Registration Dossier
Registration Dossier
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EC number: 632-619-2 | CAS number: 881685-58-1
Biodegradation in soil
Administrative data
Link to relevant study record(s)
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 24 Apr 2006 to 11 Dec 2007
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 307 (Aerobic and Anaerobic Transformation in Soil)
- Version / remarks:
- 24 April 2002
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- other: EPA 162-1, Aerobic Soil Metabolism Studies
- Version / remarks:
- 1982
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 006
- Soil no.:
- #1
- Soil type:
- loam
- % Clay:
- 22
- % Silt:
- 28
- % Sand:
- 50
- % Org. C:
- 2.55
- pH:
- 6
- CEC:
- 17.8 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 30.2
- Soil no.:
- #2
- Soil type:
- sandy loam
- % Clay:
- 8
- % Silt:
- 19
- % Sand:
- 73
- % Org. C:
- 1.57
- pH:
- 7.4
- CEC:
- 6.1 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 28.2
- Soil no.:
- #3
- Soil type:
- loam
- % Clay:
- 10
- % Silt:
- 46
- % Sand:
- 44
- % Org. C:
- 2.55
- pH:
- 7.3
- CEC:
- 10.5 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 38
- Soil no.:
- #4
- Soil type:
- silty clay
- % Clay:
- 41
- % Silt:
- 54
- % Sand:
- 5
- % Org. C:
- 1.39
- pH:
- 8.3
- CEC:
- 10.6 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 23.4
- Details on soil characteristics:
- Characteristics of the soil are provided in Table 1 in 'Any other information on materials and methods incl. tables'.
SOIL COLLECTION AND STORAGE
- Geographic location:
18 Acres: Jealott’s Hill Farm, Bracknell, Berkshire, UK
Pappelacker: Les Barges, Switzerland
Gartenacker: Les Barges, Switzerland
Marsillargues: Marsillargues Field Station, La Paluzette, 34490 Marsillargues, France
- Pesticide use history at the collection site: The soils used have received no pesticide treatment for at least 12 months.
- Collection procedures: The soils were sampled in the field after removal of turf, where present.
- Sampling depth (cm): The soil was sampled to a depth of 20 cm for 18 Acres soil and 15 cm for Pappelacker, Gartenacker and Marsillargues soils.
- Storage conditions: After sieving, the soil was placed in loosely tied plastic bags and stored in a controlled temperature room (ca. 20°C). The moisture adjusted soil was stored in plastic containers at 20 ± 2 ˚C in the dark prior to dispensing into glass pots.
- Soil preparation: The soils were partially dried where necessary and sieved (2 mm mesh). Prior to incubation under study conditions, the soil was adjusted to a moisture content equivalent to pF 2 by the addition of ultra-pure water.
- Soil transportation: Soils from outside the UK were transported unfrozen. - Soil No.:
- #1
- Duration:
- 120 d
- Soil No.:
- #2
- Duration:
- 120 d
- Soil No.:
- #3
- Duration:
- 365 d
- Soil No.:
- #4
- Duration:
- 120 d
- Soil No.:
- #1
- Initial conc.:
- 0.17 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #2
- Initial conc.:
- 0.17 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #3
- Initial conc.:
- 0.17 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #4
- Initial conc.:
- 0.17 mg/kg soil d.w.
- Based on:
- test mat.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 20 ± 2˚C
- Humidity:
- approximately pF2 (29.78%)
- Microbial biomass:
- 610.1 (start) to 309.5 (end) mg C/100 g
- Soil No.:
- #2
- Temp.:
- 20 ± 2˚C
- Humidity:
- approximately pF2 (29.93%)
- Microbial biomass:
- 533.4 (start) to 359.1 (end) mg C/100 g
- Soil No.:
- #3
- Temp.:
- 20 ± 2˚C
- Humidity:
- approximately pF2 (38.95%)
- Microbial biomass:
- 671.9 (start) to 380.7 (end) mg C/100 g
- Soil No.:
- #4
- Temp.:
- 20 ± 2˚C
- Humidity:
- approximately pF2 (22.71%)
- Microbial biomass:
- 482.4 (start) to 398.3 (end) mg C/100 g
- Details on experimental conditions:
- An overview of the study design is provided in Table 2 in 'Any other information on materials and methods incl. tables'.
EXPERIMENTAL DESIGN
- Soil preincubation conditions: The soil was pre-incubated in the soil pots under study conditions for either 12 days (18 Acres, Pappelacker and Gartenacker soils) or 19 days (Marsillargues soil) prior to treatment with the application solution. The moisture content of the soils was checked by weighing the pots at approximately fortnightly intervals. Any moisture losses were replaced on these occasions by the addition of ultra-pure water.
- Soil condition: Fresh soil
- Soil: 100 g (dry weight) per replicate
- No. of replication treatments: 2
- Test apparatus: Glass centrifuge tube. Moist air flow through system, connections made with glass and PVC tubing
- Details of traps for CO2 and organic volatile: Volatile products produced were trapped using a flow-through system. Air was pushed (using a vacuum pump) through a water trap, then through the incubation vessel and any volatiles were collected in an outlet 2M NaOH trap.
- Identity and concentration of co-solvent: Acetonitrile
Test material application
- Volume of test solution used/treatment: 136 µL
- Application method: 34 x 4 µL droplets by pipette
Experimental conditions
- Moisture maintenance method: The moisture content of the soil samples was checked by weighing the pots at regular intervals. Any moisture/weight losses were replaced by the addition of ultra pure water.
- Continuous darkness: Yes
SAMPLING DETAILS
- Sampling intervals: Aerobic, non-sterile, duplicate samples from each soil type as follows: 18 Acres, Pappelacker = 0, 7, 14, 29, 43, 61, 90 and 120 DAT, Gartenacker = 0, 7, 14, 29, 43, 61, 90, 120, 180, 279 and 369 DAT, Marsillargues = 0, 7, 14, 30, 44, 58, 90 and 120 DAT. Untreated soils for biomass, prior to application for each soil type and at: 169 DAT for 18 Acres and Pappelacker soils, 134, 183 and 369 DAT for Gartenacker soil, 128 DAT for Marsillargues soil.
- Sampling method for soil samples: Complete treated samples were removed at each sampling time and extracted.
- Method of collection of CO2 and volatile organic compounds: The volume in each 2 M NaOH trap was recorded and triplicate aliquots taken for LSC quantification.
- Sample storage before analysis: All samples were extracted in the day of analysis (with the exception of the ‘spare’ Gartenacker samples used for further investigation at the end of the incubation period). - Soil No.:
- #1
- % Total extractable:
- 91.4
- % Non extractable:
- 2.5
- % CO2:
- 0.2
- % Recovery:
- 94.2
- Remarks on result:
- other: Mean value of duplicate samples; 120 DAT
- Soil No.:
- #2
- % Total extractable:
- 92
- % Non extractable:
- 5.2
- % CO2:
- 0.7
- % Recovery:
- 97.9
- Remarks on result:
- other: Mean value of duplicate samples; 120 DAT
- Soil No.:
- #3
- % Total extractable:
- 52.7
- % Non extractable:
- 29.6
- % CO2:
- 2.3
- % Recovery:
- 84.6
- Remarks on result:
- other: Mean value of duplicate samples; 369 DAT
- Soil No.:
- #4
- % Total extractable:
- 90.4
- % Non extractable:
- 3.3
- % CO2:
- 0.3
- % Recovery:
- 94
- Remarks on result:
- other: Mean value of duplicate samples; 120 DAT
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 16.9
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 23.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 82.9
- Parameter:
- radiochem. meas.
- Sampling time:
- 369 d
- Parent/product:
- parent
- Soil No.:
- #4
- % Degr.:
- 36.2
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Key result
- Soil No.:
- #1
- DT50:
- 592 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #2
- DT50:
- 349 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 121 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #4
- DT50:
- 231 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Transformation products:
- not specified
- Remarks:
- M1, M2 and M3
- Details on transformation products:
- An overview of the results is provided in Table 8 - Table 11 in 'Any other information on results incl. tables'.
Only one metabolite peak was observed at levels of > 5% of the applied radioactivity during the time course of the experiment in the Pappelacker, Gartenacker and Marsillargues soil extracts. This peak was assigned to M1 and M2 by co-chromatography with authenticated reference compounds. Using HPLC method 1, maximum levels of 9.7% and 18.0% of applied were observed in Pappelacker and Marsillargues soil samples respectively at 120 DAT. A maximum level of 20.0% of applied was observed in Gartenacker soil samples at 180 DAT and thereafter declined to 15.8% (average of replicates) by 369 DAT. In 18 Acres soil, the peak corresponding to M1 and M2 reached a maximum level of 4.3% of applied at 120 DAT. Further separation of the metabolite components using HPLC method 2 did not significant effect the amount of M1 and M2 observed since relatively good agreement (within 2.8%) in the amount of these metabolites was obtained for both HPLC methods 1 and 2. Numerous minor metabolite peaks were detected in all four soils, each of which individually comprised < 5% of the applied radioactivity.
- Analysis of the 120 DAT soil extracts: The 120 DAT concentrated extract 1 and extract 2 samples from 18 Acres, Pappelacker, Gartenacker and Marsillargues soils were analysed by 2D-TLC. With the exception of parent, only one component was again observed at levels of > 5% of applied upon TLC analysis of the 120 DAT Pappelacker, Gartenacker and Marsillargues soil extracts. This component was identified as M1 by co-chromatography. In 18 Acres soil, the region corresponding to the M1 metabolite comprised only 2.5% of the applied radioactivity at 120 DAT. The M2 was present at only very low levels in the 18 Acres and Pappelacker soil extracts (0.3% and 0.1% of applied respectively). This metabolite M2 was not observed in either the Gartenacker or Marsillargues 120 DAT soil extracts. Numerous minor metabolite regions were observed in all four soils, each of which individually comprised <5% of the applied radioactivity. These included small amounts (0.1 – 1.2% of applied) of the M13 and M16 which was observed in all four soils. A comparison of the TLC and HPLC analysis of Parent, M1 and M2, reasonable agreement was achieved between the amount of parent material and the sum of M1 and M2 in the 2D-TLC analysis and the HPLC analyses using methods 1 and 2.
- LC-MS-MS confirmation: Identification of the components present within each sample was undertaken by matching the retention times of the radioactive peaks, total ion chromatogram and extracted ion chromatograms of the components in the experimental samples with the authenticated reference compounds. The MS fragmentation patterns of the experimental sample components were also compared with those of the authenticated standard reference compounds to ensure that the same fragmentation pattern was obtained. Syn- and anti- isomers of the test substance were detected in all the samples analysed with the exception of the 180 DAT concentrated extract 1 sample from Gartenacker soil where no anti- isomer was observed. The only metabolite that exceeded > 5% of applied in Pappelacker, Gartenacker and Marsillargues soils was confirmed as the syn isomer of the hydroxylated metabolite M1. This metabolite (M1) was also found to be present in 18 Acres soil. The anti isomer of the hydroxylated metabolite (M2) was observed in the 120 DAT 18 Acres, Pappelacker, Gartenacker and Marsillargues soil extracts but was absent in the 180 DAT Gartenacker extracts.
- LC-MS-MS analysis of 12C-labelled M3 in soil extracts: Cleavage of the parent molecule into the N-demethylated pyrazole acid M3 has been observed in other 14C-pyrazole labelled test item studies and hence attempts were made to determine if this metabolite was also present in soil extracts from this study. A linear relationship was observed between the concentration of M3 and the LC-MS-MS response. No M3 was detected in any of the 18 Acres soil extracts indicating that the compound was either not formed during the time course of the experiment or was present at levels below the limit of detection. M3 was detected in Pappelacker, Gartenacker and Marsillargues soil extracts. However, repeat analysis of Gartenacker soil extracts demonstrated that the quantification of M3 in these extracts under the conditions used was unreliable since high coefficients of variation (>10%) were obtained. This was believed to be possibly due to:
(a) The low levels of M3 present in the samples analysed. The small peak size relative to the background noise resulted in high variability in the quantification of M3.
(b) The presence of acetonitrile in the sample. Higher levels of organic solvents in the sample composition have been shown to deteriorate the chromatography.
Although it was not possible to confidently determine the exact levels of M3 in the Pappelacker, Gartenacker and Marsillargues soil extracts, levels of up to approximately 5-10% of applied were observed in some Gartenacker soil extracts from later sampling times. - 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 11 in 'Any other information on results incl. tables'.
- Microbial biomass: The results for the soil microbial biomass analysis undertaken prior to application and after incubation in the test system for 169 DAT for 18 Acres and Pappelacker soils, 128 DAT for Marsillargues soil and 134 DAT, 183 DAT and 369 DAT for Gartenacker soil. The quantity of microbial biomass carbon constituted a minimum of 2.39% and a maximum of 3.68% of the soil organic carbon in the 18 Acres, Pappelacker, Marsillargues and Gartenacker soils prior to treatment. This indicated the soils supported a viable microbial population and that these soils were suitable for use in a laboratory degradation study. The quantity of microbial biomass carbon measured at the end of the incubation period constituted a minimum of 1.44% of the soil organic carbon and a maximum of 2.99% for the four soils. This indicated the soils supported a viable microbial population throughout the incubation period.
- Mass balance: The total radioactivity recovered was calculated by the summation of activity in the soil extracts, soil residue on combustion and 2 M sodium hydroxide traps. The total recoveries of radioactivity for the 0 - 120 DAT 18 Acres, Pappelacker, Gartenacker and Marsillargues soil samples were between 89.2 and 100.1% of applied. The total recoveries of radioactivity for the 180-369 DAT Gartenacker soil samples were between 84.2% and 92.6% of applied. Due to the slightly low mass balance values (approximately 85% of applied) obtained for the 279 and 369 DAT Gartenacker samples, further work was undertaken to determine if any loss of radioactivity was incurred during extraction or as a result of inefficient combustion of soil residues containing high levels of radioactivity. However, no additional radioactivity was recovered upon extraction and combustion of reserve soil samples incubated for 369 DAT.
- Volatile degradation products: Only small amounts of the applied radioactivity were evolved as a volatile product(s) and trapped in sodium hydroxide. The maximum amounts of radioactivity present in the NaOH trap at any time point were 0.2% (18 Acres), 0.7% (Pappelacker), 2.6% (Gartenacker) and 0.3% (Marsillargues) of the applied radioactivity. Due to the low levels of radioactivity present in the NaOH traps, no further work was undertaken to characterise the nature of the volatile products.
- Radioactive residues in soil extracts: The amount of extractable radioactivity in 18 Acres, Pappelacker and Marsillargues soils was found to decrease only slightly with time. It ranged from 92.3 – 96.8 % at 0 DAT to 90.1 - 93.4% by 120 DAT. There was a greater decrease in the amount of extractable radioactivity in Gartenacker soil from 96.7 % at 0 DAT to 80.1-80.2% by 120 DAT and 52.5 – 52.9% by 369 DAT. The high level of extractable recoveries at zerotime indicated that the extraction method was efficient for test item. The decline in extractable radioactivity with time (despite acidic extractions using ASE) suggested that the remaining radioactivity was bound or incorporated into the soil matrix. Further characterisation of the unextracted soil residue was carried out on a single 279 DAT Gartenacker soil sample. An extraction was undertaken which separated the natural organic matter present in soil into three fractions: fulvic acids (soluble in both acid and alkali), humic acids (soluble in alkali but insoluble in acid) and humin (insoluble in both acid and alkali). A further 9.2% of the applied radioactivity was recovered in the alkali soluble fraction (humic and fulvic acids). On acidification, only 2.3% of the applied radioactivity remained in solution (fulvic fraction) whilst the remaining 6.9% precipitated out with the humic acid fraction. Total extractable residue (% of applied amount) at day 0 for soils 18 Acres, Pappelacker, Gartenacker and Marsillargues soils were 94.6, 96.8, 96.7 and 93 % respectively. Total extractable residue (% of applied amount) at end of study period for soils 18 Acres, Pappelacker, Gartenacker and Marsillargues soils were 91.4 (120 DAT), 92.0 (120 DAT), 52.7 (369 DAT) and 90.4% (120 DAT) respectively.
NON-EXTRACTABLE RESIDUES
Low levels of bound residues were observed in the 18 Acres, Pappelacker and Marsillargues soils. Bound residues increased throughout the incubation period in Gartenacker soil. Total non-Extractable residue (% of applied amount) at day 0 for soils 18 Acres, Pappelacker, Gartenacker and Marsillargues soils were 0.3, 0.1, 0.1 and 0.4 respectively. Total non-Extractable residue (% of applied amount) at end of study period for soils 18 Acres, Pappelacker, Gartenacker and Marsillargues soils were 2.6 (120 DAT), 5.2 (120 DAT), 29.7 (369 DAT) and 3.3% (120 DAT) respectively.
TEST CONDITIONS:
- Aerobicity (or anaerobicity), moisture, temperature and other experimental conditions maintained throughout the study: Yes
- Conclusions:
- In a biodegradation study in soil, performed in accordance with OECD TG 307 and EPA guideline 161-1, under aerobic condition, the calculated DT50 values were 592, 349, 121 and 231 days for 14C-phenyl labelled test item in 18 Acres, Pappelacker, Gartenacker and Marsillargues soils, respectively.
- Executive summary:
The biodegradation of the14C-phenyl labelled test item was investigated according to OECD TG 307 and EPA 162 -1 guideline in the 18 Acres (loam), Pappelacker (sandy loam), Gartenacker (loam) and Marsillargues (silty clay) soils. The study was in compliance with GLP criteria. The 14C-labelled test item wasapplied at a rate of 0.17 mg/kg dry weight of soil (equivalent to a single field application rate of 125 g/ha, incorporated into the soil to a depth of 5 cm and assuming a soil bulk density of 1.5 g/cm3).The soils were incubated under aerobic conditions in the laboratory and maintained at a soil moisture content of approximately pF 2 in the darkness at 20 ± 2 °C for 120 days (18 Acres, Pappelacker and Marsillargues soils) or 369 days (Gartenackersoil). Duplicate samples were taken for analysis for each soil at approximately 0, 7, 14, 30, 60, 90, 120 days after treatment (DAT). Additional Gartenacker soil samples were taken at 180, 279 and 369 DAT. 14CO2 was collected in aqueous NaOH traps over the course of the study. Soil extracts were quantified by LSC. Qualitative analysis and metabolite identification were performed by using HPLC or TLC followed by mass spectrometry.
The total recoveries of radioactivity for the 0 - 120 DAT 18 Acres, Pappelacker, Gartenacker and Marsillargues soil samples were between 89.2 and 100.1% of applied. The total recoveries of radioactivity for the 180 - 369 DAT Gartenacker soil samples were between 84.2% and 92.6% of applied. The amount of parent material extracted from the soil decreased over time. At the end of incubation, for the parent material, 83.1%, 76.3%, 17.2% and 63.9% of applied radioactivity (AR) was found in the 18 Acres, Pappelacker, Gartenacker and Marsillargues soils, respectively. Only one metabolite (M1) presented > 5% AR in the Pappelacker, Gartenacker and Marsillargues soil extracts, with maximum levels reaching 9.7%, 20.0% and 18.0% AR, respectively. In 18 Acres soil extracts, the same metabolite reached levels of 4.1 - 4.3% AR. The anti-isomer of the hydroxylated metabolite (M2) presented ≤ 0.3% AR in the 120 DAT 18 Acres and Pappelacker soil extracts. M2 was observed in the LC-MS-MS analysis undertaken on the 120 DAT Gartenacker and Marsillargues soil extracts but was not detected during the TLC analysis of these extracts. Numerous minor metabolite components were observed in all four soils, each of which individually comprised < 5% AR. Only small amounts (≤ 2.6% AR) were evolved as volatile products and trapped in sodium hydroxide. Cleavage of the parent molecule into M3 was observed in Pappelacker, Gartenacker and Marsillargues soil extracts. The exact levels could not be determined due to the poor chromatography obtained, which resulted in inconsistencies in the quantification. However, levels of approximately 5 - 10% AR were estimated to be present in some Gartenacker soil extracts at later sampling times. Based on these findings, the DT50 values were determined to be 592, 349, 121 and 231 days, respectively.
