

88.50

6.62

81.88

0.06

0.13

0.15

<LD

0.45

0.19

0.00

0.20

<LD

<LD

<LD

<LD

<LD

0.04

0.11

0.09

89.93

 

35

Water

A

13.79

1.00

12.79

0.15

0.09

0.02

<LD

0.56

<LD

<LD

0.02

<LD

0.06

0.23

<LD

0.09

0.06

0.06

<LD

15.14

Sediment

A

74.01

5.90

68.11

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

74.01

Total

A

87.80

6.90

80.90

0.15

0.09

0.02

<LD

0.56

<LD

<LD

0.02

<LD

0.06

0.23

<LD

0.09

0.06

0.06

<LD

89.15

Water

B

16.80

1.28

15.52

0.08

0.10

0.07

<LD

0.54

<LD

<LD

0.13

<LD

0.01

0.21

<LD

0.07

0.03

0.13

<LD

18.18

Sediment

B

71.14

6.25

64.90

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

71.14

Total

B

87.94

7.53

80.42

0.08

0.10

0.07

<LD

0.54

<LD

<LD

0.13

<LD

0.01

0.21

<LD

0.07

0.03

0.13

<LD

89.32

Water

mean

15.30

1.14

14.16

0.11

0.10

0.04

<LD

0.55

<LD

<LD

0.07

<LD

0.04

0.22

<LD

0.08

0.05

0.10

<LD

16.66

Sediment

mean

72.57

6.07

66.50

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

72.57

Total

mean

87.87

7.21

80.66

0.11

0.10

0.04

<LD

0.55

<LD

<LD

0.07

<LD

0.04

0.22

<LD

0.08

0.05

0.10

<LD

89.23

 

70

Water

A

12.37

0.73

11.64

0.04

0.02

0.02

<LD

0.24

0.08

<LD

<LD

<LD

0.04

<LD

<LD

0.03

<LD

<LD

<LD

12.85

Sediment

A

78.74

8.42

70.31

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

78.74

Total

A

91.11

9.16

81.95

0.04

0.02

0.02

<LD

0.24

0.08

<LD

<LD

<LD

0.04

<LD

<LD

0.03

<LD

<LD

<LD

91.58

Water

B

9.92

0.38

9.54

0.06

0.19

0.03

<LD

0.32

0.80

0.36

<LD

<LD

0.32

<LD

<LD

0.08

0.08

<LD

<LD

12.16

Sediment

B

78.65

7.38

71.27

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

78.65

Total

B

88.57

7.76

80.81

0.06

0.19

0.03

<LD

0.32

0.80

0.36

<LD

<LD

0.32

<LD

<LD

0.08

0.08

<LD

<LD

90.81

Water

mean

11.15

0.56

10.59

0.05

0.11

0.03

<LD

0.28

0.44

0.18

<LD

<LD

0.18

<LD

<LD

0.06

0.04

<LD

<LD

12.50

Sediment

mean

78.69

7.90

70.79

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

78.69

Total

mean

89.84

8.46

81.38

0.05

0.11

0.03

<LD

0.28

0.44

0.18

<LD

<LD

0.18

<LD

<LD

0.06

0.04

<LD

<LD

91.20

 

