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EC number: 217-588-1 | CAS number: 1897-45-6
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:
- 20 Oct 2011 to 21 Mar 2013
- 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:
- April 2002
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- EPA OPPTS 835.4100 (Aerobic Soil Metabolism)
- Version / remarks:
- October 2008
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 015
- Soil no.:
- #1
- Soil type:
- silty clay
- % Clay:
- 39
- % Silt:
- 56
- % Sand:
- 6
- % Org. C:
- 1.8
- pH:
- 7.8
- CEC:
- 12.2 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #2
- Soil type:
- sandy clay loam
- % Clay:
- 25
- % Silt:
- 24
- % Sand:
- 51
- % Org. C:
- 2.3
- pH:
- 6
- CEC:
- 18.9 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #3
- Soil type:
- loam
- % Clay:
- 12
- % Silt:
- 43
- % Sand:
- 45
- % Org. C:
- 2.6
- pH:
- 7
- CEC:
- 10.8 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #4
- Soil type:
- other: Loam/Silt loam
- % Clay:
- 20
- % Silt:
- 50
- % Sand:
- 30
- % Org. C:
- 1.7
- pH:
- 5.9
- CEC:
- 23.3 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Details on soil characteristics:
- - Soil test systems: Key soil physico-chemical properties of the four different soils are given in the table below and full details are provided in Table 1 in “Any other information on materials and emthods incl tables”. Characterisation data for each soil were provided from separate GLP studies by the Sponsor or from CEMAS, UK. All soils were stored for 52-53 days, and then sieved using a 2 mm mesh sieve prior to analyses and acclimation. All soils were acclimatised for 13-16 days and incubated at pF 2 at 20 + 2°C in the dark.
- Determination of moisture content and moisture adjustment: The moisture content was determined by drying duplicate aliquots (ca 15 g) of sieved soil in an oven set to maintain 110 °C overnight. The weight of soil was recorded before and after drying and the difference in weight attributed to moisture content. Moisture content of the sieved soils was determined using the following equation Soil Moisture Content (%) = ((Fresh Weight of Soil (g) - Oven Dry Weight of Soil (g))/ Oven Dry Weight of Soil (g)) x100. The moisture content of the soil was adjusted as close to pF 2 as possible by addition of ultra pure water using a spray bottle. Care was taken to avoid compromising the test system by the addition of too much water.
- Preparation of soil test samples: Soil samples were weighed into individual 250 mL capacity Erlenmeyer flasks with ground glass joints. The nominal weight of soil added to each flask was 121.73 g (Marsillargues),127.18 g (18 Acres), 137.05 g (Gartenacker), 123.87 g (White Swan), which was equivalent to 100 g of oven dry soil. A total of 24 test flasks and 8 biomass flasks were weighed for each soil. Soil samples were acclimatised under test conditions for at least 13 to 16 days prior to application of the test item.
- Microbial biomass of soils: The microbial biomass of the soils was determined using a fumigation extraction method. Samples were taken on or before the day of application and again on or soon after 120 days after treatment (DAT). The soil from 4 incubation vessels was transferred to a suitable container. Three of the samples were treated with ethanol free chloroform (prepared by washing 100 mL chloroform with 2 × 40 mL Milli-Q water using a separating funnel) at a rate of 10 L/g. The treated samples were placed in a chamber containing a beaker of ethanol-free chloroform. The pressure in the chamber was reduced by evacuation until the chloroform boiled then the chamber was sealed and left at least overnight. Fumigated soil samples and the control sample were extracted with ca 250 mL of 0.5 M potassium sulphate by shaking on a flat bed or orbital shaker (ca 45 min). Samples were centrifuged at ca 4000 rpm for ca 10 min and the resultant supernatant was filtered. The supernatants were analysed using a Shimadzu Total Organic Carbon Analyser 5000A. Extracts were stored in a fridge set to maintain 4ºC prior to total organic carbon (TOC) analysis. - Duration:
- 120 d
- Initial conc.:
- 1.29 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:
- Soil adjusted close to pF2 moisture tension prior to application
- Microbial biomass:
- 8.24 (start) to 7.83 (end) mg C/100 g
- Soil No.:
- #2
- Temp.:
- 20 ± 2°C
- Humidity:
- Soil adjusted close to pF2 moisture tension prior to application
- Microbial biomass:
- 19.6 (start) to 16.02 (end) mg C/100 g
- Soil No.:
- #3
- Temp.:
- 20 ± 2°C
- Humidity:
- Soil adjusted close to pF2 moisture tension prior to application
- Microbial biomass:
- 27.82 (start) to 26.59 (end) mg C/100 g
- Soil No.:
- #4
- Temp.:
- 20 ± 2°C
- Humidity:
- Soil adjusted close to pF2 moisture tension prior to application
- Microbial biomass:
- 9.69 (start) to 9.54 (end) mg C/100 g
- Details on experimental conditions:
- An overvire of study design is provided in Table 2 in "Any other information on materials and methods incl. tables"
SOLVENTS AND REAGENTS
All chemicals and reagents were purchased from commercial sources and were analytical grade or suitable equivalent.
RADIOCHEMICAL PURITY
The radiochemical purity of the stock [14C]-substance was determined by TLC Solvent System 1 and HPLC Method 1. The radiochemical purity of [14C]-substance in each treatment solution was determined before and after each application.
APPLICATION RATE
The nominal treatment rate was 1.33 µg a.i./g, equivalent to 133 µg of test item per 100 g oven dry soil. This application rate was based on a maximum field application rate of 1000 g a.i./ha, assuming a soil incorporation depth of 5 cm and a soil bulk density of 1.5 g/cm3.
PREPARATION OF TREATMENT SOLUTIONS
A treatment solution of the radiolabelled test item was prepared for each dosing occasion by dissolving [14C]-substance in acetonitrile (Marsillargues and 18 Acres: 6.9 mL) to a target concentration of 1.33 mg/mL. The Gartenacker and White Swan treatment solutions were prepared by combining [14C]-substance (remaining test item following dosing of Marsillargues and 18 Acres soils) and [14C]-substance test item. This was dissolved in 9.3 mL of acetonitrile to a target concentration of 1.33 mg/mL. The radioactivity content and homogeneity of the treatment solutions were determined by LSC. The radioactivity content was used to determine the volume of treatment solution required for each application (102 µL: Marsillargues and 18 Acres; 100 µL: Gartenacker and White Swan; equivalent to 0.1% of the soil dry weight).
APPLICATION OF [14C]-SUBSTANCE
The [14C]-substance treatment solution was applied dropwise to the soil surface using a positive displacement pipette. Following application, each flask was gently tumbled to incorporate the [14C]-substance before being reconnected to the flow through apparatus. The treatment rate was determined by taking aliquots of a full dose (mock dose) at regular intervals throughout the treatment process. Approximately every 10 samples, an aliquot of the treatment solution was added to a volumetric flask (10 mL capacity) and made to volume with acetonitrile prior to LSC.
SAMPLING
See Table 3 in “Any other information on materials and methods incl. tables”.
SAMPLE EXTRACTION AND ANALYSIS
See Table 4 in “Any other information on materials and methods incl. tables”.