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 11 May 2007 to 24 Jun 2008
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 307 (Aerobic and Anaerobic Transformation in Soil)
- Version / remarks:
- 24 April 2002
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- other: EPA 162-1
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 007
- Soil no.:
- #1
- Soil type:
- loam
- % Clay:
- 12
- % Silt:
- 43
- % Sand:
- 45
- % Org. C:
- 2.5
- pH:
- 6.7
- CEC:
- 10.8 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 30.39
- Details on soil characteristics:
- Collecting location and characteristics of the soil are provided in Table 1 in 'Any other information on materials and methods incl. tables'.
SOIL COLLECTION AND STORAGE
- Geographic location: Syngenta Crop Protection AG, Les Barges, Switzerland
- Collection procedures: Soil was sampled from Gartenacker field (field not planted and covered with meadow)
- Sampling depth: 2 - 15 cm
- Storage conditions: at ca 4°C until use.
- Storage length: 36 days (between soil collection and application of test item)
- Soil preparation: 2 mm sieved - Soil No.:
- #1
- Duration:
- 360 d
- Soil No.:
- #1
- Initial conc.:
- 0.168 mg/kg soil d.w.
- Based on:
- act. ingr.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 20 ± 2˚C
- Humidity:
- pF2
- Microbial biomass:
- 2.04 (initiation), 0.93 (120 DAT), 0.82 (termination)
- Details on experimental conditions:
- An overview of the study design is provided in Table 2 in 'Any other information on materials and methods incl. tables'.
EXPERIMENTAL DESIGN
- Soil preincubation conditions: A bulk soil sample was adjusted to pF2 soil moisture and pre-incubated at 20 ± 2°C for seven days in a large clean bucket.
- Soil condition: Fresh
- Soil (g/replicate): 100 (oven dry weight)
- No. of replication/sampling interval: 2
- Test apparatus: 250 mL glass Erlenmeyer flasks. The metabolism apparatus consisted of glass flasks (250 mL) and tubes with ground glass joints. Glassware was connected using a combination of glass connectors and PVC tubing.
- Details of traps for CO2 and organic volatile: The test vessels were incorporated into the air flow-through systems. The gas mixture leaving each soil flask was drawn through a series of two traps. The first acted as a safety trap and the second containing 2M sodium hydroxide to collect 14CO2.
- Identity and concentration of co-solvent: Acetonitrile: water (1:1 v/v)
Test material application
- Volume of test solution used/treatment: 5189 μL
- Application method: A badger 200G airbrush was used to spray the soil. The airbrush was connected to a supply of compressed air (high purity) via a regulator set to ca 18 psi and a flow meter with an internal needle valve to allow fine adjustment of the air flow. The flow from the air brush was ca 950 mL/min.
Experimental conditions
- Moisture maintenance method: The test vessels were weighed regularly (every 1 - 2 weeks) during the experimental period except for two occasions where the moisture was checked at 3 and 4 weeks, respectively. No significant moisture loss was noted on these occasions or any other occasion. Any weight loss relative to the initial sample weight was attributed to soil moisture loss and water added to restore the vessel weight.
- Continuous darkness: Yes
SAMPLING DETAILS
- Sampling intervals: Duplicate samples were taken for analysis immediately after test substance application (zero time) and after the following periods of incubation under aerobic conditions: 7, 14, 30, 45, 60, 90, 120, 150, 180, 210 and 360 Days. No trapping media were associated with the zero-time samples. The contents of the appropriate traps were sampled and replenished at 7, 14, 30, 45, 60, 90, 120, 150, 180, 210, 240, 316 and 360 Days.
- Sample storage before analysis: Sample analysis began immediately after removal of the vessel from the flow-through system. All samples generated throughout the course of the study were stored at ca -20 ˚C, except trapping solutions, which were stored under ambient laboratory conditions. Except for Day 210 solvent extracts, analysed 37 days post sampling, the soil extracts were analysed within 30 days of their respective sampling interval. - Soil No.:
- #1
- % Total extractable:
- 29.39
- % Non extractable:
- 58.27
- % CO2:
- 22.66
- % Recovery:
- 100
- Remarks on result:
- other: 360 DAT
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 97.39
- Parameter:
- radiochem. meas.
- Sampling time:
- 360 d
- Key result
- Soil No.:
- #1
- DT50:
- 39.8 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Recalculated outside of the original study (Hayes 2009)
- Soil No.:
- #1
- DT50:
- 40 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Reported in original study
- Transformation products:
- not specified
- Remarks:
- M1, M3
- Details on transformation products:
- - Distribution and composition of residues: All reported values are means of two replicates and four HPLC injections (two injections per replicate) unless otherwise stated. HPLC analysis of soil extracts (CaCl2 and solvent extract pools) demonstrated that [14C]-labelled test item degraded readily in the loam soil tested. [14C]-labelled test item decreased from 93.43% AR at zero time to 2.61% AR at 360 days. Two major (> 5% AR) degradation products were detected in soil extracts over the course of the study. The two peaks at ca 8.3 min and ca 26.3 min were identified as M3 and M1, respectively. M3, predominantly found in the CaCl2 pool extracts, reached a maximum value of 11.50% AR at Day 150 then declined to 5.38% at Day 360. M1, predominantly found in the solvent extract pools, reached a maximum of 22.31% AR at Day 45 and declined to 2.16% at Day 360. A maximum of 33 minor unidentified transformation products were detected at any one time point. No individual unidentified component accounted for greater than 4.75% AR except for one unknown degradation product. This degradation product eluted at ca 18.3 min in the HPLC method and reached a maximum of 5.39% AR (CaCl2 and solvent extracts combined) at Day 90 before declining to 2.08% AR by Day 360. However thin layer chromatography (2D TLC of isolated component) confirmed that this peak was comprised of more than one component co-eluting in the HPLC method as. The total levels of unidentified radioactivity accounted for a maximum of 28.70% AR at Day 210.
- Identification and characterisation of parent and transformation products: The test item and the degradation products M1 and M3 in the samples were identified using HPLC by comparing the retention time of the radioactive peak with that of an authentic standard. Each sample was fortified with the reference standard and analyzed by HPLC. During routine HPLC analysis the injection volume of concentrated CaCl2 extracts was high in order to reach sufficient sensitivity for detection of radiolabelled components. This led to a deterioration of the chromatography for M3. As a result of this, the radioactivity associated with M3 split into a retention time region between ca 5.4 min and 8.7 min. The radioactivity in this region was summed and assigned as M3. Several analyses were made using a smaller injection volume to improve the chromatography and this demonstrated that there was only a single peak in this region. Selected samples were also analysed by 1D TLC, to confirm the identity of test item and the degradation products M1 and M3. The identity of test item and the degradation product M1 were also confirmed by LC-MS/MS analysis of selected samples. CaCl2 and solvent extracts for Day 60 replicate 2, Day 120 replicate 2 and Day 150 replicate 1 samples were analysed by LC-MS/MS and radiodetection to confirm the presence of test item and M1. The presence of peaks at 42.7 and ca 43.6 minutes in the radiochromatogram corresponded to test item and were present in the solvent extracts of Day 60 replicate 2, Day 120 replicate 2 and Day 150 replicate 1. These peaks corresponded to peaks at 42.56 and 43.43 minutes in the extracted ion chromatogram of m/z 362. The presence of m/z 362 instead of the m/z 360 seen in the non-labelled standard is due to the incorporation of the 14C label at high specific activity. The background subtracted full scan spectrum confirms the molecular ion at m/z 362. The MSn analysis is consistent with that of the test item reference standard but also shows the +2 Da shift observed with the molecular ion. The peak at ca 27 minutes in the radiochromatogram was present in all samples analysed and corresponded to a peak in the extracted ion chromatogram of m/z 378 at 27.11 minutes. This is consistent with M1. The full scan spectrum confirms the molecular ion at m/z 378 and also shows the dehydrated ion at m/z 360 and the sodium adduct at m/z 400. MSn analysis is consistent with that of the M1 reference standard. Both the full scan spectrum and MSn analysis show a +2 Da shift compared to the reference standard due to incorporation of the 14C label at high specific activity. - 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 4 in 'Any other information on results incl. tables'.
- Test item identity and purity: The identity of the [14C]-labelled was confirmed using HPLC by co-injection of a solution of [14C]- labelled test item with unlabelled test item standard. The radiochemical purity of the application solution was determined, prior to test item application, as 100%.
- Verification of concentration procedures: The amount of radioactivity in the extract before concentration was compared with the amount of radioactivity following concentration. Procedural recoveries were within the range of 91.1% - 107.3% for CaCl2 extract pools and 92.2% - 107.0% for solvent extract pools and were therefore regarded as quantitative.
- Verification of HPLC chromatographic procedures: A solution containing unlabelledtest item was analyzed prior to the analysis of radiolabelled dose samples in order to confirm effective operation of the column and instrument. A solution containing unlabelled test item, M1 and M3 reference substances was analyzed prior to the analysis of radiolabelled soil extracts. The analytical method (HPLC) was verified by comparing, for selected analyses, the amount of radioactivity injected onto the column with the amount of radioactivity recovered from the column. Recoveries of radioactivity were in the range 92.2%-101.3% AR.
- Material Balance: Material balances were quantitative with mean values in the range 93.43% AR to 110.32% AR. All further reported recovery values are means of two replicates unless otherwise stated. Extractable radioactivity decreased throughout the study period from 93.44% AR at zero time to 29.39% AR at Day 360. As extractability decreased non-extractable residues increased from 0.27% AR at zero time to a maximum of 58.27% AR by the end of the study period. Following extraction and combustion analysis, the non-extractable residues of Day 360 samples were further analysed. Harsh extraction of the residues and subsequent organic matter fractionation into humin, fulvic acid and humic acid were performed. The majority of the radioactivity in Day 360 residues (41.56 and 44.29% AR for Replicate 1 and Replicate 2, respectively) was characterised as being associated with the humin fraction of the soil organic matter. The radioactivity associated with 14CO2 also increased over the course of the study reaching a maximum of 22.66% AR by Day 360. Samples of sodium hydroxide associated with the Day 360 samples were treated with saturated barium chloride. The subsequent quantitative precipitation of radioactivity as barium carbonate indicated that the radioactivity present in these traps was attributable to 14CO2.
- Kinetic analysis of data: The SFO half-life and DT90 values of the test substance were 40 days and 133 days, respectively.
- Aerobicity (or anaerobicity), moisture, temperature and other experimental conditions maintained throughout the study: Yes - Conclusions:
- In a biodegradation study in soil, performed in accordance with OECD TG 307 and EPA guideline 162-1, under aerobic condition, the calculated DT50 value was 40 days for the 14C-pyrazole labelled test substance in Gartenacker (loam) Soil. This DT50 value was re-calculated to be 39.8 days out side of the original study using simple first order kinetics.
- Executive summary:
The biodegradation of the14C-pyrazole labelled test item in Gartenacker (Loam) soil was investigated according to OECD TG 307 and EPA 162 -1 guidelines. The study was in compliance with GLP criteria and was conducted in the dark for 360 days at 20 ± 2°C. The 14C-labelled test itemwas applied to a bulk soil sample at a rate of 0.1682 mg/kg soil dw (equivalent to a field use rate of 126.2 g/ha soil, assuming 5 cm incorporation depth and a bulk density of 1.5g/cm3).The moisture content of the soil was maintained at pF2 during the study. The testsystem consisted of a flow through apparatus containing test vessels of treated soil connected to 2M NaOH and saturated barium chloride solution traps for collecting14CO2. Duplicate samples were analysed immediately following test substance application (zero time and after the following periods of incubation under aerobic conditions: 7, 14, 30, 45, 60, 90, 120, 150, 180, 210 and 360 days. The trapping solution was analysed by LSC. For soil extracts, qualitative analysis and metabolite identification of the soil extracts were performed by HPLC, LSC, TLC and followed by LC-MS/MS for confirmation.
The material balance was maintained in a range of 93.43% of applied radioactivity (AR) to 110.32% AR throughout the study. The radioactivity associated with 14CO2 increased over the course of the study reaching a maximum of 22.7% AR by Day 360. The HPLC analysis of soil extracts (CaCl2 and solvent extract pools) demonstrated that the [14C]-labelled test item degraded readily in the loam soil tested. The [14C]-labelled test item decreased from 93.4% AR at zero time to 2.6% AR by Day 360. Two major (> 5% AR) degradation products were detected in soil extracts over the course of the study. M1 reached a maximum of 22.3% AR at Day 45 before declining to 2.2% AR by the end of the study. M3 reached a maximum of 11.5% AR at Day 150 before declining to 5.4% AR at Day 360. A maximum of 33 minor unidentified transformation products were detected at any one time point. No individual unidentified component accounted for greater than 5% AR except for one unknown degradation product which reached a maximum of 5.4% AR at Day 90 before declining to 2.1% AR by Day 360. However, the 2D TLC analysis revealed that this degradation product contained several components co-eluting in the HPLC method. The total levels of unidentified radioactivity accounted for a maximum of 28.7% AR at Day 210. Based on these findings, the DT50 and DT90 values of the [14C]-labelled test item were calculated to be 40 and 133 days, respectively. The DT50 value was recalculated outside of the original study and was determined to be 39.8 days, using simple first order kinetics (Hayes, 2009).
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 28 Jun 2007 to 28 Jul 2008
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 307 (Aerobic and Anaerobic Transformation in Soil)
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 007
- Soil no.:
- #1
- Soil type:
- sandy clay loam
- % Clay:
- 23.43
- % Silt:
- 25.24
- % Sand:
- 51.33
- % Org. C:
- 3.9
- pH:
- 6.5
- CEC:
- 15.7 other: mmol/kg soil
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 35.52
- Soil no.:
- #2
- Soil type:
- sandy loam
- % Clay:
- 8.45
- % Silt:
- 33.06
- % Sand:
- 58.49
- % Org. C:
- 2.7
- pH:
- 7.2
- CEC:
- 8.9 other: mmol/kg soil
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 35
- Soil no.:
- #3
- Soil type:
- silty clay loam
- % Clay:
- 33.87
- % Silt:
- 56.6
- % Sand:
- 9.53
- % Org. C:
- 1.1
- pH:
- 7.8
- CEC:
- 16.8 other: mmol/kg soil
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 34.69
- Soil no.:
- #4
- Soil type:
- sandy loam
- % Clay:
- 7.01
- % Silt:
- 24.38
- % Sand:
- 68.61
- % Org. C:
- 1.6
- pH:
- 7.1
- CEC:
- 1.6 other: mmol/kg soil
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 29.21
- Details on soil characteristics:
- Soil properties of the four different soils are provided in Table 1 in “Any other information on materials and emthods incl tables”.
SOIL COLLECTION AND STORAGE
- Geographic location:
Soil I (18 Acres): Winkfield (Winkfield, England, 51°26' N, 0°42' W)
Soil II (Gartenacker): Les Barges (Vouvry, Switzerland, 46°20' N, 06°53' E)
Soil III (Marsillargues): Marsillargues (34590 Marsillargues, France, 43°39' N, 4°10' E)
Soil IV (Pappelacker): Les Barges (Vouvry, Switzerland, 46°20' N, 06°53' E)
- Pesticide use history at the collection site: None of the soils had been fertilised or treated with pesticides for at least 12 months prior to sampling.
- Collection procedures: Sampling and handling of the soils was performed in accordance with ISO 10381-6 “(Soil Quality-Sampling-Guidance on the collection, handling and storage of soil for the assessment of aerobic microbial processes in the laboratory)”.
- Sampling depth:
Soil I (18 Acres) was sampled from the top 5 to 15 cm soil layer.
Soil II (Gartenacker) was sampled from the top 2 to 15 cm soil layer.
Soil III (Marsillargues) was sampled from the top 5 to 15 cm soil layer.
Soil IV (Pappelacker) was sampled from the top 2 to 15 cm soil layer.
- Soil preparation: Soils were sieved to 2 mm after sampling and arrived in good condition at the test facility. The soils were passed again through a 2-mm sieve and thoroughly homogenised before use. Once sieved, the soil moisture content was determined for triplicate subsamples by oven drying and weighing. - Soil No.:
- #1
- Duration:
- 123 d
- Soil No.:
- #2
- Duration:
- 361 d
- Soil No.:
- #3
- Duration:
- 123 d
- Soil No.:
- #4
- Duration:
- 123 d
- Soil No.:
- #1
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.169 mg/kg dw
- Soil No.:
- #2
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.177 mg/kg dw
- Soil No.:
- #3
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.175 mg/kg dw
- Soil No.:
- #4
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.169 mg/kg dw
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 20 ± 2°C
- Humidity:
- pF 2.0 (35.52 g water/100g soil)
- Microbial biomass:
- 338 (0 DAT) - 287 (123 DAT) mg micr. C/kg dry soil
- Soil No.:
- #2
- Temp.:
- 20 ± 2°C
- Humidity:
- pF 2.0 (35.00 g water/100g soil)
- Microbial biomass:
- 200 (0 DAT) - 339 (361 DAT) mg micr. C/kg dry soil
- Soil No.:
- #3
- Temp.:
- 20 ± 2°C
- Humidity:
- pF 2.0 (34.69 g water/100g soil)
- Microbial biomass:
- 122 (0 DAT) - 185 (123 DAT) mg micr. C/kg dry soil
- Soil No.:
- #4
- Temp.:
- 20 ± 2°C
- Humidity:
- pF 2.0 (29.21 g water/100g soil)
- Microbial biomass:
- 319 (0 DAT) - 160 (123 DAT) mg micr. C/kg dry soil
- Details on experimental conditions:
- EXPERIMENTAL DESIGN
- Soil condition: Fresh
- Soil: 75 g dw/replicate
- No. of replication treatments: 2
- Test apparatus: All-glass one-litre cylindrical metabolism flasks
- Details of traps for CO2 and organic volatile: Sodium hydroxide (NaOH) and ethylene glycol traps were monitored for radioactivity by LSC at every sampling interval. The actual volume of sodium hydroxide and ethylene glycol solutions was determined and their radioactivity content was measured by LSC separately for each trap. Due to the very low amount of radioactivity in the sodium hydroxide solutions, it was not necessary to confirm the presence of 14CO2 by precipitation with barium hydroxide. Each system consisted of duplicate flasks connected in series and continuously ventilated with moistened air. The exhaust air was passed through a trapping system equipped with two absorption traps containing 50 mL of 2 N NaOH and 50 mL ethylene glycol to trap 14CO2 and organic volatiles, respectively. For sampling day 0, no absorption traps were set up.
- Identity and concentration of co-solvent: 50 mL acetone/water (1:4; v/v).
PREPARATION OF APPLICATION SOLUTION
An application solution was prepared for the study by taking an aliquot of the radiolabelled test item and diluting it in 50 mL acetone/water (1:4; v/v). The total amount of 14C-test item in this solution was determined by liquid scintillation counting (LSC) of three 50 μL subsamples. Based on the total mean amount of radioactivity measured (723’685’000 dpm/50 mL) and the specific activity of the radiolabelled test item (2.09 MBq/mg), the concentration of the application solution was calculated to be 0.115 mg test item/mL.
- Application method: Spray to the soil. An airbrush was used to spray the bulk soil. The airbrush was connected to a supply of compressed air via a regulator set to ca. 2 bar and a flow meter with an internal needle valve to allow fine adjustment of the air flow. Spraying took place in a constructed spray tent within a fume hood. Soil batches were spread out into a polythene square ca. 50 x 90 cm and ca. 2 cm in depth. Before the spraying was started, the back pressure in the air brush was released and spraying commenced. Spraying started at the back top right hand corner of the soil square and continued in forward and backward lines across the soil. Care was taken not to spray too near the edges of the soil. Three times in between, the soil was mixed with a spatula and the spraying continued. The airbrush was held ca. 5 cm from the soil surface. Due to the amount of soil to be sprayed (ca. 3 kg) 6.06 mL of the application solution was used, taking into account about 20% losses by drift as determined in a pre-test. Once the dose solution was applied, the soil was mixed thoroughly using a mixer for about 30 to 60 min. The homogeneity was determined by combustion of five aliquots of 0.6 - 1.0 g of soil. Thereafter, aliquots were transferred into the metabolism flasks.