100

Water

A

8.09

0.95

7.13

0.03

0.04

0.12

<LD

0.15

0.05

0.19

0.70

0.68

0.53

<LD

<LD

<LD

<LD

<LD

<LD

10.58

Sediment

A

80.65

7.91

72.74

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

80.65

Total

A

88.74

8.87

79.87

0.03

0.04

0.12

<LD

0.15

0.05

0.19

0.70

0.68

0.53

<LD

<LD

<LD

<LD

<LD

<LD

91.22

Water

B

9.20

0.33

8.87

0.02

<LD

0.02

<LD

0.09

0.60

0.19

<LD

0.07

0.14

<LD

<LD

<LD

<LD

0.07

<LD

10.40

Sediment

B

79.19

5.83

73.35

0.23

<LD

0.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

79.81

Total

B

88.39

6.17

82.22

0.25

<LD

0.42

<LD

0.09

0.60

0.19

<LD

0.43

0.15

<LD

<LD

<LD

<LD

0.07

<LD

90.21

Water

mean

8.64

0.64

8.00

0.02

0.02

0.07

<LD

0.12

0.33

0.19

0.35

0.38

0.34

<LD

<LD

<LD

<LD

0.04

<LD

10.49

Sediment

mean

79.92

6.87

73.05

0.12

<LD

0.20

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

80.23

Total

mean

88.56

7.52

81.05

0.14

0.02

0.27

<LD

0.12

0.33

0.19

0.35

0.38

0.34

<LD

<LD

<LD

<LD

0.04

<LD

90.72

 

181

Water

A

5.62

0.44

5.18

0.29

0.20

0.04

<LD

0.03

<LD

<LD

0.24

1.09

0.43

<LD

<LD

0.08

<LD

0.14

<LD

8.16

Sediment

A

76.70

5.97

70.73

1.81

0.65

0.53

<LD

<LD

<LD

<LD

<LD

<LD

1.16

<LD

<LD

<LD

<LD

<LD

<LD

80.86

Total

A

82.32

6.40

75.92

2.11

0.84

0.58

<LD

0.03

<LD

<LD

0.24

1.09

1.59

<LD

<LD

0.08

<LD

0.14

<LD

89.02

Water

B

4.25

0.27

3.97

0.14

0.11

0.10

<LD

<LD

<LD

<LD

0.91

0.44

0.30

0.22

0.05

0.13

0.09

0.10

0.09

6.92

Sediment

B

79.47

5.89

73.58

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.98

<LD

<LD

1.80

<LD

0.56

0.61

84.41

Total

B

83.72

6.17

77.55

0.14

0.11

0.10

<LD

<LD

<LD

<LD

0.91

0.44

2.27

0.22

0.05

1.93

0.09

0.66

0.70

91.33

Water

mean

4.93

0.35

4.58

0.22

0.15

0.07

<LD

0.01

<LD

<LD

0.58

0.77

0.36

0.11

0.02

0.10

0.04

0.12

0.05

7.54

Sediment

mean

78.09

5.93

72.16

0.91

0.32

0.27

<LD

<LD

<LD

<LD

<LD

<LD

1.57

<LD

<LD

0.93

<LD

0.28

0.30

82.63

Total

mean

83.02

6.28

76.73

1.12

0.47

0.34

<LD

0.01

<LD

<LD

0.58

0.77

1.93

0.11

0.02

1.00

0.04

0.40

0.35

90.17

 

360

Water

A

1.83

0.12

1.71

0.31

0.15

0.20

<LD

0.07

0.18

<LD

1.84

0.47

0.70

0.21

0.09

0.14

0.06

<LD

<LD

6.24

Sediment

A

80.43

7.15

73.28

0.79

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.09

<LD

<LD

0.32

<LD

1.34

<LD

83.96

Total

A

82.26

7.26

75.00

1.10

0.15

0.20

<LD

0.07

0.18

<LD

1.84

0.47

1.79

0.21

0.09

0.45

0.06

1.34

<LD

90.51

Water

B

2.64

0.17

2.47

0.44

0.53

0.20

<LD

0.42

0.34

0.33

0.75

0.04

0.25

0.08

0.19

0.19

0.15

0.10

<LD

6.65

Sediment

B

82.67

7.63

75.04

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

0.92

<LD

<LD

1.01

<LD

0.78

<LD

85.38

Total

B

85.31

7.80

77.51

0.44

0.53

0.20

<LD

0.42

0.34

0.33

0.75

0.04

1.16

0.08

0.19

1.19

0.15

0.87

<LD

92.03

Water

mean

2.23

0.14

2.09

0.38

0.34

0.20

<LD

0.24

0.26

0.16

1.30

0.25

0.48

0.14

0.14

0.16

0.10

0.05

<LD

6.60

Sediment

mean

81.55

7.39

74.16

0.39

<LD

<LD

<LD

<LD

<LD

<LD

<LD

<LD

1.01

<LD

<LD

0.66

<LD

1.06

<LD

84.67

Total

mean

83.78

7.53

76.25

0.77

0.34

0.20

<LD

0.24

0.26

0.16

1.30

0.25

1.48

0.14

0.14

0.83

0.10

1.11

<LD

91.27

U1 and U2 cochromatographed with M4 and M1; Test item is the sum of Anti and Syn isomers; LD= 0.01-0.10 %