STRUCTURE ASSIGNMENT
Structural assignments were made using a combination of 1D-TLC (Solvent System 1, 2, 3 and 4) and HPLC (Method 1, 2, 3 and 4) by co-chromatography with authentic reference standards (See Table 6 in “Any other information on materials and methods incl tables”. LC-MS analysis using multiple reaction monitoring (MRM) was also used to identify components, where adequate resolution could not be achieved using co-chromatography. The following table indicates the solvent systems used for quantification and ID confirmation of [14C]-substance and associated degradates. The systems chosen were those in which the degradate in question was most clearly resolved from the other degradates. - Soil No.:
- #1
- % Total extractable:
- 47
- % Non extractable:
- 38.4
- % CO2:
- 8.6
- % Recovery:
- 93.9
- Remarks on result:
- other: on day 120
- Soil No.:
- #2
- % Total extractable:
- 59.7
- % Non extractable:
- 28.9
- % CO2:
- 8.2
- % Recovery:
- 96.8
- Remarks on result:
- other: on day 120
- Soil No.:
- #3
- % Total extractable:
- 49.4
- % Non extractable:
- 33.7
- % CO2:
- 12.8
- % Recovery:
- 95.8
- Remarks on result:
- other: on day 120
- Soil No.:
- #4
- % Total extractable:
- 59.3
- % Non extractable:
- 30.4
- % CO2:
- 2.3
- % Recovery:
- 92
- Remarks on result:
- other: on day 120
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 98.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 98.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 99.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #4
- % Degr.:
- 99.5
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Key result
- Soil No.:
- #1
- DT50:
- 4.7 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #2
- DT50:
- 4.7 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 1.5 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #4
- DT50:
- 5.1 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Transformation products:
- not specified
- Details on transformation products:
- DISTRIBUTION OF RADIOACTIVE RESIDUES
- The distribution of radioactivity for all soils is presented in Tables 1 to 4 in 'Any other information on results incl tables'.
- Radioactive residues in soil extracts: Data summarising the quantification of radioactive components in the soil extracts are provided in Table 5 to 8 in “Any other information on results incl tables”. Extract 1 was analysed by 1D-TLC (Solvent System 1) for all soils immediately after sampling for identification and quantification. Extract 2, or Extracts 2 and 3 combined (1:1 v/v) for timepoints where Extract 3 contained >5% AR, were also analysed by 1D-TLC (Solvent System 1) for all soils immediately after sampling for identification and quantification. Solvent system 1 was successful in resolving non-polar degradates, however a second TLC system (Solvent System 2) was required in order to resolve polar degradates. In addition, a combination of data from Solvent Systems 1 and 3 was used to generate individual quantification data for M13 and M20. Reference standards were underspotted to aid identification of [14C] residues. The position of radioactive components was compared with reference standards and, where there was co- chromatography, this was used for purposes of identification. Selected White Swan extracts were analysed by Solvent System 2 and the region corresponding to unresolved components M22 and M25 was isolated. The isolated region was then analysed by Solvent System 4 in order to investigate the presence of M22 and/or M25. Extract 1 samples were prepared, mixed with reference standards and analysed by reversed phase HPLC Method 1 and 2 in order to confirm identifications made using TLC analysis (Solvent System 1, 2, 3 and 4). The stability of the test substance was affected during preparation of extracts for HPLC analysis, (therefore this method was used to qualitatively confirm component identifications and used to give an indication of the predominant metabolite in unresolved regions in TLC analysis. Selected samples from Marsillargues, 18 Acres, Gartenacker and White Swan soils were analysed by MRM in order to investigate the presence of the following components: M22, M3, M4, M21 and M24. The LOQ for TLC and HPLC analysis was <0.1% AR.
- Marsillargues: The results are provided in Table 5 in “Any other information on results incl tables”. Unchanged test substance accounted for the majority of the radioactivity present in extracts at 0 to 7 DAT, with mean levels decreasing from 100.1% AR at 0 DAT to 31.2% AR at 7 DAT. Over the remainder of the study, test substance levels decreased to a mean of 1.2% AR at 120 DAT. M4, formed via oxidative dechlorination, was the major degradate formed from aerobic degradation in Marsillargues soil. It was detected from 3 h onwards, reaching a maximum mean of 22.9% AR at 30 DAT, then plateauing at this level for the remainder of the study. M5 was detected from 7 DAT onwards. This degradate reached a maximum of 7.5% AR at 30 DAT, then declined. M3, formed via a glutathione conjugation pathway, was detected from 6 h, reaching a maximum mean of 5.8% AR at 60 DAT. Unresolved M13 and M20 were detected from 7 DAT onwards. Extracts containing >5% AR unresolved M13 and M20 were investigated and M13 was found to be the predominant component. M13 reached a mean maximum of 5.4% AR at 14 DAT, then declined. M20, M21, M8 and M10, and unresolved components M23/M24 and M22/M25 were also detected, but individually did not exceed a maximum mean of 3.8% AR.
- 18 Acres: The results are provided in Table 6 in “Any other information on results incl tables”. Unchanged test substance accounted for the majority of the radioactivity present in the extracts at 0 to 7 DAT, with mean levels decreasing from 102.1% AR at 0 DAT to 31.5% AR at 7 DAT. Over the remainder of the study, test substance levels decreased to a mean of 1.2% AR at 120 DAT. M4 was the major degradate formed from aerobic degradation in 18 Acres soil. It was detected from 3 h onwards, reaching a maximum mean of 18.3% AR at 14 DAT and then declining. M3 was detected at 6 h (0.3% AR) reaching a maximum mean of 15.2% AR at 30 DAT, then declining. At 1 DAT, M5 was detected reached a maximum mean of 6.2% AR at 30 DAT. At 30 DAT, M21, a degradation product of M4, was detected and increased over the course of the study reaching a maximum mean at 120 DAT (5.8% AR) and then declining. M10 was detected from 7 DAT and reached a maximum mean of 5.3% AR at 30 DAT. Unresolved components M23 and M24 were detected at 1 DAT (0.9% AR) and a maximum mean was observed at 90 DAT (5.2%). A replicate sample at 90 DAT was investigated by HPLC and M23 was found to be the major component, while levels of M24 were found to be- Gartenacker: The results are provided in Table 7 in “Any other information on results incl tables”. Unchanged substance accounted for the majority of the radioactivity present in the extracts at 0 to 1 DAT, with levels decreasing from a mean of 95.9% AR at 0 DAT to a mean of 56.1% AR at 1 DAT. Over the remainder of the study substance levels decreased to 0.2% AR at 120 DAT. M4 was the major degradate formed from the aerobic degradation in Gartenacker soil, detected from 0 DAT onwards, reaching a maximum mean of 32.2% AR at 7 DAT then declining. At 1 DAT, M13 was detected (4.7% AR) reaching a maximum mean of 8.1% AR at 7 DAT. Unresolved components M22 and M25 were detected at 1 DAT and increased to a mean 7.9% AR at 14 DAT. Over the remainder of the study, these components decreased to a mean 0.6% AR at 120 DAT. HPLC analysis of selected Gartenacker samples has shown that M22 was the major component and levels of M25 were - White Swan: The results are provided in Table 8 in “Any other information on results incl tables”. Unchanged substance accounted for the majority of the radioactivity present in the extracts at 0 to 30 DAT, with levels decreasing from a mean of 95.6% AR at 0 DAT to a mean of 13.3% AR at 30 DAT. Over the remainder of the study substance levels decreased to a mean of 0.5% AR at 120 DAT. M3, a degradation product formed via a glutathione conjugation pathway, was the major degradate formed from aerobic degradation in White Swan soils. It was detected from 3 h onwards, reaching a maximum mean of 14.4% AR at 14 DAT. The hydroxy degradate M4 was detected at 0 h (0.2% AR) reaching a maximum mean of 8.5% AR at 7 DAT, then declining. At 1 DAT, M8 was detected and reached a maximum mean of 5.2% AR at 7 DAT. M5 was detected at 1 DAT and continued to increase over the course of the study, reaching a maximum mean of 6.4% AR at 90 DAT. Unresolved components M22 and M25 were detected at 7 DAT and reached a maximum mean of 6.1% AR at 90 DAT. TLC analysis of isolated samples from 60-120 DAT has shown that M25 is the major component and levels of M22 are
PROPOSED DEGRADATION PATHWAY
The degradation of substance was complex and involved numerous reactions:
- Oxidative dichlorination
- Oxidation/hydrolysis of nitrile groups to form amides with subsequent oxidative deamination
- Reductive dechlorination
- Reaction with glutathione
- Degradation of glutathione moieties resulting in cysteine conjugate
- Oxidative cleavage of the glutathione conjugate to form the sulphate - Evaporation of parent compound:
- no
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- MICROBIAL BIOMASS
Results for the microbial biomass at study initiation and study termination are provided in Table 1 in 'Any other information on materials and methods incl tables'. Biomass results indicated viable microflora at study initiation. Microbial biomass for Marsillargues, 18 Acres, Gartenacker and White Swan was 18.3, 43.6, 61.8 and 21.6 mg carbon/100 g, respectively, at the start of incubation and 17.3, 35.6, 59.1, 21.1 mg carbon/100 g at the end of the incubation. These measurements demonstrated that the test systems remained viable throughout the study.