Experimental conditions
- Moisture maintenance method: The moisture content of the soils was continuously maintained at a water content corresponding to pF 2.0 throughout the study. Soil water losses were kept to a minimum by circulating moistened air at a minimum volumetric flow rate sufficient enough to pass through the trapping system. Water loss was compensated for by weighing the samples periodically during the study (every two to three weeks). Where necessary, the amounts of evaporated water were added uniformly over the soil and the flask gently shaken to incorporate homogeneously the water.
- Continuous darkness: Yes
SAMPLING DETAILS
- Sampling intervals: Duplicate samples per soil were taken for analysis after 0, 7, 14, 27, 56, 90 and 123 days of incubation. For soil II, three additional sampling intervals were taken on days 195, 271 and 361. At each sampling interval, the samples were submitted to the work-up procedure. - Soil No.:
- #1
- % Total extractable:
- 97.3
- % Non extractable:
- 5
- % CO2:
- 0.3
- % Other volatiles:
- < 0.1
- % Recovery:
- 100
- Remarks on result:
- other: on day 123
- Soil No.:
- #2
- % Total extractable:
- 67.3
- % Non extractable:
- 23.1
- % CO2:
- 1.5
- % Other volatiles:
- < 0.1
- % Recovery:
- 91.9
- Remarks on result:
- other: on day 361
- Soil No.:
- #3
- % Total extractable:
- 96.9
- % Non extractable:
- 6.2
- % CO2:
- 0.7
- % Other volatiles:
- < 0.1
- % Recovery:
- 100
- Remarks on result:
- other: on day 123
- Soil No.:
- #4
- % Total extractable:
- 96.5
- % Non extractable:
- 4.8
- % CO2:
- 0.2
- % Other volatiles:
- < 0.1
- % Recovery:
- 100
- Remarks on result:
- other: on day 123
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 12.4
- Parameter:
- radiochem. meas.
- Sampling time:
- 123 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 75.9
- Parameter:
- radiochem. meas.
- Sampling time:
- 361 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 43.4
- Parameter:
- radiochem. meas.
- Sampling time:
- 123 d
- Parent/product:
- parent
- Soil No.:
- #4
- % Degr.:
- 30.6
- Parameter:
- radiochem. meas.
- Sampling time:
- 123 d
- Key result
- Soil No.:
- #1
- DT50:
- 976 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Recalculated outside of the original study (Hayes 2009)
- Key result
- Soil No.:
- #2
- DT50:
- 141 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 149 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #4
- DT50:
- 233 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Soil No.:
- #1
- DT50:
- > 1 yr
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: reported in the original study
- Transformation products:
- not specified
- Remarks:
- M1
- Details on transformation products:
- The test item as well as the major radioactive fraction F6 were identified by LC/MS as well as by co-chromatography with the reference items test item and M1, respectively. M1 represented the major degradate and reached its maximum of 23.6% of applied radioactivity on day 195 and decreased thereafter to 21.2% on day 361 in soil II. F1, a radioactive fraction, amounted to a maximum of 10.5% of applied radioactivity on Day 271. On day 361 its amount decreased to 6.4% of applied radioactivity. F1 corresponds to radioactivity at the origin of the TLC plate and consisted of several components, all less than 4% of applied radioactivity, as shown by HPLC and TLC analyses. All other radioactive fractions did not exceed 3% of applied radioactivity at any sampling interval.
- Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results is provided in Table 2 - Table 10 in 'Any other information on results incl. tables'.
TEST CONDITIONS
- Aerobicity (or anaerobicity), moisture, temperature and other experimental conditions maintained throughout the study: Yes
- Radiochemical purity and stability of the 14C-labelled test item: The radiochemical purity of 14C-labelled test item prior to treatment was determined by TLC to be 100%. The content of the test item in the application solution after treatment was 100%, thereby indicating its stability during the application procedure.
- Soil biomass: The microbial biomass of the soils determined at start of incubation was 338, 200, 122 and 319 mg microbial C/kg for soils I, II, III and IV, respectively. At the end of incubation (soils I, III and IV) or day 123 for soil II, the corresponding values were 287, 240, 185 and 160 mg microbial C/kg, respectively. The microbial biomass of soils II after 361 days of incubation was 339 mg microbial C/kg. The results show that the soils remained microbially active for the duration of the study.
- Recovery and distribution of radioactivity: The mean recoveries were 102.2 ± 0.9%, 98.1 ± 2.6%, 103.9 ± 0.8% and 101.1 ± 1.9% of applied radioactivity for soils I to IV, respectively. The amount of total extractable radioactivity remained high for all four soils, decreasing from an initial amount of more than 97% of the applied radioactivity to levels of 97.3%, 88.8%, 96.9% and 96.5% in soils I to IV, respectively, after 123 days of incubation. In soil II, total extractables continued to decrease and represented on day 361 67.3% of the applied radioactivity. The amounts of radioactivity in the calcium chloride extracts were low. Reflux extraction released maximum levels of 26.1%, 8.7%, 16.8% and 5.7% of the applied radioactivity for soils I, II, III and IV, respectively. The maximum amount of non-extractable radioactivity in the soils during 123 days of incubation varied between 5.7% (soil I), 12.7% (soil II), 6.2% (soil III) and 8.4% (soil IV) of the applied radioactivity. In soil II, unextracted residues increased to 23.1% of applied on day 361. For soil II on day 361, the soil remaining after reflux extraction with acetonitrile/water (4:1;v/v) was subjected to a harsh extraction with acetonitrile/0.1M hydrochloric acid under reflux conditions, releasing 2.1% of applied radioactivity. Thereafter, a fractionation of the soil organic matter into humic acid, fulvic acid and humin fractions was performed. More than two thirds of the bound radioactivity, i.e. 69.6% corresponding to 14.4% of the applied radioactivity was incorporated into the humin fraction and the humic acids, i.e. into the less mobile soil organic compounds. The radioactivity associated with the fulvic acids fraction correspondingly represented 30.4% of the non-extractable radioactivity (or 6.3% of the applied radioactivity). Low mineralization of the radioactive residues was observed. Radioactive carbon dioxide accounted for less than 1% of applied for all four soils during 123 days of incubation. In soil II, 14CO2 represented 1.5% of applied on day 361. Very low amounts of other organic volatile radioactivity were evolved throughout incubation (< 0.1% of applied for all soils).
- Characterisation of radioactivity: Calcium chloride and combined acetonitrile/water extracts were analysed separately by one dimensional TLC: The results were confirmed by HPLC and two dimensional TLC. The amount of test item in all four soils steadily decreased with time. Immediately after treatment (time 0), the parent compound represented between 95.8% and 102.3% of the applied radioactivity. On day 123, it decreased to 87.6%, 48.4%, 56.6% and 69.4% of the applied radioactivity for soils I, II, III and IV, respectively. For soil II, the pattern of degradation was further investigated and the incubation prolonged. On day 361, the amounts of test item represented 24.1% of the applied radioactivity. Only low amounts could be extracted with CaCl2 solution and decreased continuously from 3.4% of applied radioactivity on day 0 to 0.6% on day 361. The reflux extraction did not extract more than 5.1% of the applied radioactivity. Characterisation of extracts from soil II showed that test item was degraded to at least eight components. The test item as well as the major radioactive fraction F6 were identified by LC/MS as well as by co-chromatography with the reference items parent and M1, respectively. M1 represented the major degradate and reached its maximum of 23.6% of applied radioactivity on day 195 and decreased thereafter to 21.2% on day 361 in soil II. F1, a radioactive fraction, amounted to a maximum of 10.5% of applied radioactivity on Day 271. On day 361 its amount decreased to 6.4% of applied radioactivity. F1 corresponds to radioactivity at the origin of the TLC plate and consisted of several components, all less than 4% of applied radioactivity, as shown by HPLC and TLC analyses. All other radioactive fractions did not exceed 3% of applied radioactivity at any sampling interval.
MAJOR TRANSFORMATION PRODUCTS
M1 was the only major degradate observed and amounted to a maximum of 23.6% of the applied radioactivity on day 195. Thereafter, it decreased to 21.2% on day 361.
MINOR TRANSFORMATION PRODUCTS
All other radioactive fractions did not exceed 4% of applied radioactivity at any sampling interval.
TOTAL UNIDENTIFIED RADIOACTIVITY (RANGE) OF APPLIED AMOUNT: not exceeding 4% of applied
EXTRACTABLE RESIDUES
- % of applied amount at day 0: 97.7% (soil I), 97.6% (soil II), 102.5% (soil III) and 99.1% (soil IV)
- % of applied amount at end of study period: 97.3% (soil I), 67.3% (soil II), 96.9% (soil III) and 96.5% (soil IV)
NON-EXTRACTABLE RESIDUES
- % of applied amount at day 0: 5.4% (soil I), 2% (soil II), 2.6% (soil III) and 1.4% (soil IV)
- % of applied amount at end of study period: 5% (soil I), 23.1% (soil II), 6.2% (soil III) and 4.8% (soil IV)
MINERALISATION
- % of applied radioactivity present as CO2 at end of study: 0.3% (soil I), 1.5% (soil II), 0.7% (soil III) and 0.2% (soil IV)
- Degradation rate of test item in soil: The measured amount of 14C-labelled test item in the soil extracts and its total amount are reported in % of the applied radioactivity. Based on these results, the following half-lives and DT90 values were calculated for test item using the total amount of test item (mean values, without bound residues) and the kinetic calculation software and single first-order kinetics (SFO).
- DT50: 976 days (soil I), 141 days (soil II), 149 days (soil III) and 233 days (soil IV)
- DT90: >>1 year (soil I), 470 days (soil II), 494 days (soil III) and >1 year (soil IV) - Conclusions:
- In a biodegradation study in soil, performed according to OECD TG 307, the DT50 values were calculated to be > 1 year, 141 days, 149 days, and 233 days for 18 Acres, Gartenacker, Marsillargues and Pappelacker, respectively. The DT50 value for 18 Acres was recalculated outside of the original study and was determined to be 976 days, using SFO (Hayes, 2009). The pathways of disappearance of the test item was via degradation to M1 and numerous minor metabolites (not exceeding 4% of applied) as well as the formation of unextracted residues.
- Executive summary:
The biodegradation of the14C-phenyl labelled test item was studied according to OECD TG 307 in four soils: I (18 Acres, sandy clay loam), II (Gartenacker, sandy loam), III (Marsillargues, silty clay loam) and IV (Pappelacker, sandy loam) incubated under aerobic conditions at 20 °C for a period of 123 days (soils I, III and IV) or 361 days (soil II). The study was complied with GLP criteria. The soils were treated with the 14C-labelled test item at a target concentration of 0.167 mg/kg dry soil (corresponds to the recommended field rate of 125 g/ha, assuming a homogeneous distribution of the test item in the upper 5 cm of the soil layer and a soil density of 1.5 g/cm3). The test item was applied as a fine spray over the soil surface as a bulk. After treatment, the soils were mixed, and the amount applied checked by combustion of five soil aliquots. Thereafter, 75 g dry weight subsamples were redistributed in the flasks. The actual amount of test item applied corresponded to 0.169 - 0.177 mg/kg dry soil (corresponding to 101% to 106% the target concentration). The treated soil samples were then incubated at 20 ± 2 °C in the dark under continuous ventilation with moistened air. The exhaust air was passed through a trapping system consisting of flasks of sodium hydroxide and ethylene glycol in series. The moisture content of each soil sample was maintained at pF 2.0 throughout the study. The soil microbial biomass determined prior to treatment, on day 123 and/or at the end of the study, showed that the soil samples were microbially active. Duplicate samples per soil were taken immediately after treatment (time 0) and after 7, 14, 27, 56, 90 and 123 days of aerobic incubation. For soil II, incubation was extended with additional sampling intervals on days 195, 271 and 361. The radioactivity quantification and metabolites identification were performed and by HPLC, TLC and LC/MS.
Mean recoveries of radioactivity were 102.2 ± 0.9%, 98.1 ± 2.6%, 103.9 ± 0.8% and 101.1 ± 1.9% of applied for soils I to IV, respectively. Very low mineralization of the radioactive residues was observed in all soils. Radioactive carbon dioxide accounted for less than 1% of applied for all four soils during 123 days of incubation. In soil II, 14CO2 represented 1.5% of applied on day 361. Very low levels of organic volatile compounds were evolved throughout the incubation (< 0.1% of applied for all soils). The degradation was fastest for soil II with the 14C-labelled test item decreasing from 95.8% of the applied radioactivity to 48.4% after 123 days of aerobic incubation. The corresponding values for soil I were 96.9% and 87.6%, for soil III, 102.3% and 56.6% and for soil IV, 98.9% and 69.4%, respectively. Incubation for soil II was continued until day 361 where the 14C-labelled test item amounted to 24.1% of applied. Besides the parent compound, eight degradation fractions were detected. M1 was the only major degradate observed and amounted to a maximum of 23.6% of the applied radioactivity on day 195. Thereafter, it decreased to 21.2% on day 361. All other radioactive fractions did not exceed 4% of applied radioactivity at any sampling interval. Based on these findings, the DT50 and DT90 values were calculated to be > 1 year (soil I), 141 days (soil II), 149 days (soil III) and 233 days (soil IV) for the test item using the simple first-order kinetics (SFO). The DT50 value for soil I was recalculated outside of the original study and was determined to be 976 days, using SFO (Hayes, 2009).
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 19 Feb 2008 to 12 Oct 2010
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 307 (Aerobic and Anaerobic Transformation in Soil)
- Version / remarks:
- 24 April 2002
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- other: EPA 162-1
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 009
- Soil no.:
- #1
- Soil type:
- clay loam
- % Clay:
- 37.73
- % Silt:
- 27.67
- % Sand:
- 34.6
- % Org. C:
- 2.91
- pH:
- 5.43
- CEC:
- 34.97 other: mmol/100g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 44.72
- Soil no.:
- #2
- Soil type:
- clay
- % Clay:
- 61.9
- % Silt:
- 18.7
- % Sand:
- 19.4
- % Org. C:
- 1.86
- pH:
- 3.98
- CEC:
- 21.14 other: mmol/100g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 33.63
- Soil no.:
- #3
- Soil type:
- sand
- % Clay:
- 6.35
- % Silt:
- 0.63
- % Sand:
- 93.03
- % Org. C:
- 0.47
- pH:
- 4.24
- CEC:
- 3.47 other: mmol/100g soil d.w.
- Bulk density (g/cm³):
- 1.5
- % Moisture content:
- 14.34
- Details on soil characteristics:
- Soil properties are provided in Table 1 in “Any other information on materials and methods incl. tables”.
SOIL COLLECTION AND STORAGE
- Geographic location:
Soil I was sampled from an area in Piracicaba (São Paulo, Brazil).
Soil II was sampled from an area in Veranópolis (Rio Grande do Sul, Brazil).
Soil III was sampled from an area in Piracicaba (São Paulo, Brazil).
- Sampling depth: 20 cm
- Soil preparation: The soils were passed through a 2-mm sieve and thoroughly homogenised before use. Once sieved, the soil moisture content was determined for triplicate subsamples by halogen drying and weighing. - Soil No.:
- #1
- Duration:
- 120 d
- Soil No.:
- #2
- Duration:
- 120 d
- Soil No.:
- #3
- Duration:
- 120 d
- Soil No.:
- #1
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.120 mg/kg soil d.w.
- Soil No.:
- #2
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.165 mg/kg soil d.w.
- Soil No.:
- #3
- Initial conc.:
- 0.167 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- measured concentration: 0.107 mg/kg soil d.w.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 20 ± 2 °C
- Humidity:
- Soil adjusted close to pF2 moisture tension
- Microbial biomass:
- 449 (start) - 300 (120 d) mg micr. C/kg dry soil
- Soil No.:
- #2
- Temp.:
- 20 ± 2 °C
- Humidity:
- Soil adjusted close to pF2 moisture tension
- Microbial biomass:
- 135 (start) - 119 (120 d) mg micr. C/kg dry soil
- Soil No.:
- #3
- Temp.:
- 20 ± 2 °C
- Humidity:
- Soil adjusted close to pF2 moisture tension
- Microbial biomass:
- 368 (start) - 203 (120 d) mg micr. C/kg dry soil
- Details on experimental conditions:
- EXPERIMENTAL DESIGN
- Soil condition: Fresh
- Soil: 100 g/replicate
- No. of replication treatments: 2
- Test apparatus: All-glass one-litre cylindrical metabolism flasks
- Details of traps for CO2 and organic volatile: The trapping system, consists of 50 mL ethylene glycol to trap organic volatiles and one containing 50 mL 2N NaOH to trap 14CO2. For the samples of day 0, no absorption traps were set up.
Test material application
- Volume of test solution used/treatment: 5 mL (Soil I and III), 15 mL (soil II)
- Application method: Spraying. The test item was applied to the soil by a spraying process using an airbrush. Spraying took place in a constructed spray tent within a fume hood. The test item was sprayed on soil batches that were spread out in polythene trays measuring about 50 x 90 cm and 2 cm in depth. Care was taken not to spray too near the edges of the tray. For soil II, a volume of 15 mL application solution was used to treat about 3.2 kg soil (fresh weight). Spraying was interrupted three times in order to mix the soil with a spatula. After treatment, the soil was mixed thoroughly using a mixer and the homogeneity was determined by combustion of five aliquots of up to 0.26 g soil. For soils I and III, a volume of about 5 mL application solution was used to treat about 3.14 kg soil I or 2.66 kg soil III (fresh weights). Spraying was interrupted six times in order to mix the soil with a spatula. The homogeneity was determined thereafter by combustion of ten aliquots of up to 0.65 g soil. The soil moisture of the treated soil was determined. Aliquots corresponding to 100 g dry soil were transferred into the flasks and the soil moisture was adjusted to about pF 2. The flasks were then incubated in an air-conditioned room at about 20 °C. During incubation, the system was continuously ventilated with air. For soils I and III, the amount of radioactivity applied to the test system was determined by combustion of 10 soil aliquots. For soil II, the applied amount was determined by the radioactivity recovered by extraction and combustion of both replicates of the 0-day sample. The mean values of the applied radioactivity (100% applied) are as follows for each soil [mg/kg]: 0.120 (Soil I), 0.165 (Soil II), 0.107 (Soil III)
- Preparation of Application Solution: Soils I and III: A stock solution of 14C-test item in acetonitrile was measured in triplicate aliquots to contain 285’623’000 dpm/ml. An application solution was prepared by diluting 0.49 mL stock solution with 4.51 mL acetonitrile and then with water to a final volume of 10 ml. The application solution was measured in triplicate aliquots to contain 13’946’700 dpm/mL corresponding to 0.111 mg/mL 14C-test item considering the specific activity of 2.0868 MBq/mg. Soil II: An application solution was prepared by dissolving an aliquot of the radiolabeled test item in 100 mL acetone/water (2:1; v/v). The amount of 14C-test item in solution was determined by liquid scintillation counting (LSC) in triplicate subsamples to be 4’184’000 dpm/mL, corresponding to 0.033 mg/mL, considering the specific activity of 2.0868 MBq/mg.
Experimental conditions
- Moisture maintenance method: The moisture content of the soils was maintained at a water content near pF 2.0 throughout the study. Soil water losses were kept to a minimum by circulating moistened air at a minimum volumetric flow rate sufficient enough to pass through the trapping system. Water loss was determined by weighing the samples periodically during the study (up to 9 times). Where necessary, water was added uniformly over the soil and the flask gently shaken to incorporate homogeneously the water.