Validity criteria:
The total recoveries should be between 90% and 110% for radiolabelled substance
Observed value:
Procedural recoveries for the concentration of water column and sediment samples prior to HPLC were generally between 90 - 103%, which was considered acceptable.
Validity criteria fulfilled:
yes
Conclusions:
In a biodegradation study with fresh water-sediment systems, performed in accordance with OECD TG 308, EPA 162 - 3 and EPA162 - 4 guidelines, the test substance rapidly dissipated from the water to the sediment in both Rehin river and pond system under aerobic as well as anaerobic conditions. However, the test substance degraded very slowly in the sediment. The DT50 value in the total system for both Rhein river and pond (aerobic and anaerobic conditions) was determined to be >>1 year. In all tested systems and conditions, only two minor metabolites, M1 and M4, were found and identified.
Executive summary:

The degradation of [Pyrazole-14C]-labelled test item was investigated in two laboratory incubated water/sediment systems (Rhein river and pond) under aerobic and anaerobic conditions according to OECD TG 308, EPA 162 - 3 and EPA 162 - 4 guidelines. The study was in compliance with GLP criteria. The 14C-labelled test item was applied to the surface water in each vessel to give a nominal initial concentration of 0.04 μg/mL in the water phase, equivalent to a single surface over spray application of 250 g/ha, evenly distributed to a depth of 30 cm. The final ratio of sediment dry matter to water of 1:4 (river) to 1:6 (pond) (w/w), and maintained in a flow-through system at 20 ± 1 ºC in the dark for up to 181 days for the aerobic system and 360 days for the anaerobic system. The flow through gases for the systems was air for the aerobic systems and oxygen-free nitrogen for the anaerobic systems. The distribution of 14C-labelled test item and its metabolites were determined at a number of time points. The amount of produced CO2, radioactivity and the degraded metabolites were analysed using LSC, HPLC and MS.

The mean mass balance from all aerobic systems ranged from 90.4 to 95.6% of the applied radioactivity (AR). The mean mass balance from all anaerobic systems rangedfrom 90.2 to 95.5% AR. Under both aerobic and anaerobic conditions in both systems, the 14C-labelled test substance dissipated rapidly from the water phase to the sediment. However, the degradation of the test substance in the whole water/sediment systems was slow. At the end of the incubation, there were 24.99%, 32.45%, 12.63% and 16.22% AR of the 14C-labelled test substance was degraded in the aerobic river, aerobic pond, anaerobic river and anaerobic pond systems, respectively.Very low level of 14CO2 was produced during the incubation. The maximum level of 14CO2 (0.6% AR) was found in the aerobic pond system indicating that mineralisation is not a major route of test item degradation in soil. Two minor degradation products were identified as M4 and M1 reaching a maximum levels of 4.2 and 4.6% AR, respectively, in the aerobic pond system. In both anaerobic systems, they were below 1.2%. No other single metabolite was observed above 2.5% of the applied dose in water or 3.6 % in sediment.Based on these finding, the DT50 value in the total system for both Rhein river and pond (aerobic and anaerobic conditions) was determined to be >>1 year. The DT 50 values in the water compartment were calculated to be 2.0, 2.6, 8.8 and 7.1 days foraerobic river, aerobic pond, anaerobic river and anaerobic pond systems, respectively.

Description of key information

All available data was assessed. The standard guideline followed study representing the direct biodegradation in the water-sediment system was included as key study and its effect values were used as key values in a weight of evidence approach. The other study was included as supporting information.