PHYSICAL CONDITIONS
The temperature of the room in which the test system was housed was in the range 20 ± 2 °C. On two occasions the temperature dropped to 17.7 °C (19-20 DAT for Marsillargues and 18 Acres; 11-12 DAT for Gartenacker and White Swan) and 17.0 °C (22-23 DAT for Marsillargues and 18 Acres; 14-15 DAT for Gartenacker and White Swan). These short-lived, minor temperature deviations had no impact on the study.
RADIOCHEMICAL PURITY
The radiochemical purity of the [14C]-substance in the treatment solutions determined by TLC and HPLC before and after application was > 97.6%.
TREATMENT RATE
Analysis of mock dose samples indicated that the treatment solutions remained homogenous throughout the treatment process. The actual treatment rate, determined by analysis of mock dose samples, was 129 µg a.i./g oven dry soil equivalent to 967.5 g a.i./ha (assuming an incorporation depth of 5 cm and a bulk density of 1.5 g/cm3).
MASS BALANCE
The distribution and recovery of radioactivity (mass balance) for each soil are presented in Tables 1 to 4 in “Any other information on results incl tables”. Six samples had a mass balance of < 90% (mean range 84.8 - 89.9%). Mass balance results for this study were quantitative but in a minority of samples (no discernable pattern observed) were slightly out with acceptance criteria (90 - 110%). This was deemed to have no effect on the overall outcomes for the study.
VOLATILE DEGRADATION PRODUCTS
The recovery of volatile radioactivity from each soil is included in Tables 1 to 4 in “Any other information on results incl tables”. Confirmation that radioactivity recovered in the NaOH trap solutions was 14CO2 was obtained by the loss of radioactivity as barium carbonate following addition of saturated barium chloride.
BOUND RESIDUES AND ORGANIC MATTER FRACTIONATION
The nature of the non-extractable residue in the 120 DAT samples was investigated by reflux extractions and organic matter fractionation (OMF). Results are provided in Tables 9 to 12 in “Any other information on results incl tables”. The mean levels of radioactivity associated with the reflux extract were 11.3, 9.4, 8.2 and 7.8% AR for Marsillargues, 18 Acres, Gartenacker and White Swan, respectively. TLC analysis of the reflux extracts confirmed that no components not already present in extracts 1-3 were significant following reflux extraction.
DEGT50 OF THE TEST SUBSTANCE IN SOILS
The degradation rate (DegT50) of the parent was determined using non-linear regression and a single first order kinetic model (CAKE, Version 1.4). Two replicate data points for each sampling interval was used, thereby generating a single DegT50 estimate for each soil. Results are provided in Table 13 in “Any other information on results incl tables”. The DegT50 was 4.7 days in Marsillargues and 18 Acres and 1.5 and 5.1 days in Gartenacker and White Swan, respectively. - Conclusions:
- Based on the findings, the DT50 values were calculated to be 4.7, 4.7, 1.5 and 5.1 days in Marsillargues, 18 Acres, Gartenacker and white Swan soils, respectively.
- Executive summary:
The aerobic rate and route of degradation of [14C]-substance was investigated in four different soils, which were designated Marsillargues (silty clay), 18 Acres (sandy clay loam), Gartenacker (loam) and White Swan(loam/silt loam). [14C]-substance was applied at a rate of 129 µg/100g soil (dry weight), which is equivalent to a nominal field application rate of 968 g a.i./ha (assuming an incorporation depth of 5 cm and a bulk density of 1.5 g/cm3). The soils were incubated under aerobic conditions in the laboratory and maintained at soil moisture of pF 2 in the dark at 20 °C for up to 120 days post application. Duplicate samples were analysed immediately following application (zero time) and at 3 h and 6 h then 1, 7, 14, 30, 60, 90 and 120 days after treatment (DAT) using TLC. Volatile radioactivity was continuously flushed from the test vessels and passed through sodium hydroxide and activated carbon. The identity of metabolites was confirmed using a combination of TLC, HPLC and LC-MS analysis.
The mean mass balance was 92.7 ± 5.5%, 98.1 ± 3.8%, 95.6 ± 4.1% and 93.8 ± 3.9% applied radioactivity (AR) for Marsillargues, 18 Acres, Gartenacker and White Swan, respectively. Evolved 14CO2 accounted for a maximum mean value of 8.6%, 8.2%, 12.8% and 2.3% applied radioactivity (AR) by the end of the incubation period, for Marsillargues, 18 Acres, Gartenacker and White Swan soils, respectively.
In Marsillarges soil, the major metabolites was identified as M4 (maximum mean 22.9% AR, 30 DAT). Components identified with > 5% AR were M5 (maximum mean 7.5% AR, 30 DAT), M3 (maximum mean 5.8% AR, 60 DAT) and M13 (maximum mean 5.4% AR, 14 DAT). A number of other radiolabelled components were detected, which individually accounted for ≤ 3.8% AR and included M20, M21, M8, M10, M1/M2 (unresolved), and M22/M3 (unresolved). In 18 Acres soil, the major metabolites was identified as M4 (maximum mean 18.3% AR, 14 DAT). Components identified as M21 (maximum mean 5.8% AR, 120 DAT), M5 (maximum mean 6.2% AR, 30 DAT), M3 (maximum mean 15.2% AR, 30 DAT) and M10 (maximum mean 5.3% AR, 30 DAT) were detected. Unresolved components M1 and M2 were detected and reached a maximum mean of 5.2% AR (90 DAT). A number of radiolabelled components were detected, which included M13, M20, M8 and M22/3 (unresolved), none accounting for greater than 4.2% AR (mean) at any timepoint. In Gartenacker soil, the major metabolite was identified as M4 (maximum mean 32.2% AR, 7 DAT). Components identified as M5 (maximum mean 7.1% AR, 14 DAT), M13 (maximum mean 8.1% AR, 7 DAT) and M3 (maximum mean 7.4% AR, 90 DAT) were detected. Unresolved components M22 and M3 were detected and reached a maximum mean of 7.9% AR (14 DAT). A number of radiolabelled components were detected, which included M20, M21, M8, M10 and M1/M2 (unresolved), none accounting for greater than 3.0% AR (mean) at any timepoint. In White Swan soil, the major metabolite was identified as M3 (maximum 14.4% AR). Components identified as M4 (maximum mean 8.5% AR), M5 (maximum mean 6.4%), M8 (maximum mean 5.2%) and unresolved components M22 and M3 maximum mean 6.1% AR) were detected. The amount of parent (substance) material extracted from the soil decreased over time.