- Continuous darkness: Yes
- Sampling intervals: Duplicate samples per soil were taken immediately after treatment (time 0) and after 7, 14, 28, 59 (soils I and III) or 61 (soil II), 92 (soils I and III) or 90 (soils II) and 120 days of incubation. - Soil No.:
- #1
- % Total extractable:
- 95.2
- % Non extractable:
- 4.5
- % CO2:
- 1.9
- % Other volatiles:
- < 0.1
- % Recovery:
- 100
- Remarks on result:
- other: day 120
- Soil No.:
- #2
- % Total extractable:
- 80.7
- % Non extractable:
- 13.4
- % CO2:
- 3.1
- % Other volatiles:
- < 0.1
- % Recovery:
- 97.25
- Remarks on result:
- other: day 120
- Soil No.:
- #3
- % Total extractable:
- 99.7
- % Non extractable:
- 3.9
- % CO2:
- 0.6
- % Other volatiles:
- < 0.1
- % Recovery:
- 100
- Remarks on result:
- other: day 120
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 26.6
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 55.4
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 24.3
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Key result
- Soil No.:
- #1
- DT50:
- 271 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #2
- DT50:
- 121 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 264 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Transformation products:
- not specified
- Remarks:
- M1
- Details on transformation products:
- Besides the parent compound, numerous degradation fractions were detected. The major degradate was M1, reaching a plateau at 8.6% to 9.8% in soil II from day 61 onwards. In soils I and III, M1 reached 6.9% and 8.4% by day 120, respectively.
- Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- - Aerobicity (or anaerobicity), moisture, temperature and other experimental conditions maintained throughout the study: Yes
- Soil Biomass: The microbial biomass of the soils determined at start of incubation was 449, 135 and 368 mg microbial C/kg for soils I, II and III, respectively. At the end of incubation the corresponding values were 300, 119 and 203 mg microbial C/kg, respectively. The results show that the soils remained microbially active for the duration of the study.
- Recovery and Distribution of Radioactivity: The mean recoveries were 102.7 ± 1.6%, 98.8 ± 1.4% and 103.5 ± 1.5% of the applied radioactivity for soils I to III, respectively. The total extractable radioactivity remained high during the whole study, amounting to levels of 93.9% to 102.1% (soil I), 80.7% to 92.7% (soil II) and 95.7% to 102.5% (soil III). Reflux extraction released up to 10.0%, 13.2% and 7.1% of the applied radioactivity for soils I to III, respectively. The amount of non-extractable radioactivity accounted for up to 5.7%, 13.4% and 7.3% of the applied radioactivity for soils I to III, respectively. Low levels of mineralization were observed. The levels of radioactive carbon dioxide peaked at 1.9% of the applied radioactivity in soil I and 3.1% in soil II and 0.6% in soil III towards the end of the study. Negligible levels of organic volatiles were observed during the study (< 0.1% of applied for all soils).
- Characterization of Radioactivity: The amount of the test substance decreased with time in soils I to III. The dissipation rate of the test substance was fastest in soil II where the level of the test substance decreased from 88.4% immediately after application to 44.6% by day 120. In soils I and III, the levels of the test substance decreased from 99.8% to 73.4% and from 102.5% to 75.7%, respectively. - Conclusions:
- In a biodegradation study in soil, performed according to OECD TG 307 and EPA guidelines 162-1, under aerobic condition, the DT50 values of the 14C-phenyl labelled test item were determined to be 271, 121, and 264 days for Argissolo, Latossolo and Neossolo soils, respectively. The test item dissipated from the soil via formation of M1 (6.9% to 9.8%) and numerous minor metabolites, as well as the formation of non-extractable residues (5.7% to 13.4%) and some mineralization (0.6% to 3.1%).
- Executive summary:
The biodegradation of the14C-phenyl labelled test item was studied according to OECD TG 307 and EPA guideline 162-1 in three Brazilian soils: Argissolo (clay loam), Latossolo (clay) and Neossolo (sand). The study complied with GLP criteria. The 14C-labelled test item was applied at a nominal rate of 0.167 mg/kg dry weight of soil (equivalent to a single field application rate of 125 g/ha, incorporated into the soil to a depth of 5 cm and assuming a soil bulk density of 1.5 g/cm3). The 14C-labelled test item was applied as a fine spray over the soil surface as a bulk. After treatment, the soils were mixed, and the amount applied checked by combustion of five soil aliquots. Thereafter, 100 g dry weight subsamples were redistributed in the flasks. The actual amount of test item applied to the three soils corresponded to 0.107 - 0.165 mg/kg dry soil. The treated soils were incubated under aerobic conditions at 20 ± 2 °C in the dark for 120 days. The soil moisture was maintained to near pF 2.0 throughout the study. Continuous ventilation with moistened air was provided to the system. The exhaust air was passed through a trapping system consisting of flasks of ethylene glycol and sodium hydroxide in series. The soil microbial biomass, determined prior to treatment and at the end of the study, showed that the soil samples were microbially active. Duplicate samples per soil were taken immediately after treatment (time 0) and after 7, 14, 28, 59 (soils I and III) or 61 (soil II), 92 (soils I and III) or 90 (soils II) and 120 days of incubation. Radioactivity qualification and metabolite identification were analysed by using HPLC and TLC.
Mean recoveries of radioactivity were 102.7 ± 1.6%, 98.8 ± 1.4% and 103.5 ± 1.5% of the applied radioactivity for soils I to III, respectively. Low levels of mineralization were observed. The levels of radioactive carbon dioxide increased to 1.9% of the applied radioactivity in soil I by the end of the incubation period (120 days) and reached maximum levels of 3.1% and 0.6% in soils II and III, respectively after 90 to 120 days. Negligible levels of organic volatiles were observed during the study (< 0.1% of applied for all soils). The dissipation rate of 14C-labelled test item was fastest in soil II where the level of test item decreased from 88.4% immediately after application to 44.6% by day 120. In soils I and III, the levels of the test item decreased from 99.8% to 73.4% and from 102.5% to 75.7%, respectively, over the same incubation period. Besides the parent compound, numerous degradation fractions were detected. The major degradate was M1, reaching a plateau at 8.6% to 9.8% in soil II from day 61 onwards. In soils I and III, M1 reached 6.9% and 8.4% by day 120, respectively. Based on these findings, the DT50 values were determined to be 271, 121, and 264 days for Argissolo, Latossolo and Neossolo soils, respectively.
Referenceopen allclose all
Table 3. Mass Balance
Total radioactivity |
Sum of activity in the soil extracts, soil residue on combustion and that trapped in the 2M sodium hydroxide traps (presumed to be 14CO2). |
|
Recovery at 0 DAT |
Range 92.4 to 96.9% of applied dose |
|
Total radioactivity |
Sum of activity in the soil extracts, soil residue on combustion and that trapped in the 2M sodium hydroxide traps (presumed to be 14CO2). |
|
|
Average 95.5% |
|
Overall recovery (all samples) |
0-120 DAT (18 Acres, Pappelacker, Gartenacker and Marsillargues soils) |
Range 89.2 to 100.1% Average 96.1% |
|
180-369 DAT (Gartenacker soil) |
Range 84.3 to 92.6% Average 87.5% |
Table 4. Mass balance and distribution of radioactivity in 18 Acres soil – individual replicates (values as % of applied).
Fraction |
Replicate |
Incubation time (days after treatment, DAT) |
|||||||
0 |
7 |
14 |
29 |
43 |
61 |
90 |
120 |
||
Extract 1 |
A B |
4.0 3.8 |
3.2 3.5 |
3.3 3.0 |
3.8 3.3 |
4.0 3.8 |
3.8 4.0 |
3.9 4.0 |
4.6 4.5 |
Extract 2 |
A B |
91.0 90.4 |
91.2 90.8 |
93.0 92.5 |
91.7 92.6 |
89.3 90.1 |
90.0 90.5 |
88.5 89.0 |
86.0 87.7 |
Total Extractables |
Mean |
94.6 |
94.4 |
95.9 |
95.7 |
93.6 |
94.2 |
92.7 |
91.4 |
Non- extractables |
A
B |
0.3
0.4 |
0.5
0.5 |
0.7
0.7 |
1.1
1.0 |
1.7
1.6 |
1.8
1.6 |
2.0
1.9 |
2.6
2.5 |
NaOH trap |
A B |
- - |
0.1 0.1 |
0.1 0.2 |
0.2 0.2 |
0.2 0.2 |
0.2 0.2 |
0.2 0.2 |
0.2 0.2 |
Total |
A B |
95.3 94.6 |
95.0 94.9 |
97.1 96.4 |
96.8 97.1 |
95.2 95.7 |
95.8 96.3 |
94.6 95.1 |
93.4 94.9 |
Mean ± SD |
|
95.5 ± 1.0 |
|||||||
Table 5. Mass balance and distribution of radioactivity in Pappelacker soil -individual replicates (values as % of applied).
Fraction |
Replicate |
Incubation time (days after treatment, DAT) |
|||||||
0 |
7 |
14 |
29 |
43 |
61 |
90 |
120 |
||
Extract 1 |
A B |
6.6 7.1 |
5.8 6.1 |
5.7 5.7 |
7.4 7.7 |
9.5 9.4 |
10.4 11.0 |
11.1 10.9 |
11.3 11.3 |
Extract 2 |
A B |
90.2 89.6 |
87.8 90.1 |
92.7 92.9 |
89.5 91.1 |
87.1 87.2 |
85.6 85.5 |
83.1 83.7 |
82.1 79.3 |
Total Extractables |
Mean |
96.8 |
94.9 |
98.5 |
97.9 |
96.6 |
96.3 |
94.4 |
92.0 |
Non- extractables |
A
B |
0.1
0.1 |
0.4
0.4 |
0.7
0.7 |
1.1
1.0 |
1.7
1.7 |
2.4
2.4 |
3.6
3.7 |
5.1
5.3 |
NaOH trap |
A B |
- - |
0.1 0.1 |
0.2 0.2 |
0.3 0.3 |
0.4 0.4 |
0.5 0.5 |
0.6 0.6 |
0.7 0.7 |
Total |
A B |
96.9 96.8 |
94.1 96.7 |
99.3 99.5 |
98.3 100.1 |
98.7 98.7 |
98.9 99.4 |
98.4 98.9 |
99.2 96.6 |
Mean ± SD |
|
98.2 ± 1.5 |
|||||||
Table 6. Mass balance and distribution of radioactivity in Gartenacker soil - individual replicates (values as % of applied).
Fraction |
Replicate |
Incubation time (days after treatment, DAT) |
||||||||||
0 |
7 |
14 |
29 |
43 |
61 |
90 |
120 |
180 |
279 |
369 |
||
Extract 1 |
A B |
4.7 4.9 |
5.1 5.4 |
5.5 5.6 |
9.3 9.0 |
11.6 11.7 |
12.4 11.2 |
13.7 13.3 |
13.4 13.1 |
13.0 12.8 |
11.9 12.2 |
11.3 11.6 |
Extract 2 |
A B |
92.0 91.8 |
91.3 89.4 |
93.1 92.2 |
87.6 87.6 |
81.7 81.3 |
79.1 79.6 |
72.6 73.2 |
66.7 67.1 |
59.0 58.6 |
47.7 45.8 |
41.6 40.9 |
Total Extractables |
Mean |
96.7 |
95.6 |
98.2 |
96.8 |
93.2 |
91.2 |
86.4 |
80.2 |
71.7 |
58.8 |
52.7 |
Fulvic fraction |
A
B |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
2.3
- |
-
- |
Humic fraction |
A
B |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
-
- |
6.9
- |
-
- |
Non- extractables |
A
B |
0.1
0.1 |
0.5
0.5 |
0.7
0.7 |
1.7
1.7 |
3.5
3.9 |
5.4
5.3 |
9.1
9.2 |
12.8
12.8 |
18.2
18.6 |
13.4*
25.4 |
29.6
29.7 |
NaOH trap |
A B |
- - |
0.2 0.2 |
0.3 0.3 |
0.6 0.6 |
1.0 1.0 |
1.1 1.1 |
1.6 1.5 |
1.6 1.7 |
2.4 2.4 |
2.6 2.3 |
2.5 2.0 |
Total |
A B |
96.8 96.8 |
97.1 95.5 |
99.6 98.8 |
99.2 98.9 |
97.8 97.9 |
98.0 97.2 |
97.0 97.2 |
94.5 94.7 |
92.6 92.4 |
84.8 85.7 |
85.0 84.2 |
Mean ± SD |
0-120 DAT |
97.3 ± 1.5 |
||||||||||
180-369 DAT |
87.5 ± 3.9 |
|||||||||||
* Humin/soil residue fraction remaining after further extraction
Table 7. Mass balance and distribution of radioactivity in Marsillargues soil - individual replicates (values as % of applied).
Fraction |
Replicate |
Incubation time (days after treatment, DAT) |
|||||||
0 |
7 |
14 |
30 |
44 |
58 |
90 |
120 |
||
Extract 1 |
A B |
8.7 8.5 |
6.7 6.4 |
6.2 6.5 |
7.8 7.6 |
8.9 8.6 |
10.1 10.1 |
11.6 11.5 |
12.3 12.6 |
Extract 2 |
A B |
83.6 85.2 |
84.1 82.7 |
85.8 81.2 |
82.3 80.9 |
81.6 82.8 |
83.7 82.5 |
84.4 79.0 |
78.4 77.5 |
Total Extractables |
Mean |
93.0 |
90.0 |
89.9 |
89.3 |
91.0 |
93.2 |
93.3 |
90.4 |
Non- extractables |
A
B |
0.1
0.7 |
1.0
0.8 |
2.2
1.4 |
2.1
3.9 |
1.6
2.1 |
1.6
1.8 |
3.0
2.6 |
3.3
3.3 |
NaOH trap |
A B |
- - |
0.1 0.1 |
0.1 0.1 |
0.2 0.2 |
0.3 0.3 |
0.3 0.3 |
0.3 0.3 |
0.3 0.3 |
Total |
A B |
92.4 94.4 |
91.9 90.0 |
94.3 89.2 |
92.4 92.6 |
92.4 93.8 |
95.7 94.7 |
99.3 93.4 |
94.3 93.7 |
Mean ± SD |
|
93.4 ± 2.3 |
|||||||
Table 8. Summary of product distribution in extracts of 18 Acres soil (values as % of applied).
Retention time (Co-chromatographs with) |
Replicate |
Incubation time (days after treatment, DAT) |
|||||||
0 |
7 |
14 |
29 |
43 |
61 |
90 |
120 |
||
~24.30 mins (Parent) |
A B |
95.0 |
93.6 |
95.4 |
91.3 |
87.4 |
87.2 |
85.1 |
82.7 |
94.2 |
93.6 |
94.7 |
91.5 |
88.2 |
86.8 |
85.5 |
83.5 |
||
Mean |
94.6 |
93.6 |
95.1 |
91.4 |
87.8 |
87.0 |
85.3 |
83.1 |
|
~19.36 mins |
A B |
0.0 0.0 |
0.1 0.1 |
0.1 0.1 |
0.1 1.3 |
1.6 1.3 |
1.4 2.1 |
1.9 1.6 |
2.1 2.9 |
Mean |
0.0 |
0.1 |
0.1 |
0.7 |
1.5 |
1.8 |
1.8 |
2.5 |
|
~18.18 mins (M1+M2) |
A B |
0.0 |
0.2 |
0.4 |
2.2 |
2.1 |
3.0 |
2.7 |
4.1 |
0.0 |
0.3 |
0.3 |
1.0 |
2.2 |
2.6 |
2.9 |
4.3 |
||
Mean |
0.0 |
0.3 |
0.4 |
1.6 |
2.2 |
2.8 |
2.8 |
4.2 |
|
~16.48 mins |
A B |
0.0 0.0 |
0.3 0.2 |
0.3 0.3 |
1.7 1.9 |
1.9 1.9 |
2.0 2.7 |
2.2 2.6 |
1.1 0.9 |
Mean |
0.0 |
0.3 |
0.3 |
1.8 |
1.9 |
2.4 |
2.4 |
1.0 |
|
Total of remaining peaks each < 2% of applied |
A B |
0.0 |
0.2 |
0.2 |
0.2 |
0.3 |
0.3 |
0.4 |
0.6 |
0.0 |
0.2 |
0.2 |
0.2 |
0.3 |
0.4 |
0.4 |
0.7 |
||
Mean |
0.0 |
0.2 |
0.2 |
0.2 |
0.3 |
0.4 |
0.4 |
0.7 |
|
Table 9. Summary of product distribution in extracts of Pappelacker soil (values as % of applied).
Retention time (Co-chromatographs with) |
Replicate |
Incubation time (days after treatment, DAT) |
|||||||
0 |
7 |
14 |
29 |
43 |
61 |
90 |
120 |
||
~24.30 mins (Parent) |
A B |
96.8 96.7 |
92.7 95.5 |
97.0 97.1 |
93.6 93.6 |
89.6 89.7 |
86.2 86.5 |
82.5 81.2 |
78.2 74.3 |
Mean |
96.8 |
94.1 |
97.1 |
93.6 |
89.7 |
86.4 |
81.9 |
76.3 |
|
~18.18 mins |
A B |
0 |
0.4 |
0.6 |
1.3 |
4.1 |
6.2 |
7.5 |
8.7 |
(M1+M2) |
0 |
0.3 |
0.6 |
3.0 |
4.1 |
5.6 |
8.0 |
9.7 |
|
Mean |
0.0 |
0.4 |
0.6 |
2.2 |
4.1 |
5.9 |
7.8 |
9.2 |
|
~16.12-16.24 mins |
A B |
0.0 0.0 |
0.2 0.2 |
0.3 0.3 |
0.4 0.4 |
0.6 0.6 |
0.9 0.9 |
0.8 0.9 |
2.6 1.7 |
Mean |
0.0 |
0.2 |
0.3 |
0.4 |
0.6 |
0.9 |
0.9 |
2.2 |
|
Total of remaining peaks each < 2% of applied |
A |
0.0 |
0.4 |
0.6 |
1.6 |
2.2 |
2.6 |
3.0 |
3.9 |
B |
0.0 |
0.2 |
0.5 |
1.7 |
2.2 |
3.5 |
4.6 |
4.9 |
|
Mean |
0.0 |
0.3 |
0.6 |
1.7 |
2.2 |
3.1 |
3.8 |
4.4 |
|
Table 10. Summary of product distribution in extracts of Gartenacker soil (values as % of applied).