Geomean DT50 value of the test substance in freshwater-sediment >> 1 year, OECD TG 308, EPA 162 -3, EPA 162 -4, Stoll & Nicollier 2008

Key value for chemical safety assessment

Whole System

Half-life in whole system:
1 yr
at the temperature of:
20 °C
Type of system:
fresh water and sediment

Additional information

Two GLP complied studies are available for this endpoint. The first study (Stoll & Nicollier 2008) is a laboratory study, which followed standard test guidelines (OECD TG 308, EPA 162 - 3 and EPA 162 - 4 guidelines). The study directly represents the biodegradation process of the test substance in the water-sediment system. Thus, it is selected as the key study and its effect values were used as key values in a weight of evidence approach. The Pyrazole-14C-labelled test item was investigated in two water/sediment systems (Rhein river and pond) under aerobic and anaerobic conditions. The test conditions and results were summarized in the Table below.

The second study used an outdoor freshwater-sediment microcosm with a representative community of macrophytes and macroinvertebrates (France & Kuet 2008). There was no standard guideline available for this type of study. But the study considered OECD TG 308, EPA 162 -3 and EPA 162 -4. This type of study is not designed to represent degradation process alone and thus cannot be considered to yield a degradation half-life that can be used for the CSA according to ECHA Guideline on Information requirements and chemical safety assessment, Chapter R.7b: Endpoint specific guidance. Therefore, this study is selected as supporting study. The system consisted of a 10 cm layer of sediment and a 30 cm layer of natural overlying water, matured for 13 weeks to develop a representative community of macrophytes and macroinvertebrates. The 14C-pyrazole labelled test substance and 14C-phenyl labelled test substance were applied separately to two separate systems at initial nominal aqueous phase concentrations of 15.9 μg/L and 14.2 μg/L, respectively (assuming even distribution throughout the water column). In addition, a control pond was included as well without test substance treatment. The ponds were left open to the ambient climatic conditions throughout the study duration (100 days). The 14C-labelled test substances rapidly dissipated from the water compartment. The DT50 values for the water column and the total system were determined to be 3.5 days and 21.2 days, respectively.

Table. DT50 values for the substance in freshwater-sediment system under aerobic standard test conditions (key study)

Compound

Test system

Test conditions

Compartment

DT50 [d] –

Kinetic model

Author / Year / Smartdoc No.

Pyrazole labelled test item

River – sediment: sandy loam, pH 7.3, 1.9% OC

Aerobic, 20°C, dark, 181 days

Water

2.0 d - SFO

Stoll & Nicollier, 2008

Pyrazole labelled test item

River – sediment: sandy loam, pH 7.3, 1.9% OC

Aerobic, 20°C, dark, 181 days

Total system

>>1 yr

Stoll & Nicollier, 2008

Pyrazole labelled test item

Pond – sediment: silt loam, pH 7.3, 4.9% OC

Aerobic, 20°C, dark, 181 days

Water

2.6 d - SFO

Stoll & Nicollier, 2008

Pyrazole labelled test item

Pond – sediment: silt loam, pH 7.3, 4.9% OC

Aerobic, 20°C, dark, 181 days

Total system

>>1 yr

Stoll & Nicollier, 2008

Pyrazole labelled test item

River – sediment: sandy loam, pH 7.3, 1.9% OC

Anaerobic, 20°C, dark, 360 days

Water

8.8 d - SFO

Stoll & Nicollier, 2008

Pyrazole labelled test item

River – sediment: sandy loam, pH 7.3, 1.9% OC

Anaerobic, 20°C, dark, 360 days

Total system

>>1 yr

Stoll & Nicollier, 2008

Pyrazole labelled test item

Pond – sediment: silt loam, pH 7.3, 4.9% OC

Anaerobic, 20°C, dark, 360 days

Water

7.1 d - SFO

Stoll & Nicollier, 2008

Pyrazole labelled test item

Pond – sediment: silt loam, pH 7.3, 4.9% OC

Anaerobic, 20°C, dark, 360 days

Total system

>>1 yr

Stoll & Nicollier, 2008

Geomean DT50 (days)

 

 

Total system

>>1 yr