Based on the findings, the DT50 values were calculated to be 4.7, 4.7, 1.5 and 5.1 days in Marsillargues, 18 Acres, Gartenacker and white Swan soils, respectively.
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 1 Jul 1999 to 18 Feb 2000
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- other: EPA 162 - 1
- GLP compliance:
- yes
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 1 999
- Soil no.:
- #1
- Soil type:
- sandy clay loam
- Details on soil characteristics:
- SOIL COLLECTION AND STORAGE
- Geographic location: Jealotts Hill Farm, Nuptovvn Road, Bracknell, Berkshire, UK
- Pesticide use history at the collection site: This field site has received no pesticide treatment for at least five years.
- Collection procedures and sampling depth: The soil was sampled on 1st July 1999 to a total depth of approximately 5 to 20 cm (after removal of the turf).
- Soil preparation: The soil was partially dried over 1 day and sieved (2 mm mesh).
- Storage conditions: After sieving, the soil was placed in loosely folded plastic bags in a controlled temperature room (20°C) where the soil incubation would take place.
- Storage length: 3 days
- Prior to incubation under the study conditions, the soil was adjusted to a moisture content equivalent to pF 2 (32.0 g/100 g soil at 100 cm tension) by the addition of ultra-pure water. The moisture adjusted soil was stored in plastic containers at 20 ± 2°C in the dark for 3 days prior to dispensing into glass pots. - Soil No.:
- #1
- Duration:
- 125 d
- Soil No.:
- #1
- Initial conc.:
- 0.1 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #1
- Initial conc.:
- 1 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #1
- Initial conc.:
- 10 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #1
- Initial conc.:
- 25 mg/kg soil d.w.
- Based on:
- test mat.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 20°C
- Humidity:
- The soil was adjusted to a moisture content equivalent to pF 2 (32.0 g/100 g soil @ 100 cm tension) by the addition of ultra-pure water.
- Microbial biomass:
- not reported
- Details on experimental conditions:
- EXPERIMENTAL DESIGN
- Soil preincubation conditions: Prior to incubation under study conditions, the soil was adjusted to a moisture content equivalent to pF 2 (32.0 g/100 g soil at 100 cm tension) by the addition of ultra-pure water. The moisture adjusted soil was stored in plastic containers at 20 ± 2°C in the dark for 3 days prior to dispensing into glass pots (the test system). After dispensing into glass pots, the soil was preincubated in the test system under study conditions for 9 days prior to the application of the treatment solutions.
- Soil (g/replicate): 40 g dry soil
- No. of replication treatments: 2
- Test apparatus: Glass pot (4.6 cm diameter and 6.0 cm high)
TEST MATERIALS PREPARATION AND APPLICATION
- Preparation: The test material was blown to dryness using nitrogen and diluted with predetermined amounts of acetone and non-radiolabelled test substance to give four treatment solutions for the required application rates of 0.1, 1, 10 and 25 µg/g dry weight of soil and the calculated specific activity of 7290 Bq/µg, 3000 Bq/µg, 300 Bq/µg and 120 Bq/µg respectively.
- Application: Aliquots of the treatment solutions were applied dropwise to the soil surface of each soil pot using a pipette. After application the soil in each pot was mixed thoroughly using a spatula, to ensure even distribution of the test material. Four aliquots of each treatment solution were taken immediately before and on completion of application to the soil. These were used to determine the actual treatment rates and to check the homogeneity of the treatment solutions. Each aliquot was diluted and radioactivity determined by LSC. The radiochemical purity of the treatment solutions were determined immediately prior to and immediately after application, by TLC in solvent systems 47, 48 and
49.
- Homogeneity and purity of treatment solutions: The four treatment solutions remained homogeneous throughout the application process. The variation in the homogeneity of the test solutions was < 2.7%. The treatment rates were provided in Table 1 in "Any other information on materials and methods incl. tables".
TRAPPING OF VOLATILE PRODUCTS
The effluent air from each glass cylinder was sequentially passed through a polyurethane foam bung followed by two carbon sieves. The first sieve, traps volatile products of five to twelve carbon units and the second, traps volatile products of two to five carbon units. Beyond the carbon traps the effluent air was subsequently drawn through two tubes of 2M sodium hydroxide to absorb any 14CO2 produced. The second tube of sodium hydroxide was used in case the primary tube became saturated with carbon dioxide.
SAMPLING DETAILS
- Sampling Regime of the Treated Soils: Soil pots were sampled in triplicate from each treatment immediately after application (zero time) and in duplicate after 2, 7, 15, 22, 34, 64 and 125 days incubation after application. At zero time, duplicate pots from each treatment were extracted and analysed for radioactive residues. On each subsequent sampling day, one pot from each treatment was analysed for radioactive residues. At all sampling intervals the soil pots not extracted were covered with Parafilm and frozen whole. These reserve samples were stored at -20 °C to be used if any specific analytical issues arose - Soil No.:
- #1
- % Total extractable:
- 34.9
- % Non extractable:
- 40.2
- % CO2:
- 22.1
- % Recovery:
- 97.2
- Remarks on result:
- other: Treatment Rate 0.1 µg/g; on day 125
- Soil No.:
- #1
- % Total extractable:
- 37.1
- % Non extractable:
- 43.4
- % CO2:
- 17.2
- % Recovery:
- 97.7
- Remarks on result:
- other: Treatment Rate 1 µg/g; on day 125
- Soil No.:
- #1
- % Total extractable:
- 53.8
- % Non extractable:
- 34.2
- % CO2:
- 10.3
- % Recovery:
- 98.3
- Remarks on result:
- other: Treatment Rate 10 µg/g; on day 125
- Soil No.:
- #1
- % Total extractable:
- 72
- % CO2:
- 4.4
- % Recovery:
- 96.7
- Remarks on result:
- other: Treatment Rate 25 µg/g; on day 125
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 99.1
- Parameter:
- radiochem. meas.
- Sampling time:
- 125 d
- Remarks on result:
- other: Treatment Rate 0.1 µg/g
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 99.4
- Parameter:
- radiochem. meas.
- Sampling time:
- 125 d
- Remarks on result:
- other: Treatment Rate 1 µg/g
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 99
- Parameter:
- radiochem. meas.
- Sampling time:
- 125 d
- Remarks on result:
- other: Treatment Rate 10 µg/g
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 69.6
- Parameter:
- radiochem. meas.
- Sampling time:
- 125 d
- Remarks on result:
- other: Treatment Rate 25 µg/g
- Key result
- Soil No.:
- #1
- DT50:
- < 1 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Treatment Rate 0.1 µg/g
- Key result
- Soil No.:
- #1
- DT50:
- < 1 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Treatment Rate 1 µg/g
- Key result
- Soil No.:
- #1
- DT50:
- 7 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Treatment Rate 10 µg/g
- Key result
- Soil No.:
- #1
- DT50:
- 12 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Treatment Rate 25 µg/g
- Transformation products:
- not specified
- Details on transformation products:
- The degradation products detected in the soil extracts over the course of the incubation at > 10% of applied dose were M4, M9 and M1. M13, M5, M23, M3 and M10 were detected at levels <10% of applied dose. M8 and M20 co-eluted in solvent system 33. M18 and M24 were not detected. M3, M10 and M1 were only co-chromatographed with standard reference compounds for the soil extracts from day 125.