Retention time (Co- chromatographs with) |
Replicate |
Incubation time (days after treatment, DAT) |
||||||||||
0 |
7 |
14 |
29 |
43 |
61 |
90 |
120 |
180 |
279 |
369 |
||
~24.30 mins (Parent) |
A B |
96.7 96.7 |
95.1 93.5 |
94.4 93.8 |
86.0 84.9 |
79.1 74.3 |
70.2 70.8 |
55.1 56.7 |
48.5 44.9 |
33.7 32.6 |
21.9 21.1 |
17.5 16.8 |
Mean |
96.7 |
94.1 |
94.1 |
85.5 |
76.7 |
70.5 |
55.9 |
46.7 |
33.2 |
21.5 |
17.2 |
|
~19.36 mins |
A B |
0.0 0.0 |
0.0 0.0 |
0.1 0.1 |
1.4 0.9 |
1.3 1.0 |
1.5 1.8 |
2.2 2.0 |
1.4 1.9 |
2.0 1.9 |
1.8 1.9 |
1.9 1.7 |
Mean |
0.0 |
0.0 |
0.1 |
1.2 |
1.2 |
1.7 |
2.1 |
1.7 |
2.0 |
1.9 |
1.8 |
|
~18.18 mins (M1+M2) |
A B |
0.0 0.0 |
0.6 0.7 |
2.6 2.5 |
6.4 7.3 |
8.4 10.9 |
12.7 11.2 |
16.1 16.3 |
16.5 17.6 |
20.0 19.2 |
17.2 16.8 |
16.5 15.1 |
Mean |
0.0 |
0.7 |
2.6 |
6.9 |
9.7 |
12.0 |
16.2 |
17.1 |
19.6 |
17.0 |
15.8 |
|
~16.48 mins |
A B |
0.0 0.0 |
0.3 0.2 |
0.4 0.4 |
0.5 0.6 |
0.6 0.7 |
0.8 0.6 |
2.6 2.0 |
1.7 2.2 |
2.7 3.5 |
3.1 3.2 |
2.7 3.3 |
Mean |
0.0 |
0.3 |
0.4 |
0.6 |
0.7 |
0.7 |
2.3 |
2.0 |
3.1 |
3.2 |
3.0 |
|
~16.12-16.24 mins |
A B |
0.0 0.0 |
0.3 0.4 |
0.3 0.3 |
0.6 0.6 |
0.9 1.8 |
1.1 1.0 |
3.3 3.3 |
3.8 3.7 |
3.9 3.7 |
3.9 2.8 |
3.1 2.5 |
Mean |
0.0 |
0.4 |
0.3 |
0.6 |
1.4 |
1.1 |
3.3 |
3.8 |
3.8 |
3.4 |
2.8 |
|
~13.48-14.30 mins |
A B |
0.0 0.0 |
0.0 0.0 |
0.2 0.2 |
0.6 0.7 |
0.9 2.0 |
2.9 3.3 |
3.1 2.1 |
2.8 3.2 |
3.0 2.5 |
3.2 3.4 |
2.5 1.9 |
Mean |
0.0 |
0.0 |
0.2 |
0.7 |
1.5 |
3.1 |
2.6 |
3.0 |
2.8 |
3.3 |
2.2 |
|
~13.06-13.24 mins |
A B |
0.0 0.0 |
0.0 0.0 |
0.1 0.1 |
0.3 0.3 |
0.5 0.5 |
0.5 0.4 |
0.5 0.6 |
0.9 1.3 |
1.7 2.4 |
2.2 1.7 |
1.2 2.3 |
Mean |
0.0 |
0.0 |
0.1 |
0.3 |
0.5 |
0.5 |
0.6 |
1.1 |
2.1 |
2.0 |
1.8 |
|
Total of remaining peaks each < 2% of applied |
A B |
0.0 0.0 |
0.0 0.0 |
0.5 0.4 |
1.1 1.3 |
1.6 1.8 |
1.8 1.7 |
3.4 3.6 |
4.4 5.1 |
5.0 5.7 |
6.3 7.0 |
7.5 8.9 |
Mean |
0.0 |
0.0 |
0.5 |
1.2 |
1.7 |
1.8 |
3.5 |
4.8 |
5.4 |
6.7 |
8.2 |
|
Table 11. Summary of product distribution in extracts of Marsillargues soil (values as % of applied).
Retention time (Co-chromatographs with) |
Replicate |
Incubation time (days after treatment, DAT) |
|||||||
0 |
7 |
14 |
30 |
44 |
58 |
90 |
120 |
||
~24.30 mins (Parent) |
A B |
91.5 92.8 |
89.6 87.8 |
88.6 85.6 |
83.3 80.9 |
78.5 80.8 |
80.6 78.8 |
70.8 65.5 |
64.5 63.2 |
Mean |
92.2 |
88.7 |
87.1 |
82.1 |
80.0 |
79.7 |
68.2 |
63.9 |
|
~18.18 mins (M1+M2) |
A B |
0.0 |
0.4 |
1.9 |
4.6 |
7.8 |
9.7 |
14.8 |
16.9 |
0.0 |
0.4 |
0.9 |
4.4 |
7.3 |
9.5 |
15.5 |
18.0 |
||
Mean |
0.0 |
0.4 |
1.4 |
4.5 |
7.6 |
9.6 |
15.2 |
17.5 |
|
~16.48 mins |
A B |
0.0 0.0 |
0.4 0.5 |
0.6 0.6 |
1.0 1.8 |
2.1 1.6 |
1.0 1.0 |
2.3 3.1 |
3.0 3.4 |
Mean |
0.0 |
0.5 |
0.6 |
1.4 |
1.9 |
1.0 |
2.7 |
3.2 |
|
Total of remaining peaks each < 2% of applied |
A B |
0.8 |
0.4 |
0.9 |
1.2 |
2.2 |
2.5 |
8.1 |
6.3 |
0.9 |
0.4 |
0.7 |
1.4 |
1.8 |
3.3 |
6.5 |
5.5 |
||
Mean |
0.9 |
0.4 |
0.8 |
1.3 |
2.0 |
2.9 |
7.3 |
5.9 |
|
Table 3. Mass Balance and distribution of radioactivity in extracts– individual replicates (values expressed as % of applied)
Fraction |
Rep. |
Sampling Interval (Days after Treatment) |
|||||||||||
0 |
7 |
14 |
30 |
45 |
60 |
90 |
120 |
150 |
180 |
210 |
360 |
||
Extraction 1 |
1 |
1.93 |
5.41 |
8.16 |
10.67 |
12.48 |
11.24 |
12.49 |
12.54 |
11.73 |
11.57 |
11.38 |
7.26 |
2 |
1.94 |
5.62 |
8.19 |
11.23 |
12.14 |
11.36 |
12.26 |
12.28 |
11.78 |
11.55 |
10.58 |
5.73 |
|
Extraction 2 |
1 |
0.80 |
4.16 |
5.73 |
7.39 |
7.87 |
8.20 |
8.29 |
7.23 |
6.47 |
6.30 |
5.79 |
3.69 |
2 |
0.76 |
4.33 |
5.75 |
7.56 |
7.67 |
8.48 |
8.18 |
7.27 |
6.56 |
5.99 |
5.55 |
3.16 |
|
Extraction 3 |
1 |
60.25 |
61.86 |
54.11 |
44.85 |
44.17 |
33.29 |
28.77 |
25.44 |
21.35 |
17.46 |
17.70 |
9.29 |
2 |
61.68 |
55.53 |
56.26 |
42.58 |
46.44 |
34.28 |
30.49 |
27.41 |
20.19 |
18.02 |
15.83 |
8.22 |
|
Extraction 4 (ASE) |
1 |
30.51 |
24.11 |
25.35 |
22.73 |
21.24 |
23.98 |
21.68 |
19.61 |
16.34 |
15.95 |
15.87 |
11.31 |
2 |
29.00 |
27.55 |
24.83 |
25.90 |
17.90 |
24.15 |
21.65 |
17.30 |
17.78 |
14.84 |
15.89 |
10.12 |
|
Total Extractabl e |
Mean |
93.44 |
94.29 |
94.19 |
86.46 |
84.96 |
77.49 |
71.91 |
64.54 |
56.10 |
50.84 |
49.30 |
29.39 |
Un- extractable |
1 |
<LOQ |
0.92 |
1.89 |
7.14 |
17.08 |
18.13 |
20.89 |
24.68 |
31.03 |
31.91 |
32.19 |
57.66 |
2 |
0.54 |
2.06 |
2.25 |
7.24 |
15.79 |
16.56 |
19.46 |
26.71 |
28.36 |
32.76 |
33.56 |
58.87 |
|
14CO2 |
1 |
- |
<LO Q |
0.06 |
0.36 |
0.71 |
1.92 |
4.62 |
4.30 |
8.75 |
9.99 |
11.62 |
22.05 |
2 |
- |
<LO Q |
0.06 |
0.44 |
0.89 |
1.97 |
4.34 |
2.20 |
8.84 |
10.53 |
12.29 |
23.27 |
|
TOTAL |
1 |
93.49 |
96.46 |
95.30 |
93.14 |
103.55 |
96.76 |
96.74 |
93.80 |
95.67 |
93.18 |
94.55 |
111.26 |
2 |
93.92 |
95.09 |
97.34 |
94.95 |
100.83 |
96.80 |
96.38 |
93.17 |
93.51 |
93.69 |
93.70 |
109.37 |
|
Mean ± SD |
96.8 ± 5.0% |
||||||||||||
<LOQ = sample recoveries below the level of quantification (liquid samples LOQ = 46 dpm above background, combustion samples LOQ = 53 dpm above background)
- = no sample
Table 4: Summary of product distribution in CaCl2 and solvent extracts (resultscombined and expressed as % of applied radioactivity)
Sampling Interval |
Rep. No./ Inj. No. |
Component as % Applied Radioactivity |
|||||
Anti-isomer test item |
Syn isomer test item |
Total test item |
M1 |
M3 |
Unidentified Radioactivity |
||
Day 0 |
1/1 1/2 |
26.63 27.39 |
66.86 66.10 |
93.49 93.49 |
nd nd |
0.00 0.00 |
0.00 0.00 |
2/1 2/2 |
27.83 26.88 |
65.55 66.50 |
93.38 93.38 |
nd nd |
0.00 0.00 |
0.00 0.00 |
|
Mean |
27.18 |
66.25 |
93.43 |
nd |
0.00 |
0.00 |
|
Day 7 |
1/1 1/2 |
18.49 19.37 |
61.31 61.07 |
79.80 80.44 |
4.87 4.36 |
0.00 0.00 |
10.88 10.75 |
2/1 2/2 |
17.84 17.85 |
57.13 57.86 |
74.97 75.71 |
4.84 5.00 |
0.00 0.00 |
13.22 12.33 |
|
Mean |
18.39 |
59.34 |
77.73 |
4.77 |
0.00 |
11.80 |
|
Day 14 |
1/1 1/2 |
14.99 14.15 |
49.87 52.01 |
64.86 66.16 |
12.99 10.50 |
0.93 0.46 |
14.55 16.25 |
2/1 2/2 |
14.84 14.64 |
54.07 54.09 |
68.91 68.73 |
11.02 10.93 |
0.87 0.00 |
14.23 15.39 |
|
Mean |
14.66 |
52.52 |
67.18 |
11.36 |
0.57 |
15.11 |
|
Day 30 |
1/1 1/2 |
9.02 10.22 |
36.50 35.06 |
45.52 45.28 |
18.52 16.01 |
2.69 4.88 |
18.90 19.86 |
2/1 2/2 |
9.69 10.07 |
34.33 34.35 |
44.02 44.42 |
19.74 18.72 |
3.35 3.51 |
20.15 20.60 |
|
Mean |
9.75 |
35.07 |
44.82 |
18.25 |
3.61 |
19.89 |
|
Day 45 |
1/1 1/2 |
8.33 7.97 |
29.54 31.00 |
37.87 38.97 |
23.59 22.59 |
3.62 3.55 |
20.69 20.64 |
2/1 2/2 |
7.47 7.68 |
30.08 28.60 |
37.55 36.28 |
21.60 21.43 |
3.28 4.23 |
21.72 22.22 |
|
Mean |
7.86 |
29.81 |
37.67 |
22.31 |
3.67 |
21.33 |
|
Day 60 |
1/1 1/2 |
5.33 5.66 |
21.52 20.46 |
26.85 26.12 |
19.14 18.16 |
5.07 5.01 |
25.67 27.43 |
2/1 2/2 |
5.58 6.28 |
20.74 21.45 |
26.32 27.73 |
21.07 20.91 |
5.09 5.66 |
25.32 23.52 |
|
Mean |
5.71 |
21.04 |
26.75 |
19.82 |
5.21 |
25.56 |
|
Day 90 |
1/1 |
3.52 |
18.97 |
22.49 |
17.32 |
8.20 |
23.21 |
1/2 |
4.41 |
16.63 |
21.04 |
16.94 |
9.55 |
23.71 |
|
2/1 |
4.06 |
17.86 |
21.92 |
15.00 |
9.25 |
26.41 |
|
2/2 |
4.79 |
16.93 |
21.72 |
15.69 |
9.19 |
25.98 |
|
Mean |
4.20 |
17.60 |
21.80 |
16.24 |
9.06 |
24.85 |
|
Day 120 |
1/1 1/2 |
2.81 3.01 |
11.60 12.97 |
14.41 15.98 |
11.73 12.02 |
9.96 8.97 |
28.74 27.85 |
2/1 2/2 |
3.15 3.16 |
12.58 12.02 |
15.73 15.18 |
13.46 12.26 |
9.10 8.89 |
25.52 27.29 |
|
Mean |
3.03 |
12.29 |
15.33 |
12.37 |
9.23 |
27.39 |
|
Day 150 |
1/1 1/2 |
2.58 3.02 |
10.84 10.75 |
13.42 13.77 |
9.99 9.03 |
10.34 11.84 |
20.23 21.25 |
2/1 2/2 |
1.71 2.94 |
10.56 9.75 |
12.27 12.69 |
8.82 7.66 |
11.04 12.80 |
24.19 23.16 |
|
Mean |
2.56 |
10.48 |
13.04 |
8.88 |
11.50 |
22.23 |
|
Day 180 |
1/1 1/2 |
1.61 1.73 |
8.15 8.37 |
9.76 10.10 |
5.62 5.83 |
9.11 9.16 |
26.77 26.19 |
2/1 2/2 |
1.92 1.36 |
6.50 7.61 |
8.42 8.97 |
6.35 5.42 |
9.05 9.30 |
26.58 26.72 |
|
Mean |
1.66 |
7.66 |
9.32 |
5.81 |
9.17 |
26.59 |
|
Day 210 |
1/1 1/2 |
1.30 1.45 |
7.08 7.64 |
8.38 9.09 |
6.39 6.46 |
5.81 5.89 |
30.17 29.31 |
2/1 2/2 |
1.39 0.87 |
7.11 5.98 |
8.50 6.85 |
4.95 4.85 |
8.09 7.09 |
26.32 29.00 |
|
Mean |
1.25 |
6.96 |
8.21 |
5.67 |
6.72 |
28.76 |
|
Day 360 |
1/1 1/2 |
0.52 0.37 |
2.29 2.68 |
2.81 3.05 |
2.63 2.68 |
4.99 5.99 |
20.63 19.50 |
2/1 2/2 |
0.38 0.67 |
1.87 1.63 |
2.25 2.30 |
1.94 1.36 |
4.78 5.74 |
17.76 17.33 |
|
Mean |
0.49 |
2.12 |
2.61 |
2.16 |
5.38 |
18.86 |
|
Table 2. Distribution and Recovery of Radioactivity in Soil I (18-Acres, Sandy Clay Loam), Values in percent of applied radioactivity
Soil I (18 Acres) |
Sample |
Incubation time (days) |
||||||
% of applied radioactivity |
0 |
7 |
14 |
27 |
56 |
90 |
123 |
|
Extraction with CaCl2 solution1) |
A |
1.4 |
2.1 |
2.8 |
3.2 |
3.6 |
3.4 |
3.2 |
B |
1.5 |
2.1 |
2.9 |
3.2 |
3.5 |
3.5 |
3.1 |
|
mean |
1.4 |
2.1 |
2.9 |
3.2 |
3.5 |
3.5 |
3.2 |
|
Extraction with acetonitrile/water1) |
A |
95.0 |
93.3 |
92.8 |
72.4 |
67.8 |
68.4 |
67.7 |
B |
97.6 |
93.6 |
90.3 |
74.4 |
67.1 |
68.2 |
74.7 |
|
mean |
96.3 |
93.5 |
91.5 |
73.4 |
67.5 |
68.3 |
71.2 |
|
Reflux 2) |
A |
n.p. |
n.p. |
5.4 |
21.5 |
24.7 |
26.6 |
25.9 |
B |
n.p. |
n.p. |
6.7 |
19.3 |
25.2 |
25.6 |
20.1 |
|
mean |
n.p. |
n.p. |
6.1 |
20.4 |
25.0 |
26.1 |
23.0 |
|
Total extractables from soil |
A |
96.5 |
95.4 |
101.1 |
97.1 |
96.1 |
98.5 |
96.8 |
B |
99.0 |
95.7 |
99.9 |
96.8 |
95.8 |
97.3 |
97.9 |
|
mean |
97.7 |
95.5 |
100.5 |
96.9 |
96.0 |
97.9 |
97.3 |
|
Non-Extractables |
A |
6.0 |
5.5 |
0.8 |
5.2 |
5.7 |
5.6 |
5.5 |
B |
4.8 |
5.3 |
1.1 |
4.7 |
5.6 |
5.2 |
4.5 |
|
mean |
5.4 |
5.4 |
1.0 |
5.0 |
5.7 |
5.4 |
5.0 |
|
14CO2 |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.6 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.1 |
<0.1 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.3 |
|
Other Volatiles in EG |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Total |
A |
102.4 |
100.9 |
101.9 |
102.3 |
101.9 |
104.1 |
103.0 |
B |
103.8 |
101.0 |
101.0 |
101.5 |
101.5 |
102.6 |
102.4 |
|
mean |
103.1 |
101.0 |
101.5 |
101.9 |
101.7 |
103.3 |
102.7 |
|
MEAN +/- SD |
|
|
102.2 |
± |
0.9 |
|
|
|
1) Gentle extraction at room temperature using 0.01 M CaCl2solution (once) followed by extraction with acetonitrile/water (4:1; v/v), three or four times.
2) Extraction under reflux using acetonitrile/water (4:1; v/v) for two hours EG Ethylene glycol
n.p. Not performed
SD Standard deviation
Table 3. Distribution and Recovery of Radioactivity in Soil II (Gartenacker, Sandy Loam) Values in percent of applied radioactivity
Soil II (Gartenacker) |
Sample |
Incubation time (days) |
|||||||||
% of applied radioactivity |
0 |
7 |
14 |
27 |
56 |
90 |
123 |
195 |
271 |
361 |
|
Extraction with CaCl2 solution1) |
A |
3.7 |
4.4 |
6.1 |
9.6 |
16.2 |
20.1 |
20.5 |
20.1 |
20.0 |
18.1 |
B |
3.6 |
4.5 |
6.2 |
10.0 |
16.1 |
19.7 |
20.6 |
20.8 |
19.3 |
17.8 |
|
mean |
3.7 |
4.4 |
6.2 |
9.8 |
16.2 |
19.9 |
20.6 |
20.4 |
19.7 |
18.0 |
|
Extraction with acetonitrile/ water1) |
A |
93.2 |
91.7 |
87.6 |
83.2 |
73.0 |
64.9 |
61.4 |
52.2 |
45.3 |
41.9 |
B |
94.7 |
91.5 |
88.0 |
85.1 |
72.7 |
65.8 |
60.9 |
53.2 |
45.9 |
41.3 |
|
mean |
93.9 |
91.6 |
87.8 |
84.1 |
72.8 |
65.3 |
61.2 |
52.7 |
45.6 |
41.6 |
|
Reflux 2) |
A |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
7.0 |
8.6 |
8.3 |
7.4 |
B |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
7.2 |
8.7 |
8.3 |
7.9 |
|
mean |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
7.1 |
8.7 |
8.3 |
7.7 |
|
Total extractables from soil |
A |
96.9 |
96.1 |
93.7 |
92.8 |
89.2 |
85.0 |
89.0 |
80.9 |
73.6 |
67.5 |
B |
98.3 |
95.9 |
94.3 |
95.1 |
88.8 |
85.5 |
88.7 |
82.6 |
73.6 |
67.0 |
|
mean |
97.6 |
96.0 |
94.0 |
93.9 |
89.0 |
85.2 |
88.8 |
81.8 |
73.6 |
67.3 |
|
Non-Extractables |
A |
2.0 |
4.8 |
5.2 |
5.8 |
9.2 |
12.8 |
9.7 |
14.2 |
20.9 |
22.8 |
B |
2.0 |
4.8 |
5.3 |
6.3 |
9.0 |
12.5 |
9.9 |
13.9 |
20.4 |
23.3 |
|
mean |
2.0 |
4.8 |
5.2 |
6.1 |
9.1 |
12.7 |
9.8 |
14.1 |
20.6 |
23.1 |
|
14CO2 |
A |
n.p. |
<0.1 |
<0.1 |
0.1 |
0.2 |
0.8 |
1.2 |
0.4 |
1.7 |
1.3 |
B |
n.p. |
<0.1 |
0.1 |
0.2 |
0.3 |
0.6 |
0.6 |
1.2 |
2.1 |
1.7 |
|
mean |
n.p. |
<0.1 |
<0.1 |
0.1 |
0.2 |
0.7 |
0.9 |
0.8 |
1.9 |
1.5 |
|
Other Volatiles in EG |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Total |
A |
98.9 |
100.9 |
98.9 |
98.6 |
98.5 |
98.6 |
99.9 |
95.5 |
96.1 |
91.6 |
B |
100.3 |
100.8 |
99.6 |
101.6 |
98.1 |
98.6 |
99.2 |
97.8 |
96.1 |
92.1 |
|
mean |
99.6 |
100.9 |
99.3 |
100.1 |
98.3 |
98.6 |
99.6 |
96.7 |
96.1 |
91.9 |
|
MEAN +/- SD |
|
|
|
98.1 |
± |
2.6 |
|
|
|
|
|
1) Extraction at room temperature using 0.01 M CaCl2solution (once) followed by acetonitrile/water (4:1; v/v), three or four times.
2) Extraction under reflux using acetonitrile/water (4:1; v/v) for two hours EG Ethylene glycol
n.p. Not performed
SD Standard deviation
Table 4 Distribution and Recovery of Radioactivity in Soil III (Marsillargues, Silty Clay Loam) Values in percent of applied radioactivity
Soil III (Marsillargues) |
Sample |
Incubation time (days) |
||||||
% of applied radioactivity |
0 |
7 |
14 |
27 |
56 |
90 |
123 |
|
Extraction with CaCl2 solution1) |
A |
5.4 |
7.0 |
8.4 |
11.0 |
14.3 |
17.0 |
17.8 |
B |
5.3 |
7.1 |
8.8 |
10.7 |
13.7 |
16.3 |
18.0 |
|
mean |
5.3 |
7.0 |
8.6 |
10.9 |
14.0 |
16.6 |
17.9 |
|
Extraction with acetonitrile/water1) |
A |
96.8 |
95.3 |
89.1 |
70.7 |
62.8 |
67.8 |
66.0 |
B |
97.4 |
93.0 |
93.1 |
75.0 |
72.5 |
65.8 |
66.7 |
|
mean |
97.1 |
94.1 |
91.1 |
72.8 |
67.7 |
66.8 |
66.3 |
|
Reflux 2) |
A |
n.p. |
n.p. |
n.p. |
18.1 |
20.3 |
15.0 |
13.9 |
B |
n.p. |
n.p. |
n.p. |
15.1 |
13.3 |
13.7 |
11.5 |
|
mean |
n.p. |
n.p. |
n.p. |
16.6 |
16.8 |
14.3 |
12.7 |
|
Total extractables from soil |
A |
102.2 |
102.3 |
97.5 |
99.8 |
97.4 |
99.7 |
97.7 |
B |
102.8 |
100.0 |
101.8 |
100.8 |
99.5 |
95.8 |
96.2 |
|
mean |
102.5 |
101.2 |
99.6 |
100.3 |
98.4 |
97.7 |
96.9 |
|
Non-Extractables |
A |
4.1 |
3.4 |
4.4 |
3.9 |
4.6 |
5.3 |
6.4 |
B |
1.1 |
2.7 |
4.5 |
3.4 |
3.5 |
5.1 |
6.0 |
|
mean |
2.6 |
3.0 |
4.4 |
3.7 |
4.0 |
5.2 |
6.2 |
|
14CO2 |
A |
n.p. |
<0.1 |
<0.1 |
0.1 |
0.2 |
0.3 |
0.8 |
B |
n.p. |
<0.1 |
0.1 |
0.1 |
0.2 |
0.4 |
0.6 |
|
mean |
n.p. |
<0.1 |
0.1 |
0.1 |
0.2 |
0.3 |
0.7 |
|
Other Volatiles in EG |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Total |
A |
106.3 |
105.7 |
101.9 |
103.8 |
102.2 |
105.2 |
104.8 |
B |
103.9 |
102.8 |
106.4 |
104.3 |
103.1 |
101.3 |
102.8 |
|
mean |
105.1 |
104.2 |
104.1 |
104.1 |
102.7 |
103.3 |
103.8 |
|
MEAN +/- SD |
|
|
103.9 |
± |
0.8 |
|
|
|
1) Extraction at room temperature using 0.01 M CaCl2solution (once) followed by acetonitrile/water (4:1; v/v), three or four times.
2) Extraction under reflux using acetonitrile/water (4:1; v/v) for two hours EG Ethylene glycol
n.p. Not performed
SD Standard deviation
Table 5. Distribution and Recovery of Radioactivity in Soil IV (Pappelacker, Sandy Loam) Values in percent of applied radioactivity
Soil IV (Pappelacker) |
Sample |
Incubation time (days) |
||||||
% of applied radioactivity |
0 |
7 |
14 |
27 |
56 |
90 |
123 |
|
Extraction with CaCl2 solution1) |
A |
3.7 |
3.8 |
4.6 |
6.3 |
10.0 |
13.8 |
14.9 |
B |
3.8 |
3.9 |
4.7 |
6.3 |
10.3 |
13.5 |
14.5 |
|
mean |
3.8 |
3.8 |
4.6 |
6.3 |
10.2 |
13.7 |
14.7 |
|
Extraction with acetonitrile/water1) |
A |
95.9 |
93.6 |
90.6 |
90.4 |
85.5 |
82.0 |
74.9 |
B |
94.7 |
93.4 |
87.2 |
90.1 |
86.4 |
79.2 |
77.2 |
|
mean |
95.3 |
93.5 |
88.9 |
90.3 |
86.0 |
80.6 |
76.1 |
|
Reflux 2) |
A |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
5.7 |
B |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
5.7 |
|
mean |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
5.7 |
|
Total extractables from soil |
A |
99.6 |
97.5 |
95.2 |
96.8 |
95.5 |
95.9 |
95.6 |
B |
98.5 |
97.2 |
91.9 |
96.4 |
96.8 |
92.7 |
97.4 |
|
mean |
99.1 |
97.4 |
93.5 |
96.6 |
96.1 |
94.3 |
96.5 |
|
Non-Extractables |
A |
1.4 |
3.5 |
3.9 |
5.5 |
6.3 |
8.5 |
4.9 |
B |
1.5 |
3.4 |
3.6 |
5.3 |
6.2 |
8.3 |
4.6 |
|
mean |
1.4 |
3.5 |
3.7 |
5.4 |
6.2 |
8.4 |
4.8 |
|
14CO2 |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
0.2 |
0.2 |
0.2 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.2 |
0.2 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.2 |
0.2 |
|
Other Volatiles in EG |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Total |
A |
101.0 |
101.0 |
99.1 |
102.3 |
102.0 |
104.5 |
100.7 |
B |
100.0 |
100.7 |
95.5 |
101.8 |
103.0 |
101.2 |
102.2 |
|
mean |
100.5 |
100.8 |
97.3 |
102.1 |
102.5 |
102.9 |
101.5 |
|
MEAN +/- SD |
|
|
101.1 |
± |
1.9 |
|
|
|
1) Extraction at room temperature using 0.01 M CaCl2solution (once) followed by acetonitrile/water (4:1; v/v), three or four times.
2) Extraction under reflux using acetonitrile/water (4:1; v/v) for two hours EG Ethylene glycol
n.p. Not performed
SD Standard deviation
Table 6. Amount of 14C-test item in the Soil Extracts of Soils I and II, Values in percent of applied radioactivity
Soil |
Distribution of test item % of applied radioactivity |
Sample |
Incubation time (days) |
361 |
||||||||
0 |
7 |
14 |
27 |
56 |
90 |
123 |
195 |
271 |
||||
Soil I (18 Acres) |
Test item in extractables 1) |
A |
95.0 |
92.9 |
91.2 |
71.2 |
65.2 |
65.5 |
63.8 |
- |
- |
- |
B |
98.7 |
93.3 |
88.7 |
72.9 |
64.9 |
65.6 |
69.2 |
- |
- |
- |
||
mean |
96.9 |
93.1 |
89.9 |
72.1 |
65.1 |
65.5 |
66.5 |
- |
- |
- |
||
Test item in reflux extract 2) |
A |
n.p. |
n.p. |
5.3 |
20.7 |
23.4 |
25.0 |
24.0 |
- |
- |
- |
|
B |
n.p. |
n.p. |
6.5 |
18.5 |
23.9 |
24.1 |
18.3 |
- |
- |
- |
||
mean |
n.p. |
n.p. |
5.9 |
19.6 |
23.6 |
24.6 |
21.1 |
- |
- |
- |
||
Total SYN520453 |
A |
95.0 |
92.9 |
96.5 |
91.9 |
88.5 |
90.5 |
87.8 |
- |
- |
- |
|
B |
98.7 |
93.3 |
95.1 |
91.4 |
88.8 |
89.7 |
87.5 |
- |
- |
- |
||
mean |
96.9 |
93.1 |
95.8 |
91.6 |
88.7 |
90.1 |
87.6 |
- |
- |
- |
||
Soil II (Gartenacker) |
Test item in extractables 1) |
A |
93.4 |
93.5 |
87.5 |
79.9 |
62.6 |
49.3 |
45.2 |
31.6 |
24.7 |
21.6 |
B |
98.2 |
93.4 |
88.0 |
82.5 |
62.2 |
50.0 |
41.9 |
32.5 |
24.4 |
19.3 |
||
mean |
95.8 |
93.4 |
87.7 |
81.2 |
62.4 |
49.6 |
43.6 |
32.0 |
24.5 |
20.5 |
||
Test item in reflux extract 2) |
A |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
4.9 |
5.0 |
4.3 |
3.7 |
|
B |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
4.7 |
5.1 |
4.2 |
3.6 |
||
mean |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
4.8 |
5.0 |
4.2 |
3.7 |
||
Total test item |
A |
93.4 |
93.5 |
87.5 |
79.9 |
62.6 |
49.3 |
50.2 |
36.6 |
29.0 |
25.3 |
|
B |
98.2 |
93.4 |
88.0 |
82.5 |
62.2 |
50.0 |
46.7 |
37.5 |
28.5 |
22.9 |
||
mean |
95.8 |
93.4 |
87.7 |
81.2 |
62.4 |
49.6 |
48.4 |
37.1 |
28.8 |
24.1 |
||
1) Extraction at room temperature using 0.01 M CaCl2solution (once) followed by acetonitrile/water (4:1; v/v), three or four times.
2) Extraction under reflux using acetonitrile/water (4:1; v/v) for two hours
- Not applicable
Table 7. Amount of14C-test item in the Soil Extracts of Soils III and IV, Values in percent of applied radioactivity
Soil |
Distribution oftest item |
Sample |
Incubation time (days) |
361 |
||||||||
% of applied radioactivity |
0 |
7 |
14 |
27 |
56 |
90 |
123 |
195 |
271 |
|||
Soil III (Marsillargues) |
Test itemin extractables 1) |
A |
101.9 |
96.9 |
89.0 |
67.9 |
54.9 |
55.7 |
47.9 |
- |
- |
- |
B |
102.6 |
92.7 |
93.6 |
71.8 |
64.5 |
54.8 |
47.8 |
- |
- |
- |
||
mean |
102.3 |
94.8 |
91.3 |
69.8 |
59.7 |
55.2 |
47.8 |
- |
- |
- |
||
Test itemin reflux extract 2) |
A |
n.p. |
n.p. |
n.p. |
16.5 |
17.0 |
11.8 |
9.6 |
- |
- |
- |
|
B |
n.p. |
n.p. |
n.p. |
13.8 |
11.3 |
10.8 |
7.9 |
- |
- |
- |
||
mean |
n.p. |
n.p. |
n.p. |
15.1 |
14.2 |
11.3 |
8.7 |
- |
- |
- |
||
Totaltest item |
A |
101.9 |
96.9 |
89.0 |
84.4 |
71.9 |
67.4 |
57.4 |
- |
- |
- |
|
B |
102.6 |
92.7 |
93.6 |
85.6 |
75.8 |
65.6 |
55.7 |
- |
- |
- |
||
mean |
102.3 |
94.8 |
91.3 |
85.0 |
73.9 |
66.5 |
56.6 |
- |
- |
- |
||
Soil IV (Pappelacker) |
Test itemin extractables 1) |
A |
99.4 |
96.1 |
92.1 |
91.3 |
81.4 |
73.9 |
64.0 |
- |
- |
- |
B |
98.3 |
95.7 |
89.3 |
90.8 |
82.1 |
71.4 |
65.5 |
- |
- |
- |
||
mean |
98.9 |
95.9 |
90.7 |
91.0 |
81.7 |
72.6 |
64.8 |
- |
- |
- |
||
Test itemin reflux extract 2) |
A |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
4.6 |
- |
- |
- |
|
B |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
4.6 |
- |
- |
- |
||
mean |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
n.p. |
4.6 |
- |
- |
- |
||
Totaltest item |
A |
99.4 |
96.1 |
92.1 |
91.3 |
81.4 |
73.9 |
68.7 |
- |
- |
- |
|
B |
98.3 |
95.7 |
89.3 |
90.8 |
82.1 |
71.4 |
70.1 |
- |
- |
- |
||
mean |
98.9 |
95.9 |
90.7 |
91.0 |
81.7 |
72.6 |
69.4 |
- |
- |
- |
||
1) Extraction at room temperature using 0.01 M CaCl2solution (once) followed by acetonitrile/water (4:1; v/v), three or four times.
2) Extraction under reflux using acetonitrile/water (4:1; v/v) for two hours
- Not applicable
Table 8. Characterization of the Gartenacker Soil CaCl2Extract from Soil II using one dimensional TLC, Values in percent of applied radioactivity
Extraction with |
Sample |
|
|
|
INCUBATION TIME IN DAYS |
|
|
|
|||
0.01 M CaCl2 |
0 |
7 |
14 |
27 |
56 |
90 |
123 |
195 |
271 |
361 |
|
Parent |
A |
3.4 |
3.0 |
3.1 |
3.0 |
2.6 |
2.1 |
2.0 |
1.4 |
1.1 |
0.7 |
B |
3.5 |
3.1 |
3.2 |
3.6 |
2.3 |
1.9 |
1.7 |
1.5 |
1.2 |
0.6 |
|
Mean |
3.4 |
3.1 |
3.2 |
3.3 |
2.5 |
2.0 |
1.9 |
1.5 |
1.1 |
0.6 |
|
F1 |
A |
0.2 |
0.3 |
0.3 |
1.0 |
4.9 |
7.0 |
5.4 |
4.0 |
5.6 |
4.1 |
B |
0.1 |
0.2 |
0.3 |
1.1 |
5.2 |
7.2 |
4.8 |
5.2 |
5.2 |
3.1 |
|
Mean |
0.1 |
0.3 |
0.3 |
1.1 |
5.0 |
7.1 |
5.1 |
4.6 |
5.4 |
3.6 |
|
F2 |
A |
* |
* |
* |
* |
2.0 |
1.6 |
1.3 |
1.5 |
1.1 |
1.4 |
B |
* |
0.2 |
* |
* |
2.1 |
1.5 |
1.4 |
1.4 |
1.4 |
1.5 |
|
Mean |
* |
0.1 |
* |
* |
2.1 |
1.6 |
1.3 |
1.5 |
1.2 |
1.4 |
|
F3 |
A |
0.1 |
0.5 |
* |
2.9 |
0.8 |
0.9 |
1.0 |
1.2 |
1.0 |
0.5 |
B |
* |
0.4 |
* |
2.3 |
0.8 |
0.9 |
1.1 |
1.1 |
1.2 |
0.4 |
|
Mean |
0.0 |
0.4 |
* |
2.6 |
0.8 |
0.9 |
1.1 |
1.2 |
1.1 |
0.4 |
|
F4 |
A |
* |
0.2 |
1.3 |
0.4 |
0.5 |
0.3 |
* |
0.5 |
0.7 |
0.9 |
B |
* |
0.1 |
1.1 |
0.5 |
0.6 |
0.4 |
* |
0.5 |
0.5 |
0.9 |
|
Mean |
* |
0.1 |
1.2 |
0.5 |
0.5 |
0.3 |
* |
0.5 |
0.6 |
0.9 |
|
F5 |
A |
* |
* |
0.5 |
* |
* |
* |
* |
0.7 |
1.1 |
1.1 |
B |
* |
* |
0.6 |
0.2 |
* |
* |
* |
0.8 |
1.0 |
1.2 |
|
Mean |
* |
* |
0.5 |
0.1 |
* |
* |
* |
0.7 |
1.0 |
1.2 |
|
F6 (M1) |
A |
0.1 |
0.3 |
0.7 |
2.0 |
4.8 |
7.7 |
10.3 |
10.2 |
9.0 |
7.8 |
B |
0.1 |
0.3 |
0.8 |
1.9 |
4.5 |
7.4 |
11.1 |
9.8 |
8.6 |
8.0 |
|
Mean |
0.1 |
0.3 |
0.8 |
1.9 |
4.6 |
7.5 |
10.7 |
10.0 |
8.8 |
7.9 |
|
F7 |
A |
* |
0.1 |
0.2 |
0.4 |
0.7 |
0.5 |
0.5 |
0.5 |
0.4 |
0.3 |
B |
* |
0.1 |
0.2 |
0.3 |
0.7 |
0.5 |
0.5 |
0.5 |
0.4 |
0.3 |
|
Mean |
* |
0.1 |
0.2 |
0.4 |
0.7 |
0.5 |
0.5 |
0.5 |
0.4 |
0.3 |
|
F8 |
A |
* |
* |
* |
* |
* |
* |
* |
* |
* |
1.0 |
B |
* |
* |
* |
* |
* |
* |
* |
* |
* |
1.2 |
|
Mean |
* |
* |
* |
* |
* |
* |
* |
* |
* |
1.1 |
|
F9 |
A |
* |
* |
* |
* |
* |
* |
* |
* |
* |
0.4 |
B |
* |
* |
* |
* |
* |
* |
* |
* |
* |
0.5 |
|
Mean |
* |
* |
* |
* |
* |
* |
* |
* |
* |
0.5 |
|
TOTAL |
A |
3.7 |
4.4 |
6.1 |
9.6 |
16.2 |
20.1 |
20.5 |
20.1 |
20.0 |
18.1 |
B |
3.6 |
4.5 |
6.2 |
10.0 |
16.1 |
19.7 |
20.6 |
20.8 |
19.3 |
17.8 |
|
F1 corresponds to radioactivity at the origin of the TLC plate
Table 9. Characterization of the Gartenacker Soil Organic Extracts from Soil II using one dimensional TLC, Values in percent of applied radioactivity
org. extracts (% AR) |
Sample |
|
|
|
INCUBATION TIME IN DAYS |
|
|
|
|||
0 |
7 |
14 |
27 |
56 |
90 |
123 |
195 |
271 |
361 |
||
Parent |
A |
90.0 |
90.4 |
84.4 |
77.0 |
60.0 |
47.2 |
48.1 |
35.2 |
27.9 |
22.4 |
B |
94.7 |
90.3 |
84.7 |
79.0 |
59.9 |
48.1 |
45.0 |
36.0 |
27.4 |
24.6 |
|
Mean |
92.4 |
90.3 |
84.6 |
78.0 |
59.9 |
47.6 |
46.6 |
35.6 |
27.6 |
23.5 |
|
F1 |
A |
3.1 |
* |
0.3 |
0.5 |
2.0 |
2.9 |
4.0 |
5.3 |
5.2 |
3.1 |
B |
* |
* |
0.3 |
0.7 |
1.8 |
2.7 |
4.5 |
4.5 |
4.9 |
2.5 |
|
Mean |
1.6 |
* |
0.3 |
0.6 |
1.9 |
2.8 |
4.3 |
4.9 |
5.1 |
2.8 |
|
F2 |
A |
* |
* |
* |
* |
0.2 |
1.0 |
* |
1.1 |
0.9 |
1.8 |
B |
* |
* |
* |
* |
0.2 |
1.0 |
* |
1.3 |
1.0 |
1.2 |
|
Mean |
* |
* |
* |
* |
0.2 |
1.0 |
* |
1.2 |
0.9 |
1.5 |
|
F3 |
A |
* |
* |
* |
* |
1.2 |
0.5 |
1.1 |
0.7 |
0.7 |
0.9 |
B |
* |
* |
* |
* |
1.0 |
0.6 |
1.2 |
0.8 |
0.7 |
0.3 |
|
Mean |
* |
* |
* |
* |
1.1 |
0.5 |
1.1 |
0.8 |
0.7 |
0.6 |
|
F4 |
A |
* |
0.2 |
0.8 |
1.6 |
0.9 |
0.9 |
1.1 |
1.3 |
1.3 |
1.1 |
B |
* |
0.2 |
0.8 |
1.5 |
1.0 |
1.0 |
1.2 |
1.4 |
1.4 |
0.6 |
|
Mean |
* |
0.2 |
0.8 |
1.6 |
1.0 |
0.9 |
1.2 |
1.3 |
1.4 |
0.8 |
|
F5 |
A |
* |
* |
* |
* |
* |
* |
1.0 |
1.2 |
1.8 |
1.0 |
B |
* |
* |
* |
* |
* |
* |
0.7 |
1.5 |