- M4: M4 was detected in all treatments from day 2.The maximum amount present at any one sampling interval was 18.4% of the applied dose, observed in 10 µg/g treatment. For 0.1 µg/g, 1 µg/g and 25 µg/g treatments the maximum levels reached were 12.6%, 17.9% and 16.4% of applied dose, respectively.
- M9: M9 was detected in all treatments from day 2.The maximum amount present at any one sampling interval was 12.7% of the applied dose, observed in 0.1 µg/g treatment. For 1 µg/g, 10 µg/g and 25 µg/g treatments the maximum levels reached were 9.7%, 10.1% and 6.0% of applied dose, respectively.
- M1: M1 was detected in all treatments at day 125. The maximum amount present at any one sampling interval was 11.9% of the applied dose, observed in the 0.1 µg/g treatment. For 1 µg/g, 10 µg/g and 25 µg/g treatments the amounts produced were 6.9%, 1.4% and 4.4% of applied dose, respectively.
No other individual radiolabelled compound amounted to more than 6.5% of the applied radioactivity at any time during the incubation. - Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results in provided in Table 2 - Table 6 in 'Any other information on results incl. tables'.
- Total Recovery of Applied Radioactivity: Total recoveries of radioactivity from the samples extracted immediately after application ranged between 99.4% and 102.6% of the applied dose. Recoveries determined at subsequent sampling intervals were between 84.7% and 102.2% for the four treatments. At no point in the study were the ORBO tubes extracted as the total recoveries were generally acceptable at all sampling intervals. The amount of extractable radioactivity was found to decrease as the sampling period proceeded in all four treatments, ranging from 86.8% to 100.7% on day zero to 34.9% to 72.0% by day 125. The high extractable recoveries at zero time indicates an efficient extraction method and the decline in extractable radioactivity indicates the formation of soil bound residues. Correspondingly, over the 125 day incubation period, the unextracted radioactivity in the soil residues increased from a range of 1.9% to 12.6% on day 0 to between 20.3% and 43.4% of the applied dose, by day 125.
- Radioactivity Evolved from the Soil Systems: This radioactivity is assumed to be 14C-labelled CO2 which accounts for a minimum of 4.4% from the 25 µg/g treatment and a maximum of 22.1% from the 0.1 µg/g treatment by day 125. This indicates that mineralisation of the test substance occurred in all four treatment rates. No radioactivity or volatile products were detected in the foam bungs at any sampling intervals at the four treatment rates.
- Radioactive Residues in Soil Extracts: The quantification of radiolabelled test substance and degradation products in the soil extracts was performed using TLC. The quantitative data from solvent systems 25a and 33 for the four treatment rates have been combined as not all the metabolites were separated in both solvent systems. Data for M3, M10 and M1 were taken from solvent system 10.
- Degradation of the test substance: The decline of the test substance in the three lower treatment rates, 0.1, 1 and 10 µg/g was rapid with just 0.9, 0.6 and 1.0% of applied dose remaining 125 days after application, respectively. The decline of the test substance at the highest rate 25 µg/g, was much slower with 30.4% of applied dose remaining 125 days after application. - Conclusions:
- The DT50 values for the 1 µg/g,10 µg/g and 25 µg/g treatments were 1, 7 and 12 days, respectively. The major products of degradation were M4, which increased and subsequently decreased throughout the incubation period reaching a maximum observed level of 18.4% of the applied dose in the 10 µg/g treatment at day 34. M9 increased throughout the incubation period reaching a maximum observed level of 12.7% of the applied dose in the 0.1 µg/g treatment at day 125. M1 was seen in all four treatment rates at day 125, showing a maximum of 11.9% in the 0.1 µg/g treatment, and a minimum of 1.4% in the 10 µg/g treatment. It is hypothesised for the lower treatment rates (0.1 and 1 µg/g) that the route of degradation via glutathione conjugation was more predominant than in the higher rates (10 and 25 µg/g). The glutathione route of degradation is fast but limited and therefore at higher treatment rates an increasing proportion of the applied is degraded via the other slower routes.
- Executive summary:
The rate and route of degradation of the test substance was believed to be affected by the rate at which the test substance is applied to the test system. This study was conducted in according to EPA guideline 162-1 and in compliance with GLP criteria. The rate and route of degradation of the test substance was investigated in 18 Acres soil (sandy clay loam) using four treatment rates. Aliquots of the pF2 adjusted soil (40 g dry weight equivalent) were dispensed into pots and incubated in flow through columns under negative pressure. 14C-labelled test substance was applied at rates of 0.1, 1 , 10 and 25 µg/g soil and maintained under moist, dark conditions at a temperature of 20°C for up to 125 days. During incubation, effluent gas from each incubation column was passed through a series of traps, including 2M sodium hydroxide to trap evolved 14CO2. At pre-determined intervals after application (0, 2, 7, 15, 22, 34, 64 and 125 days) duplicate soil pots (triplicate at zerotime) were removed from each treatment rate. Of the duplicate pots, one was analysed for total radiochemical content, chlorothalonil and its metabolites (at zerotime, two pots were analysed). The replicate pot was frozen immediately for future analysis as required. Trapping units were replaced at each sampling interval. The rate of degradation was accurately described by the first order multicompartment (FOMC) model.
Total recoveries of radioactivity from the samples extracted immediately after application ranged between 99.4% and 102.6% of the applied dose. Recoveries determined at subsequent sampling intervals were between 84.7% and 102.2% for the four treatments. At no point in the study were the ORBO tubes extracted as the total recoveries were generally acceptable at all sampling intervals. The amount of extractable radioactivity was found to decrease as the sampling period proceeded in all four treatments, ranging from 86.8% to 100.7% on day zero to 34.9% to 72.0% by day 125. The high extractable recoveries at zero time indicates an efficient extraction method and the decline in extractable radioactivity indicates the formation of soil bound residues. Correspondingly, over the 125 day incubation period, the unextracted radioactivity in the soil residues increased from a range of 1.9% to 12.6% on day 0 to between 20.3% and 43.4% of the applied dose, by day 125.
This radioactivity is assumed to be 14C-labelled CO2 which accounts for a minimum of 4.4% from the 25µg/g treatment and a maximum of 22.1% from the 0.1µg/g treatment by day 125. This indicates that mineralisation of the test substance occurred in all four treatment rates. No radioactivity or volatile products were detected in the foam bungs at any sampling intervals at the four treatment rates. The major products of degradation were M4, which increased and subsequently decreased throughout the incubation period reaching a maximum observed level of 18.4% of the applied dose in the 10µg/g treatment at day 34. M9 increased throughout the incubation period reaching a maximum observed level of 12.7% of the applied dose in the 0.1µg/g treatment at day 125. M1 was seen in all four treatment rates at day 125, showing a maximum of 11.9% in the 0.1 µg/g treatment, and a minimum of 1.4% in the 10µg/g treatment.
The decline of the test substance in the three lower treatment rates, 0.1, 1 and 10 µg/g was rapid with just 0.9, 0.6 and 1.0% of applied dose remaining 125 days after application, respectively. The decline of chlorothalonil at the highest rate 25 µg/g, was much slower with 30.4% of applied dose remaining 125 days after application.