1.9 |
1.0 |
|
Mean |
* |
* |
* |
* |
* |
* |
0.9 |
1.4 |
1.8 |
1.0 |
|
F6 (M1) |
A |
* |
0.4 |
1.1 |
2.4 |
6.5 |
10.1 |
11.0 |
13.6 |
12.8 |
13.3 |
B |
* |
0.4 |
1.2 |
2.6 |
6.6 |
10.3 |
13.1 |
13.7 |
13.5 |
13.3 |
|
Mean |
* |
0.4 |
1.2 |
2.5 |
6.5 |
10.2 |
12.1 |
13.6 |
13.1 |
13.3 |
|
F7 |
A |
* |
0.6 |
1.0 |
1.7 |
2.2 |
2.3 |
2.2 |
2.4 |
1.9 |
1.9 |
B |
* |
0.6 |
1.0 |
1.4 |
2.3 |
2.2 |
2.4 |
2.7 |
2.2 |
2.0 |
|
Mean |
* |
0.6 |
1.0 |
1.6 |
2.3 |
2.2 |
2.3 |
2.6 |
2.0 |
2.0 |
|
M8 |
A |
* |
* |
* |
* |
* |
* |
* |
* |
* |
2.4 |
B |
* |
* |
* |
* |
* |
* |
* |
* |
* |
2.2 |
|
Mean |
* |
* |
* |
* |
* |
* |
* |
* |
* |
2.3 |
|
M9 |
A |
* |
* |
* |
* |
* |
* |
* |
* |
0.3 |
1.4 |
B |
* |
* |
* |
* |
* |
* |
* |
* |
0.3 |
1.5 |
|
Mean |
* |
* |
* |
* |
* |
* |
* |
* |
0.3 |
1.4 |
|
TOTAL |
A |
93.2 |
91.7 |
87.6 |
83.2 |
73.0 |
64.9 |
68.4 |
60.8 |
52.7 |
49.4 |
B |
94.7 |
91.5 |
88.0 |
85.1 |
72.7 |
65.8 |
68.1 |
61.9 |
53.2 |
49.2 |
|
F1 corresponds to radioactivity at the origin of the TLC plate
Table 10. Characterization of the Gartenacker Soil Extracted Radioactivity (Mean Values), Values in percent of applied radioactivity
Soil II |
Incubation Time in Days |
||||||||||
Pattern in total system |
|||||||||||
|
0 |
7 |
14 |
27 |
56 |
90 |
123 |
195 |
271 |
361 |
|
Parent |
0.01M CaCl2 |
3.4 |
3.1 |
3.2 |
3.3 |
2.5 |
2.0 |
1.9 |
1.5 |
1.1 |
0.6 |
org. extr. |
92.4 |
90.3 |
84.6 |
78.0 |
59.9 |
47.6 |
46.6 |
35.6 |
27.6 |
23.5 |
|
Total |
95.8 |
93.4 |
87.7 |
81.2 |
62.4 |
49.6 |
48.4 |
37.1 |
28.8 |
24.1 |
|
F1 |
0.01M CaCl2 |
0.1 |
0.3 |
0.3 |
1.1 |
5.0 |
7.1 |
5.1 |
4.6 |
5.4 |
3.6 |
org. extr. |
1.6 |
* |
0.3 |
0.6 |
1.9 |
2.8 |
4.3 |
4.9 |
5.1 |
2.8 |
|
Total |
1.7 |
0.3 |
0.6 |
1.7 |
6.9 |
9.9 |
9.4 |
9.5 |
10.5 |
6.4 |
|
F2 |
0.01M CaCl2 |
* |
0.1 |
* |
* |
2.1 |
1.6 |
1.3 |
1.5 |
1.2 |
1.4 |
org. extr. |
* |
* |
* |
* |
0.2 |
1.0 |
* |
1.2 |
0.9 |
1.5 |
|
Total |
* |
0.1 |
* |
* |
2.2 |
2.5 |
1.3 |
2.6 |
2.2 |
3.0 |
|
F3 |
0.01M CaCl2 |
<0.1 |
0.4 |
* |
2.6 |
0.8 |
0.9 |
1.1 |
1.2 |
1.1 |
0.4 |
org. extr. |
<0.1 |
* |
* |
* |
1.1 |
0.5 |
1.1 |
0.8 |
0.7 |
0.6 |
|
Total |
<0.1 |
0.4 |
* |
2.6 |
1.9 |
1.4 |
2.2 |
2.0 |
1.8 |
1.0 |
|
F4 |
0.01M CaCl2 |
* |
0.1 |
1.2 |
0.5 |
0.5 |
0.3 |
* |
0.5 |
0.6 |
0.9 |
org. extr. |
* |
0.2 |
0.8 |
1.6 |
1.0 |
0.9 |
1.2 |
1.3 |
1.4 |
0.8 |
|
Total |
* |
0.4 |
2.0 |
2.0 |
1.5 |
1.3 |
1.2 |
1.8 |
2.0 |
1.7 |
|
F5 |
0.01M CaCl2 |
* |
* |
0.5 |
0.1 |
* |
* |
* |
0.7 |
1.0 |
1.2 |
org. extr. |
* |
* |
* |
* |
* |
* |
0.9 |
1.4 |
1.8 |
1.0 |
|
Total |
* |
* |
0.5 |
0.1 |
* |
* |
0.9 |
2.1 |
2.9 |
2.2 |
|
F6 (M1) |
0.01M CaCl2 |
0.1 |
0.3 |
0.8 |
1.9 |
4.6 |
7.5 |
10.7 |
10.0 |
8.8 |
7.9 |
org. extr. |
* |
0.4 |
1.2 |
2.5 |
6.5 |
10.2 |
12.1 |
13.6 |
13.1 |
13.3 |
|
Total |
0.1 |
0.7 |
1.9 |
4.4 |
11.1 |
17.7 |
22.7 |
23.6 |
21.9 |
21.2 |
|
F7 |
0.01M CaCl2 |
* |
0.1 |
0.2 |
0.4 |
0.7 |
0.5 |
0.5 |
0.5 |
0.4 |
0.3 |
org. extr. |
* |
0.6 |
1.0 |
1.6 |
2.3 |
2.2 |
2.3 |
2.6 |
2.0 |
2.0 |
|
Total |
* |
0.7 |
1.2 |
1.9 |
3.0 |
2.8 |
2.8 |
3.1 |
2.4 |
2.3 |
|
F8 |
0.01M CaCl2 |
* |
* |
* |
* |
* |
* |
* |
* |
* |
1.1 |
org. extr. |
* |
* |
* |
* |
* |
* |
* |
* |
* |
2.3 |
|
Total |
* |
* |
* |
* |
* |
* |
* |
* |
* |
3.4 |
|
F9 |
Water |
* |
* |
* |
* |
* |
* |
* |
* |
* |
0.5 |
Extracts |
* |
* |
* |
* |
* |
* |
* |
* |
0.3 |
1.4 |
|
Total |
* |
* |
* |
* |
* |
* |
* |
* |
0.3 |
1.9 |
|
Non- extractables |
mean |
2.0 |
4.8 |
5.2 |
6.1 |
9.1 |
12.7 |
9.8 |
14.1 |
20.6 |
23.1 |
14CO2 |
mean |
n.p. |
<0.1 |
<0.1 |
0.1 |
0.2 |
0.7 |
0.9 |
0.8 |
1.9 |
1.5 |
Other volatiles |
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
TOTAL |
mean |
99.6 |
100.9 |
99.3 |
100.1 |
98.3 |
98.6 |
99.6 |
96.7 |
95.2 |
91.9 |
Org. extr.: Extraction at room temperature and under reflux.
Table 2. Distribution and Recovery of Radioactivity in Soil I (Argissolo, Clay Loam). Values Are Given in Percent of the Applied Radioactivity
14C-labelled test item Soil I (% of applied) |
Sample |
Incubation time (days) |
||||||
0 |
7 |
14 |
28 |
59 |
92 |
120 |
||
Ambient Extractions1) |
A |
97.7 |
96.5 |
95.0 |
93.7 |
90.7 |
83.8 |
89.6 |
B |
101.9 |
96.9 |
96.6 |
95.8 |
91.5 |
84.1 |
87.4 |
|
Mean |
99.8 |
96.7 |
95.8 |
94.8 |
91.1 |
84.0 |
88.5 |
|
Reflux Extraction2) |
A |
n.p. |
5.5 |
4.4 |
4.0 |
5.3 |
10.1 |
7.2 |
B |
n.p. |
5.3 |
4.0 |
4.2 |
5.0 |
9.9 |
6.2 |
|
Mean |
n.p. |
5.4 |
4.2 |
4.1 |
5.1 |
10.0 |
6.7 |
|
Total Extractables |
A |
97.7 |
102.0 |
99.4 |
97.7 |
96.0 |
93.9 |
96.8 |
B |
101.9 |
102.2 |
100.6 |
100.0 |
96.5 |
94.0 |
93.6 |
|
Mean |
99.8 |
102.1 |
100.0 |
98.9 |
96.2 |
93.9 |
95.2 |
|
Non-Extractables |
A |
3.7 |
2.2 |
2.3 |
2.8 |
3.9 |
5.8 |
4.4 |
B |
2.6 |
2.1 |
2.7 |
4.0 |
3.8 |
5.6 |
4.6 |
|
Mean |
3.1 |
2.2 |
2.5 |
3.4 |
3.9 |
5.7 |
4.5 |
|
14CO2 |
A |
n.p. |
0.4 |
0.7 |
1.1 |
1.5 |
1.6 |
2.0 |
B |
n.p. |
0.2 |
0.6 |
1.2 |
1.4 |
1.8 |
1.9 |
|
Mean |
n.p. |
0.3 |
0.7 |
1.2 |
1.5 |
1.7 |
1.9 |
|
Organic Volatiles |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
TOTAL |
A |
101.4 |
104.7 |
102.5 |
101.7 |
101.4 |
101.3 |
103.2 |
B |
104.5 |
104.5 |
104.0 |
105.2 |
101.8 |
101.4 |
100.1 |
|
MEAN ± SD |
102.7 ± 1.6 |
|||||||
1) Extraction at room temperature using acetonitrile/water (4:1; v/v), up to four times
2) Extraction under reflux using acetonitrile/water (4:1; v/v)
n.p. Not performed
SD Standard deviation
Table3. Distribution and Recovery of Radioactivity in Soil II (Latossolo, Clay).Values Are Given in Percent of the Applied Radioactivity
14C-labelled test item Soil II (% of applied) |
Sample |
Incubation time (days) |
||||||
0 |
7 |
14 |
28 |
61 |
90 |
120 |
||
Ambient Extractions1) |
A |
83.5 |
92.1 |
89.1 |
87.6 |
76.0 |
71.5 |
66.6 |
B |
93.3 |
91.9 |
90.8 |
85.0 |
77.7 |
70.8 |
68.4 |
|
mean |
88.4 |
92.0 |
90.0 |
86.3 |
76.9 |
71.2 |
67.5 |
|
Reflux Extraction2) |
A |
n.p. |
n.p. |
n.p. |
6.2 |
12.0 |
12.3 |
13.3 |
B |
n.p. |
n.p. |
n.p. |
6.7 |
10.7 |
12.9 |
13.2 |
|
mean |
n.p. |
n.p. |
n.p. |
6.4 |
11.3 |
12.6 |
13.2 |
|
Total Extractables |
A |
83.5 |
92.1 |
89.1 |
93.8 |
88.1 |
83.8 |
79.9 |
B |
93.3 |
91.9 |
90.8 |
91.7 |
88.4 |
83.7 |
81.5 |
|
mean |
88.4 |
92.0 |
90.0 |
92.7 |
88.2 |
83.8 |
80.7 |
|
Non-Extractables |
A |
15.1 |
6.2 |
10.7 |
3.3 |
9.8 |
12.1 |
13.7 |
B |
8.1 |
6.1 |
8.3 |
4.3 |
9.7 |
12.1 |
13.2 |
|
mean |
11.6 |
6.1 |
9.5 |
3.8 |
9.8 |
12.1 |
13.4 |
|
14CO2 |
A |
n.p. |
0.2 |
0.5 |
0.1 |
1.9 |
2.5 |
3.6 |
B |
n.p. |
0.3 |
0.3 |
0.9 |
2.3 |
3.7 |
2.6 |
|
mean |
n.p. |
0.2 |
0.4 |
0.5 |
2.1 |
3.1 |
3.1 |
|
Organic Volatiles |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
TOTAL |
A |
98.6 |
98.5 |
100.3 |
97.1 |
99.8 |
98.4 |
97.2 |
B |
101.4 |
98.3 |
99.4 |
96.9 |
100.4 |
99.6 |
97.3 |
|
MEAN +/- SD |
98.8 ± 1.4 |
|||||||
1) Extraction at room temperature using acetonitrile/water (4:1; v/v), up to four times
2) Extraction under reflux using acetonitrile/water (4:1; v/v)
n.p. Not performed
SD Standard deviation
Table 4. Distribution and Recovery of Radioactivity in Soil III (Neossolo, Sand).Values Are Given in Percent of the Applied Radioactivity
14C-labelled test item Soil III (% of applied) |
Sample |
INCUBATION TIME IN DAYS |
||||||
0 |
7 |
14 |
28 |
59 |
92 |
120 |
||
Ambient Extractions1) |
A |
101.0 |
101.1 |
100.1 |
100.7 |
94.9 |
89.8 |
92.3 |
B |
104.1 |
101.1 |
99.5 |
95.5 |
96.8 |
91.0 |
93.0 |
|
Mean |
102.5 |
101.1 |
99.8 |
98.1 |
95.8 |
90.4 |
92.6 |
|
Reflux Extraction2) |
A |
n.p. |
0.4 |
2.2 |
2.2 |
5.0 |
4.4 |
7.6 |
B |
n.p. |
0.8 |
2.5 |
1.7 |
5.6 |
6.2 |
6.5 |
|
Mean |
n.p. |
0.6 |
2.3 |
1.9 |
5.3 |
5.3 |
7.1 |
|
Total Extractables |
A |
101.0 |
101.4 |
102.3 |
102.9 |
99.9 |
94.2 |
99.9 |
B |
104.1 |
101.9 |
102.0 |
97.2 |
102.3 |
97.2 |
99.5 |
|
Mean |
102.5 |
101.7 |
102.1 |
100.1 |
101.1 |
95.7 |
99.7 |
|
Non-Extractables |
A |
1.1 |
2.0 |
1.3 |
1.4 |
2.2 |
8.1 |
4.0 |
B |
1.2 |
1.6 |
1.1 |
1.7 |
1.8 |
6.6 |
3.8 |
|
Mean |
1.2 |
1.8 |
1.2 |
1.6 |
2.0 |
7.3 |
3.9 |
|
14CO2 |
A |
n.p. |
<0.1 |
0.2 |
0.3 |
0.6 |
0.6 |
0.6 |
B |
n.p. |
0.1 |
0.2 |
0.3 |
0.5 |
0.6 |
0.7 |
|
Mean |
n.p. |
0.1 |
0.2 |
0.3 |
0.5 |
0.6 |
0.6 |
|
Organic Volatiles |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Mean |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
TOTAL |
A |
102.1 |
103.5 |
103.8 |
104.6 |
102.7 |
102.9 |
104.5 |
B |
105.2 |
103.6 |
103.3 |
99.2 |
104.6 |
104.4 |
104.0 |
|
MEAN ± SD |
103.5 ± 1.5 |
|||||||
1) Extraction at room temperature using acetonitrile/water (4:1; v/v), up to four times
2) Extraction under reflux using acetonitrile/water (4:1; v/v)
n.p. Not performed
SD Standard deviation
Table 5. Pattern of Radioactivity in Soil I (Argissolo, Clay Loam). Values Are Expressed in Percent of the Applied Radioactivity. For the parent substance and M1, the values represent the sum of their amounts in the ambient and reflux extracts. The other factions relate to the ambient extracts since no corresponding peak was recognized in the reflux extract.
14C-labelled test item Soil I (% of applied) |
Sample |
INCUBATION TIME IN DAYS |
||||||||
0 |
7 |
14 |
28 |
59 |
92 |
120 |
||||
Parent |
A |
97.7 |
92.5 |
91.0 |
87.5 |
78.6 |
74.4 |
74.2 |
||
B |
101.9 |
95.3 |
94.8 |
88.6 |
83.2 |
76.7 |
72.5 |
|||
Mean |
99.8 |
93.9 |
92.9 |
88.1 |
80.9 |
75.6 |
73.4 |
|||
ME1 |
A |
* |
* |
1.6 |
2.1 |
1.9 |
2.9 |
3.5 |
||
B |
* |
* |
* |
1.6 |
2.8 |
2.6 |
3.1 |
|||
Mean |
* |
* |
0.8 |
1.9 |
2.4 |
2.8 |
3.3 |
|||
ME2 = M1 |
A |
* |
* |
1.6 |
4.6 |
6.1 |
6.4 |
7.6 |
||
B |
* |
* |
2.1 |
5.5 |
4.1 |
3.7 |
6.3 |
|||
Mean |
* |
* |
1.8 |
5.1 |
5.1 |
5.1 |
6.9 |
|||
ME3 |
A |
* |
1.6 |
1.8 |
* |
4.4 |
4.1 |
3.7 |
||
B |
* |
* |
2.0 |
1.6 |
4.6 |
* |
3.5 |
|||
Mean |
* |
0.8 |
1.9 |
0.8 |
4.5 |
2.0 |
3.6 |
|||
ME5 |
A |
* |
2.4 |
* |
* |
* |
* |
* |
||
B |
* |
* |
* |
* |
* |
* |
* |
|||
Mean |
* |
1.2 |
* |
* |
* |
* |
* |
|||
ME6 |
A |
* |
* |
* |
* |
* |
* |
* |
||
B |
* |
1.6 |
* |
* |
* |
* |
* |
|||
Mean |
* |
0.8 |
* |
* |
* |
* |
* |
|||
ME7 |
A |
* |
* |
1.5 |
1.3 |
1.4 |
* |
* |
||
B |
* |
* |
* |
* |
* |
1.2 |
* |
|||
Mean |
* |
* |
0.7 |
0.7 |
0.7 |
0.6 |
* |
|||
ME8 |
A |
* |
* |
* |
* |
* |
* |
* |
||
B |
* |
* |
* |
1.6 |
* |
* |
* |
|||
Mean |
* |
* |
* |
0.8 |
* |
* |
* |
|||
ME9 |
A |
* |
* |
* |
* |
1.7 |
* |
* |
||
B |
* |
* |
* |
* |
* |
* |
* |
|||
Mean |
* |
* |
* |
* |
0.9 |
* |
* |
|||
ME10 |
A |
* |
* |
* |
* |
* |
* |
* |
||
B |
* |
* |
* |
* |
* |
* |
1.0 |
|||
Mean |
* |
* |
* |
* |
* |
* |
0.5 |
|||
ME11 |
A |
* |
* |
* |
* |
* |
* |
* |
||
B |
* |
* |
* |
* |
* |
3.5 |
* |
|||
Mean |
* |
* |
* |
* |
* |
1.7 |
* |
|||
ME14 |
A |
* |
* |
* |
* |
* |
* |
1.2 |
|
|
B |
* |
* |
* |
* |
* |
* |
1.7 |
|
||
Mean |
* |
* |
* |
* |
* |
* |
1.5 |
|
||
ME16 |
A |
* |
* |
* |
* |
* |
* |
* |
|
|
B |
* |
* |
* |
* |
* |
* |
1.2 |
|
||
Mean |
* |
* |
* |
* |
* |
* |
0.6 |
|
||
Reflux Extraction (without parent and M1) # |
A |
n.p. |
5.5 |
2.1 |
2.2 |
1.7 |
6.0 |
6.6 |
|
|
B |
n.p. |
5.3 |
1.7 |
1.1 |
1.8 |
6.2 |
4.2 |
|
||
Non-Extractables |
A |
3.7 |
2.2 |
2.3 |
2.8 |
3.9 |
5.8 |
4.4 |
|
|
B |
2.6 |
2.1 |
2.7 |
4.0 |
3.8 |
5.6 |
4.6 |
|
||
14CO2 |
A |
n.p. |
0.4 |
0.7 |
1.1 |
1.5 |
1.6 |
2.0 |
|
|
B |
n.p. |
0.2 |
0.6 |
1.2 |
1.4 |
1.8 |
1.9 |
|
||
Organic Volatiles |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
|
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
||
TOTAL |
A |
101.4 |
104.7 |
102.5 |
101.7 |
101.4 |
101.3 |
103.2 |
|
|
B |
104.5 |
104.5 |
104.0 |
105.2 |
101.8 |
101.4 |
100.1 |
|
||
* Not detected or below quantification limit
# The remaining radioactive fractions in the reflux could not be assigned to fractions seen in the analysis of the ambient extracts
n.p. Not performed
Table 6. Pattern of Radioactivity in Soil II (Latossolo, Clay). Values Are Expressed in Percent of the Applied Radioactivity. The values for the individual metabolic fractions represent the amounts in the pooled ambient and reflux extracts.
14C-labelled test item Soil II (% of applied) |
Sample |
INCUBATION TIME IN DAYS |
|
||||||||||||
0 |
7 |
14 |
28 |
61 |
90 |
120 |
|
||||||||
Parent |
A B |
83.5 |
90.0 |
83.1 |
83.7 |
66.7 |
56.5 |
44.9 |
|
||||||
93.3 |
90.0 |
83.6 |
78.2 |
65.7 |
51.8 |
44.2 |
|
||||||||
Mean |
88.4 |
90.0 |
83.4 |
81.0 |
66.2 |
54.1 |
44.6 |
|
|||||||
ME1 |
A |
* |
* |
0.8 |
1.3 |
* |
* |
* |
|
||||||
B |
* |
* |
1.0 |
1.9 |
* |
1.4 |
1.1 |
|
|||||||
Mean |
* |
* |
0.9 |
1.6 |
* |
0.7 |
0.5 |
|
|||||||
ME2=M1 |
A |
* |
1.4 |
2.5 |
5.6 |
10.2 |
8.5 |
9.0 |
|
||||||
B |
* |
1.4 |
3.1 |
6.0 |
9.3 |
8.7 |
10.4 |
|
|||||||
Mean |
* |
1.4 |
2.8 |
5.8 |
9.8 |
8.6 |
9.7 |
|
|||||||
ME3 |
A |
* |
* |
0.6 |
* |
2.0 |
2.0 |
3.3 |
|
||||||
B |
* |
* |
0.9 |
* |
2.0 |
2.5 |
3.0 |
|
|||||||
Mean |
* |
* |
0.8 |
* |
2.0 |
2.2 |
3.2 |
|
|||||||
ME7 |
A |
* |
* |
0.6 |
* |
* |
* |
* |
|
||||||
B |
* |
* |
* |
* |
* |
* |
* |
|
|||||||
Mean |
* |
* |
0.3 |
* |
* |
* |
* |
|
|||||||
ME8 |
A |
* |
* |
* |
* |
* |
2.6 |
* |
|
||||||
B |
* |
* |
* |
* |
2.1 |
* |
* |
|
|||||||
Mean |
* |
* |
* |
* |
1.0 |
1.3 |
* |
|
|||||||
ME9 |
A |
* |
* |
* |
* |
* |
* |
2.3 |
|
||||||
B |
* |
* |
0.7 |
1.7 |
* |
1.7 |
* |
|
|||||||
Mean |
* |
* |
0.3 |
0.8 |
* |
0.8 |
1.1 |
|
|||||||
ME10 |
A |
* |
* |
* |
* |
* |
1.8 |
1.6 |
|
||||||
B |
* |
* |
* |
* |
1.2 |
1.3 |
1.8 |
|
|||||||
Mean |
* |
* |
* |
* |
0.6 |
1.6 |
1.7 |
|
|||||||
ME11 |
A |
* |
* |
* |
* |
* |
* |
* |
|
||||||
B |
* |
* |
* |
1.8 |
* |
* |
* |
|
|||||||
Mean |
* |
* |
* |
0.9 |
* |
* |
* |
|
|||||||
ME14 |
A |
* |
* |
0.6 |
* |
* |
1.3 |
* |
|
||||||
B |
* |
* |
* |
* |
2.1 |
* |
1.7 |
|
|||||||
Mean |
* |
* |
0.3 |
* |
1.0 |
0.6 |
0.8 |
|
|||||||
ME16 |
A |
* |
* |
* |
* |
* |
* |
* |
|
||||||
B |
* |
* |
0.9 |
* |
* |
1.5 |
* |
|
|||||||
Mean |
* |
* |
0.4 |
* |
* |
0.8 |
* |
|
|||||||
ME17 |
A |
* |
0.7 |
* |
* |
* |
* |
* |
|
||||||
B |
* |
* |
* |
* |
* |
* |
* |
|
|||||||
Mean |
* |
0.4 |
* |
* |
* |
* |
* |
|
|||||||
ME18 |
A |
* |
* |
* |
* |
* |
* |
* |
|||||||
B |
* |
0.5 |
* |
* |
* |
* |
* |
||||||||
Mean |
* |
0.2 |
* |
* |
* |
* |
* |
||||||||
ME19 |
A |
* |
* |
0.9 |
2.0 |
9.0 |
8.1 |
3.7 |
|||||||
B |
* |
* |
0.7 |
2.1 |
4.7 |
4.9 |
4.9 |
||||||||
Mean |
* |
* |
0.8 |
2.0 |
6.9 |
6.5 |
4.3 |
||||||||
ME20 |
A |
* |
* |
* |
1.2 |
* |
1.1 |
1.3 |
|||||||
B |
* |
* |
* |
* |
* |
* |
1.1 |
||||||||
Mean |
* |
* |
* |
0.6 |
* |
0.6 |
1.2 |
||||||||
ME21 |
A |
* |
* |
* |
* |
* |
1.0 |
* |
|||||||
B |
* |
* |
* |
* |
1.3 |
1.3 |
* |
||||||||
Mean |
* |
* |
* |
* |
0.7 |
1.2 |
* |
||||||||
ME22 |
A |
* |
* |
* |
* |
* |
0.8 |
* |
|||||||
B |
* |
* |
* |
* |
* |
* |
* |
||||||||
Mean |
* |
* |
* |
* |
* |
0.4 |
* |
||||||||
ME23 |
A |
* |
* |
* |
* |
* |
* |
* |
|||||||
B |
* |
* |
* |
* |
* |
1.4 |
* |
||||||||
Mean |
* |
* |
* |
* |
* |
0.7 |
* |
||||||||
ME24 |
A |
* |
* |
* |
* |
* |
* |
7.7 |
|||||||
B |
* |
* |
* |
* |
* |
6.1 |
7.4 |
||||||||
Mean |
* |
* |
* |
* |
* |
3.0 |
7.6 |
||||||||
ME25 |
A |
* |
* |
* |
* |
* |
* |
1.7 |
|||||||
B |
* |
* |
* |
* |
* |
1.0 |
0.8 |
||||||||
Mean |
* |
* |
* |
* |
* |
0.5 |
1.3 |
||||||||
ME26 |
A |
* |
* |
* |
* |
* |
* |
2.3 |
|||||||
B |
* |
* |
* |
* |
* |
* |
1.6 |
||||||||
Mean |
* |
* |
* |
* |
* |
* |
2.0 |
||||||||
ME27 |
A |
* |
* |
* |
* |
* |
* |
2.1 |
|||||||
B |
* |
* |
* |
* |
* |
* |
1.7 |
||||||||
Mean |
* |
* |
* |
* |
* |
* |
1.9 |
||||||||
ME28 |
A |
* |
* |
* |
* |
* |
* |
* |
|||||||
B |
* |
* |
* |
* |
* |
* |
1.8 |
||||||||
Mean |
* |
* |
* |
* |
* |
* |
0.9 |
||||||||
Non-extractables |
A |
15.1 |
6.2 |
10.7 |
3.3 |
9.8 |
12.1 |
13.7 |
|||||||
B |
8.1 |
6.1 |
8.3 |
4.3 |
9.7 |
12.1 |
13.2 |
||||||||
14CO2 |
A |
n.p. |
0.2 |
0.5 |
0.1 |
1.9 |
2.5 |
3.6 |
|||||||
B |
n.p. |
0.3 |
0.3 |
0.9 |
2.3 |
3.7 |
2.6 |
||||||||
TOTAL |
A |
98.6 |
98.5 |
100.3 |
97.1 |
99.8 |
98.4 |
97.2 |
|||||||
B |
101.4 |
98.3 |
99.4 |
96.9 |
100.4 |
99.6 |
97.3 |
||||||||
* Not detected or below quantification limit
n.p. Not performed
Table 7. Pattern of Radioactivity in Soil III (Neossolo, Sand). (Values Are Expressed in Percent of the Applied Radioactivity). For the parent substance and M1, the values represent the sum of their amounts in the ambient and reflux extracts. The other factions relate to the ambient extracts since no corresponding peak was recognized in the reflux extract.
14C-labelled test item Soil III (% of applied) |
Sample |
INCUBATION TIME IN DAYS |
||||||
0 |
7 |
14 |
28 |
59 |
92 |
120 |
||
Parent |
A |
101.0 |
99.0 |
91.9 |
91.1 |
77.7 |
73.0 |
76.6 |
B |
104.1 |
93.7 |
90.6 |
83.1 |
83.6 |
75.4 |
74.8 |
|
Mean |
102.5 |
96.4 |
91.3 |
87.1 |
80.6 |
74.2 |
75.7 |
|
ME1 |
A |
* |
* |
3.8 |
2.9 |
3.9 |
3.3 |
4.2 |
B |
* |
3.1 |
3.4 |
2.6 |
4.6 |
3.1 |
4.2 |
|
Mean |
* |
1.5 |
3.6 |
2.8 |
4.2 |
3.2 |
4.2 |
|
ME2=M1 |
A |
* |
2.0 |
1.9 |
3.1 |
7.5 |
5.6 |
7.7 |
B |
* |
2.3 |
1.6 |
4.6 |
6.3 |
6.1 |
9.1 |
|
Mean |
* |
2.2 |
1.8 |
3.9 |
6.9 |
5.9 |
8.4 |
|
ME3 |
A |
* |
* |
3.2 |
4.6 |
5.2 |
4.2 |
5.2 |
B |
* |
2.1 |
3.3 |
5.8 |
5.6 |
5.5 |
5.3 |
|
Mean |
* |
1.0 |
3.3 |
5.2 |
5.4 |
4.9 |
5.2 |
|
ME7 |
A |
* |
* |
* |
* |
* |
1.7 |
* |
B |
* |
* |
1.4 |
* |
* |
1.3 |
* |
|
Mean |
* |
* |
0.7 |
* |
* |
1.5 |
* |
|
ME9 |
A |
* |
* |
* |
* |
2.1 |
1.2 |
* |
B |
* |
* |
* |
* |
* |
* |
* |
|
Mean |
* |
* |
* |
* |
1.0 |
0.6 |
* |
|
ME10 |
A |
* |
* |
* |
* |
1.6 |
0.8 |
* |
B |
* |
* |
* |
* |
* |
0.7 |
* |
|
Mean |
* |
* |
* |
* |
0.8 |
0.8 |
* |
|
ME13 |
A |
* |
* |
* |
* |
* |
1.0 |
* |
B |
* |
* |
* |
* |
* |
1.0 |
* |
|
Mean |
* |
* |
* |
* |
* |
1.0 |
* |
|
ME14 |
A |
* |
* |
* |
* |
* |
* |
* |
B |
* |
* |
* |
* |
* |
0.9 |
* |
|
Mean |
* |
* |
* |
* |
* |
0.5 |
* |
|
ME15 |
A |
* |
* |
* |
* |
* |
1.2 |
* |
B |
* |
* |
* |
* |
* |
* |
* |
|
Mean |
* |
* |
* |
* |
* |
0.6 |
* |
|
ME16 |
A |
* |
* |
* |
* |
* |
* |
* |
B |
* |
* |
* |
* |
* |
* |
1.0 |
|
Mean |
* |
* |
* |
* |
* |
* |
0.5 |
|
Reflux Extraction (without parent and M1) # |
A |
n.p. |
0.4 |
1.3 |
1.2 |
2.0 |
2.3 |
6.2 |
B |
n.p. |
0.8 |
1.6 |
1.1 |
2.2 |
3.3 |
5.2 |
|
Non-Extractables |
A |
1.1 |
2.0 |
1.3 |
1.4 |
2.2 |
8.1 |
4.0 |
B |
1.2 |
1.6 |
1.1 |
1.7 |
1.8 |
6.6 |
3.8 |
|
14CO2 |
A |
n.p. |
<0.1 |
0.2 |
0.3 |
0.6 |
0.6 |
0.6 |
B |
n.p. |
0.1 |
0.2 |
0.3 |
0.5 |
0.6 |
0.7 |
|
Organic Volatiles |
A |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
n.p. |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
TOTAL |
A |
102.1 |
103.5 |
103.8 |
104.6 |
102.7 |
102.9 |
104.5 |
B |
105.2 |
103.6 |
103.4 |
99.2 |
104.6 |
104.4 |
104.0 |
|
* Not detected or below quantification limit
n.p. Not performed
# The remaining radioactive fractions in the reflux could not be assigned to fractions seen in the analysis of the ambient extracts
Description of key information
All available data was assessed and the aerobic studies following standard test guidelines are included here in a weight of evidence approach. Other study is included as supporting information.
Geometric mean DT50 in soil = 227 d, 20 °C, OECD TG 307 and EPA 162 -1 guideline followed, Marshall 2009, Wardrope 2008a, Völkel 2008 and Walther 2010.
Key value for chemical safety assessment
- Half-life in soil:
- 227 d
- at the temperature of:
- 20 °C
Additional information
Four aerobic studies and one aerobic/anaerobic study are available for this endpoint. All of them followed standard test guideline and complied with GLP. The effect values from all four aerobic studies were used in a weight of evidence approach for the CSA. The test conditions and key effect values were summarized in the table below. Calculation of degradation half-lives according to a standardized methodology across three studies (Marshall 2009, Wardrope 2008a and Völkel 2008) is presented in Hayes (2009). In the aerobic/anaerobic study, only the DT50 value under anaerobic conditions is reported. Therefore, this study is included as a supporting study. The DT50 value was determined to be >> 1 year (aerobic phase excluded) using a SFO model. Based on this result, it is concluded that the 14C-labelled test item does not degrade under anaerobic conditions in the sandy clay loam soil tested (Wardrope 2008b).
Table 1. DT50 values for the test substance in soil under aerobic standard (a) test conditions
USDA / Name/ Origin |
OC [%] / pH (water) |
T. [°C] / Moisture |
DT50 [d] - Kinetic model in original report |
DT50 [d] - Kinetic model recalculated |
Author / Year / Smartdoc No. |
Clay loam / Argissolo / BR |
2.9 / 5.4 |
20 / pF 2 (phenyl-label) |
271* - SFO |
- |
Walther, 2010 |
Clay / Latossolo / BR |
1.9 / 4.0 |
20 / pF 2 (phenyl-label) |
121* - SFO |
- |
Walther, 2010 |
Sand / Neossolo / BR |
0.5 / 4.2 |
20 / pF 2 (phenyl-label) |
264* - SFO |
- |
Walther, 2010 |
Loam, 18 Acres, GB |
2.6 / 6.0 |
20 / pF 2 (phenyl-label) |
592 - SFO |
592* - SFO |
Marshall, 2009, Hayes, 2009 |
Sandy loam, Pappelacker, CH |
1.6 / 7.4 |
20 / pF 2 (phenyl-label) |
349 - SFO |
349* - SFO |
Marshall, 2009, Hayes, 2009 |
Loam, Gartenacker, CH |
2.6 / 7.3 |
20 / pF 2 (phenyl-label) |
121 - SFO |
121* - SFO |
Marshall, 2009, Hayes, 2009 |
Silty clay, Marsillargues, FR |
1.4 / 8.3 |
20 / pF 2 (phenyl-label) |
231 - SFO |
231* - SFO |
Marshall, 2009, Hayes, 2009 |
Loam, Gartenacker, CH |
2.5 / 7.3 (6.7 CaCl2) |
20 / pF 2 (pyrazole- label) |
40 - SFO |
39.8* - SFO |
Wardrope, 2008, Hayes, 2009 |
Sandy clay loam, 18 Acres, GB |
3.9 / 6.5 (CaCl2) |
20 / pF 2 (phenyl-label) |
> 1 year – SFO |
976* – SFO |
Völkel, 2008, Hayes, 2009 |
Sandy loam, Gartenacker, CH |
2.7 / 7.2 (CaCl2) |
20 / pF 2 (phenyl-label) |
141 - SFO |
141* - SFO |
Völkel, 2008, Hayes, 2009 |
Silty clay loam, Marsillargues, FR |
1.1 / 7.8 (CaCl2) |
20 / pF 2 (phenyl-label) |
149 – SFO |
149* – SFO |
Völkel, 2008, Hayes, 2009 |
Sandy loam, Pappelacker, FR |
1.6 / 7.1 (CaCl2) |
20 / pF 2 (phenyl-label) |
233 - SFO |
233* - SFO |
Völkel, 2008, Hayes, 2009 |
Geomean |
|
|
227 days |
|
|
a) Criteria for standard test conditions: Meet OECD, SETAC, OPPTS and JMAFF guideline requirements
* Values used for determination of the geomean. More than one set of data was available for the ‘same’ soil under similar incubation conditions, therefore a geometric mean was calculated per soil before integration into the geometric mean (e.g. for 18 Acres (n= 2), Pappelacker (n= 2), Marsillargues (n= 2) and Gartenacker (n= 3)).
Field dissipation - additional information
A large number of soil dissipation studies were conducted with the test material. As the information on soil dissipation is outside the scope of REACH, the studies are not summarized as an endpoint study entry but are briefly discussed here. The test material was tested for different applications in different bare grounds with a rate ranging between 125 - 500 g/ha. For three of these grounds, the DT50 reported in the original reports as calculated with a kinetic model were between 49 - 235 days. For the other ten soils, the DT50 values of the test substance were not calculated. The DT50 values of the test substance in all thirteen grounds were recalculated using the SFO model and were between 9.2 - 629 days. The geometric mean DT50 (n = 13) for soil dissipation was calculated to be 77.1 days (Tummon 2007a, Tummon 2007b, Tummon 2007c, Hayes 2009, Heillaut & Tummon 2009a, Heillaut & Tummon 2009b, Heillaut 2009, Simon 2008, Simon 2009a, Simon 2009b, Zeiger 2009a, Zeiger 2009b, Zeiger 2009c, Zeiger 2009d and Zeiger 2009e)
Information on Registered Substances comes from registration dossiers which have been assigned a registration number. The assignment of a registration number does however not guarantee that the information in the dossier is correct or that the dossier is compliant with Regulation (EC) No 1907/2006 (the REACH Regulation). This information has not been reviewed or verified by the Agency or any other authority. The content is subject to change without prior notice.
Reproduction or further distribution of this information may be subject to copyright protection. Use of the information without obtaining the permission from the owner(s) of the respective information might violate the rights of the owner.