Based on the findings, the rate of degradation of 14C-labeIIed test substance was fastest in the 0.1µg/g treatment with a DT50 value of less than 1 day. The DT50 values for the 1 µg/g,10 µg/g and 25 µg/g treatments were 1, 7 and 12 days, respectively.
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 15 Nov 1999 to 23 Jan 2001
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- other: EPA 162 - 1
- GLP compliance:
- yes
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Soil no.:
- #1
- Soil type:
- loam
- % Clay:
- 25
- % Silt:
- 29
- % Sand:
- 46
- % Org. C:
- 4.5
- pH:
- 6
- CEC:
- 16.2 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #2
- Soil type:
- loamy sand
- % Clay:
- 13
- % Silt:
- 4
- % Sand:
- 83
- % Org. C:
- 3.2
- pH:
- 7.5
- CEC:
- 8 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #3
- Soil type:
- sandy loam
- % Clay:
- 11
- % Silt:
- 29
- % Sand:
- 60
- % Org. C:
- 1.3
- pH:
- 6.7
- CEC:
- 4.4 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #4
- Soil type:
- loamy sand
- % Clay:
- 6
- % Silt:
- 11
- % Sand:
- 83
- % Org. C:
- 2.5
- pH:
- 5.6
- CEC:
- 5.5 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Details on soil characteristics:
- SOIL COLLECTION AND STORAGE
- Geographic location and pesticide use history at the collection site: Two soils from the United Kingdom used in this study were ‘18 Acres’ and ‘Chamberlain's Farm’. These field sites have received no pesticide treatment for at least five years. The American soil was ‘ERTC’ from the ZENECA Field Station in North Carolina, USA. The soil ‘Munster’ was from Germany. Location of Soil Sampling Sites was provided in Table 1 in "Any other information on materials and methods".
- Collection procedures and soil preparation: Soils from outside the UK were transported unfrozen to Jealott’s Hill. The soil was partially dried and sieved (2 mm mesh).
- Sampling depth: Approximately 20 cm
- Storage conditions: After sieving, the soil was placed in loosely folded plastic bags and stored in a controlled temperature room (20°C) for 3 days. Spare soil from the biomass determinations were air dried and characterised. - Duration:
- 120 d
- Initial conc.:
- 1 mg/kg soil d.w.
- Based on:
- test mat.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- test mat. analysis
- Soil No.:
- #1
- Temp.:
- 20 °C
- Humidity:
- pF2
- Microbial biomass:
- 2.01 (start) and 1.37 (end) % of soil organic carbon
- Soil No.:
- #2
- Temp.:
- 20 °C
- Humidity:
- pF2
- Microbial biomass:
- 3.09 (start) and 2.41 (end) % of soil organic carbon
- Soil No.:
- #3
- Temp.:
- 20 °C
- Humidity:
- pF2
- Microbial biomass:
- 1.12 (start) and 1.34 (end) % of soil organic carbon
- Soil No.:
- #4
- Temp.:
- 20 °C
- Humidity:
- pF2
- Microbial biomass:
- 0.61 (start) and 0.85 (end) % of soil organic carbon
- Details on experimental conditions:
- EXPERIMENTAL DESIGN
- Soil preincubation conditions: Prior to incubation under study conditions, the soil was adjusted to a moisture content equivalent to pF2 by the addition of ultra-pure water. The moisture adjusted soil was stored in plastic containers at 20 ± 2 °C in the dark for 3 days prior to dispensing into glass pots.
- Soil (g/replicate): 40 (dry soil)
- No. of replication treatments: 2
- Test apparatus: Glass pot (Approximately 4.6 cm diameter and 6.0 cm high). The soil pots were supported on metal trays and positioned in enclosed glass cylinders supplied with moistened air and maintained at 20 ± 2 °C in the dark. The soil was preincubated in the test system under study conditions for 22 days prior to treatment with the application solution.
- Moisture check: Throughout the incubation period, the moisture content of the soils was checked by weighing the pots at regular intervals. Any moisture losses were replaced on these occasions by the addition of ultra-pure water.
- Details of traps for CO2 and organic volatile: The effluent air from each glass cylinder was sequentially passed through a polyurethane foam bung held in a glass container, followed by two carbon sieves. The first sieve ORBO 100 (Carbotrap 20/40), traps volatile products of five to twelve carbon units and the second, ORBO 91 (Carbosieve S-III), traps volatile products of two to five carbon units. Beyond the carbon traps the effluent air was drawn through two tubes of 2M sodium hydroxide to absorb any 14CO2 produced. The second tube of sodium hydroxide was used in case the primary tube became saturated w'ith carbon dioxide. The foam bungs, carbon sieves and sodium hydroxide traps were replaced at each sampling interval.
- The microbial biomass in the four soils was estimated from the respiratory response following addition of glucose to the soil. Biomass measurements were made on untreated soil samples maintained under soil aerobic study conditions. Biomass determinations were made by NRM 4 days prior to treatment with the test material and 122 days after treatment.
TEST MATERIAL APPLICATION
- Volume of test solution used/treatment: Aliquots (2 x 47 µL) of the application solution were applied dropwise to each soil pot.
- Application method: Apply to the soil surface using a pipette. The application gave a nominal 40 µg and 120 KBq dose to each soil pot. After application the soil in each pot was mixed thoroughly using a spatula, to ensure even distribution of the test material.
SAMPLING DETAILS
- Aliquots sampling and test: Four aliquots of 94 µL of the application solution were taken immediately before treatment, after treatment to two soils, and on completion of treatment to all four soils. These were used to determine the actual application rates and to check the homogeneity of the application solution. Each aliquot was diluted to 10 mL with acetone and the radioactivity was determined by LSC. The actual application rates for 18 Acres and Chamberlain’s Farm soils were calculated using the before and during application checks as these two soils were treated First. The application rate for ERTC and Munster soils were calculated using the during and after application checks.
- Soil sampling: Soil pots were sampled in triplicate from each soil type. At zero time, duplicate pots from each soil type were extracted and analysed for radioactive residues. For all remaining sampling points, one pot from each soil type was analysed for radioactive residues. At all sampling intervals the soil pots not extracted were stored at -20 °C to be used if any specific analytical issues arose.
- Soil sampling intervals/times: Immediately after treatment (zero time) and in duplicate after 6 hours, 1, 3, 7, 14, 30, 58, 92 and 120 days after treatment. - Soil No.:
- #1
- % Total extractable:
- 48.2
- % Non extractable:
- 33.1
- % CO2:
- 13.5
- % Recovery:
- 94.8
- Remarks on result:
- other: 120 days after treatment
- Soil No.:
- #2
- % Total extractable:
- 33.8
- % Non extractable:
- 39.9
- % CO2:
- 23.8
- % Recovery:
- 97.5
- Remarks on result:
- other: 120 days after treatment
- Soil No.:
- #3
- % Total extractable:
- 60.9
- % Non extractable:
- 23.7
- % CO2:
- 6.3
- % Recovery:
- 90.9
- Remarks on result:
- other: 120 days after treatment
- Soil No.:
- #4
- % Total extractable:
- 56.3
- % Non extractable:
- 25.7
- % CO2:
- 11.8
- % Recovery:
- 93.8
- Remarks on result:
- other: 120 days after treatment
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 98.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 99.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 98.3
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #4
- % Degr.:
- 98.9
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Key result
- Soil No.:
- #1
- DT50:
- 1 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #2
- DT50:
- 0.3 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 1.3 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #4
- DT50:
- 1.9 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Transformation products:
- not specified
- Details on transformation products:
- IDENTIFICATION OF THE METABOLITIES OF THE TEST SUBSTANCE
An overview of the metabolites of each soil is provided in Table 3 - Table 6 in ‘Any other information on results incl. tables’
- The metabolites detected in the soil extracts over the course of the incubation at 10% or more of the applied dose were M4, M5, M9 and M10.
- M13, M8 and M1 were detected at levels <10% of applied dose. M20 was not separately quantified as it co-eluted with M13 in solvent system 8b, with the test substance and M13 in solvent system 10 and with M8 in solvent system 33.
- M4 was detected in all soils 6 hours after treatment. The maximum amount present at any one sampling interval was 25.3% of the applied dose, observed in Chamberlain’s Farm soil 7 days after treatment (DAT). For 18 Acres, ERTC and Munster soils the maximum levels reached were 8.1% at 7 DAT, 20.8% at 3 DAT and 6.3% at 3 DAT of applied dose, respectively. Levels of M4 in all soils then declined for the remainder of the study (with less than 15% remaining after 120 days).
- M5 was detected in ERTC and Munster soils 1 day after treatment, in 18 Acres soil after 3 days and in Chamberlain’s Farm soil after 7 days. The maximum amount present at any one sampling interval was 13.2% of the applied dose, observed in Munster soil at 30 DAT. For 18 Acres, Chamberlain’s Farm and ERTC soils the maximum levels reached were 4.1% at 14 DAT, 4.3% at 14 DAT and 6.0% of applied dose at 30 DAT, respectively. Levels of M5 in all soils then declined for the remainder of the study (with less than 8% remaining after 120 days).
- M9 was detected in all soils 6 hours after treatment. The maximum amount present at any one sampling interval was 14.1% of the applied dose, observed in 18 Acres soil at 7 DAT. For Chamberlain’s Farm, ERTC and Munster soils the maximum levels reached were 5.8% at 3 DAT, 12.3% at 30 DAT and 11.7% of applied dose at 14 DAT, respectively. Levels of M9 in all soils then declined for the remainder of the study (with less than 11% remaining after 120 days).
- M10 was detected in 18 Acres and Chamberlain’s Farm soils 1 day after treatment and 3 days after treatment in ERTC and Munster soils. The maximum amount present at any one sampling interval was 12.4% of the applied dose, observed in ERTC soil at 120 DAT. For 18 Acres, Chamberlain’s Farm and Munster soils the maximum levels reached were 4.0% at 58 DAT, 2.9% at 92 DAT and 6.4% of applied dose at 92 DAT, respectively. With the exception of ERTC soil, levels of M10 were decreasing by the end of the study.
- M1 was detected in 18 Acres and Munster soils 1 day after treatment and 7 days after treatment in Chamberlain’s Farm and in ERTC soils. The maximum amount present at any one sampling interval was 6.6% of the applied dose at 92 DAT, observed in 18 Acres soil. For Chamberlain’s Farm, ERTC and Munster soils the maximum levels reached were 3.8% at 120 DAT, 2.0% at 120 DAT and 3.2% of applied dose at 120 DAT, respectively.
- No other individual radiolabelled compound amounted to more than 8.6% of the applied radioactivity at any time during the incubation. Bound residues increased throughout the incubation period with maximum levels from Chamberlain’s Farm soil (39.9% of the applied dose). Levels of bound residues in 18 Acres, ERTC and Munster soils were found to be 33.1%, 23.7% and 25.7% of the applied dose, respectively.
DEGRADATION OF THE METABOLITES OF THE TEST SUBSTANCE
- The degradation of M4, M5 and M9 were adequately modelled by a simple first order model (SFO). The modelling of M4, M5 and M9 in all soils, gave half-lives of 37-131 days, 63-125 days and 63-144 days, respectively. The conversion factor is the figure entered into the model which takes account of the fraction of parent that degrades to the metabolite, but does not lake into account the molecular weight of the metabolites.
MASS SPECTROMETRY OF THE METABOLITES
- The analysis of M2 and M9 by mass spectrometry confirmed the identity of the metabolites in the soil extracts. The analysis of M5 and M10 by mass spectrometry suggested the presence of the metabolites. The presence of these metabolites could not be confirmed due to the poor sensitivity of the compounds by mass spectrometry and the very low amount of each compound available. However, the presence of these two metabolites was adequately confirmed by TLC. - Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the result is provided in Table 2 - Table 7 in ‘Any other information on results incl. tables’.
- Total Recovery of Applied Radioactivity: The total radioactivity recovered was calculated by the sum of activity in the soil extracts, soil residue on combustion and that trapped as 14CO2 in the sodium hydroxide traps. No activity was found in any of the analysed foam bungs or carbon sieves. Total recoveries of radioactivity from the samples extracted immediately after treatment ranged between 97.3% and 100.6% of the applied dose. Total radioactive recoveries for remaining sampling intervals were generally > 90% for the four soil types. The average total radioactive recovery for all soils was 94.9%.
- Radioactivity Evolved from the Soil Systems: The levels of radioactivity recovered in the sodium hydroxide traps was confirmed as 14C-labelled CO2 and accounted for between 6.3% (ERTC soil) and 23.8% (Chamberlain’s Farm soil) by day 120. This indicates that mineralisation of the test substance occurred in all four soil types. No radioactivity or volatile products were detected in the foam bungs or carbon sieves up to day 7 in any soil type. As the total radioactive recoveries were generally > 90% of applied dose there was no evidence to suggest the formation of a significant volatile product.
- Radioactive Residues in Soil Extracts: The amount of extractable radioactivity was found to decrease with time in all four soils. It ranged from 92.6% to 99.2% on day zero to 33.8% to 62.4% by day 120. The high level of extractable recoveries at zerotime indicate that the extraction method was efficient for the test substance. The decline in extractable radioactivity with time (despite acidic extractions) suggests that the remaining radioactivity is bound or incorporated into the soil matrix. The quantification of radiolabelled the test substance and degradation products in the soil extracts was performed using TLC. The TLC separation of the test substance and its individual metabolites was incomplete in any one solvent system. Therefore, the reported quantitative data for each component was individually selected to represent the most reliable value.
- Degradation of the test substance: The degradation of the test substance in the four soils was generally adequately described by a first order multicompartment model (FOMC). The degradation of the test substance was extremely rapid in all soils with half-lives and DT50 values of 0.3 - 1.9 days. The rapid decline continued with more than 90% of the applied material degraded by 8 days after application. - Conclusions:
- Based on the findings, the DT50 values were calculated to be 1, 0.3, 1.3 and 1.9 days in 18 Acres, Chamberlain's Farm, ERTC and Munster soils, respectively. The major products of degradation (> 10% of applied dose) were M4, M5, M9 and M10. All major metabolites, with the exception of M10, reached a maximum level early in the study in all soils and then declined for the remainder of the study. Maximum levels for each metabolite were as follows: M4, 25.3%, M5, 13.2%, M9, 14.1% and M10, 12.4%.
- Executive summary:
The rate and route of degradation of the test substance was investigated in four different soils: 18 Acres (loam), Chamberlain’s Farm (loamy sand), ERTC (sandy loam ) and Munster (loamy sand). The study was conduced according to guideline EPA 162-1 and in compliance with GLP criteria. 14C-labelled test substance was applied at a nominal rate of 1.0 mg/kg dry weight soil equivalent to a single field application rate of 1.5 kg ai/ha with 50% crop interception, incorporated into 5 cm soil and assuming a soil bulk density of 1.5 g/cm3. The soils were incubated under aerobic conditions in the laboratory and maintained under moist (approximately pF2), dark conditions at 20 °C for up to 120 days. Quantification of radiolabelled test substance and metabolites was performed by extraction followed by thin layer chromatography.
The total recoveries of radioactivity were good, generally > 90% of the applied dose. The rapid decline continued with more than 90% of the applied material degraded by 8 days after application. The major soil degradate of the test substance was found to be M4. Levels of M4 increased and subsequently decreased over the incubation period in all soil types. The maximum amount produced in Chamberlain’s Farm and ERTC soils was 25% of the applied dose after 7 days and 21% of the applied dose after 3 days, respectively. Levels in 18 Acres and Munster soils remained below 10% of the applied dose. The second major soil degradate was M9. M9 was detected in all soil types 6 hours after treatment with levels increasing and subsequently decreasing over the incubation period. The maximum amount produced in 18 Acres, ERTC and Munster soils was 14% of the applied dose after 7 days, 12% of the applied dose after 30 days and 12% of the applied dose after 14 days, respectively. Levels in Chamberlain’s Farm soil remained below 6% of the applied dose. The third major soil degradate was M5. Levels of M5 increased and subsequently decreased over the incubation period in all soil types. The maximum amount produced in Munster soil was 13% of the applied dose after 30 days. Levels in 18 Acres, Chamberlain’s Farm and ERTC soils remained at or below 6% of the applied dose throughout the study. M10 reached a maximum of 12% of the applied dose in ERTC soil after 120 days. Amounts of M10 in 18 Acres, Chamberlain’s Farm and Munster soils remained at or below 6% of the applied dose throughout the study. With the exception of ERTC soil, levels of M10 were decreasing by the end of the study. The modelling of M4, M5 and M9 in all soils, gave half-lives of 37-131 days, 63-125 days and 63-144 days, respectively. M10 could not be estimated. The FOMC model gave the best fit to the data for the major metabolites, however the SFO model was acceptable for modelling purposes. No other individual radiolabelled compound amounted to more than 9% of the applied dose at any time during the incubation. Carbon dioxide was a major product of metabolism in all soils reaching a maximum 24% of the applied dose by the end of the incubation. Unextracted residues increased slowly throughout the incubation, reaching a maximum of 40%. Based on the findings, the DT50 values were calculated to be 1, 0.3, 1.3 and 1.9 days in 18 Acres, Chamberlain's Farm, ERTC and Munster soils, respectively.
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- other: EPA 162-1
- GLP compliance:
- yes
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 1 993
- Soil no.:
- #1
- Soil type:
- loamy sand
- % Clay:
- 5.6
- % Silt:
- 14
- % Sand:
- 80.4
- % Org. C:
- 1.49
- pH:
- 5.1
- CEC:
- 7.02 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.31
- Details on soil characteristics:
- SOIL COLLECTION AND STORAGE
- Geographic location: Perry Township, Lake County, OH, USA
- The soil is described as a loamy sand with a 1/3 Bar moisture of 15.5% (dry weight basis)
- Storage conditions and length: Stored at about 8% moisture in the green house until the experimental start date for the study
- Soil preparation: Partially dried, screened with a 600 micron sieve
- Soil No.:
- #1
- Duration:
- 6 mo
- Soil No.:
- #1
- Initial conc.:
- 1 mg/kg soil d.w.
- Based on:
- test mat.
- Soil No.:
- #1
- Initial conc.:
- 10 mg/kg soil d.w.
- Based on:
- test mat.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 24 ± 0.6 °C
- Humidity:
- 74.5 ± 4.1 % (1 ppm soil samples; expressed in terms of percent of the 1/3 Bar moisture tension for P0 soil on the dry weight basis)
- Microbial biomass:
- Total microbial numbers (bacteria and fungi) were normal for each sample and fell within the ranges acceptable for soil samples tested soon after collection,
- Soil No.:
- #1
- Temp.:
- 24 ± 0.6 °C
- Humidity:
- 74.7 ± 2.7% (10 ppm soil samples; expressed in terms of percent of the 1/3 Bar moisture tension for P0 soil on the dry weight basis)
- Microbial biomass:
- Total microbial numbers (bacteria and fungi) were normal for each sample and fell within the ranges acceptable for soil samples tested soon after collection,
- Details on experimental conditions:
- EXPERIMENTAL DESIGN
- Soil: 50 g
- Moisture: An exact weight of water was added to each jar to adjust the soil moisture content to 11.63% (75% of the 1/3 Bar value on the dry weight basis).
- No. of replication treatments: 2
- Test apparatus: Glass jars
- Details of traps for CO2 and organic volatile: Replicate samples of moist, the test substance-treated soil were aged by incubation at 24 °C in a sealed chamber system contained in a controlled temperature laboratory. The sealed system allowed moistening of inlet air and passage of outflow air through 1M sodium hydroxide solution in a twin bubbler tower arrangement to trap acidic volatiles such as carbon dioxide. The airflow through the system was driven by a vacuum pump regulated by an air flow meter attached to the outflow line of the last bubbler tower. The sodium hydroxide traps were analyzed and replaced at 3 to 15 day intervals.
PREPARATION AND APPLICATION OF THE TEST MATERIALS
- Preparation: Uniform 14C-(benzene ring)-labelled test substance, dissolved in acetonitrile, was analyzed by HPLC to determine specific activity and radiochemical purity. When necessary (e.g., in the preparation of the 10-ppm dosing solution), isotopic dilution of label was done by addition of nonradioactive, analytical grade test substance, also contained in acetonitrile solution.
- Application: The test substance was applied to PO soil using a bulk process. All of the labeled test substance was added in acetonitrile solution to about 10% of the required total amount of soil mass. The vehicle was evaporated in the hood to produce a free flowing material and the remaining soil was added in three 30% portions each followed by roller mixing. The total amount of PO soil treated at 1 ppm and mixed in this way was about 1700 g. It was important that the soil was just wet enough (with water) to be still flowable, but not so dry as to generate interfering static charge, these conditions. With the PO soil, a moisture content of 2 to 5% met these conditions. The resultant treated soil was shown by combustion analysis to be homogeneous after one hour of roller mixing; the coefficient of variation for 14C concentration, dpm/g, was less than 10%.
Experimental conditions (in addition to defined fields)
- Moisture maintenance method: An exact weight record for each soil sample and jar (= sample replicate) allowed maintenance of the soil moisture for the entire soil aging period. Moisture in all incubated jars was assessed by soil sample gross weight (soil + jar) each time that soil samples were taken for solvent extractive analysis or for the measure of evolved 14CO2. Soil samples that had lost moisture were adjusted by adding water to increase sample weight to a moisture content above 75% of the 1/3 Bar so that an average of near 75% could be maintained over the incubation period.
- Continuous darkness: Yes
SAMPLING DETAILS
- Soil Moisture record: The soil moisture records were reported in terms of the average moisture content for all samples incubated through each given time interval and were expressed in terms of the percent of the 1/3 Bar moisture content. The results were obtained for the start and end of each reported aging interval when water was again added to the set of samples for the start of the next interval. The data per interval were then averaged. The median between average start and ending moistures provided a "time averaged" moisture content for the given time interval. The overall average moisture content for the entire study aging period was calculated as the mean and standard deviation of all averaged start and ending moisture values reported.
At each sampling interval one or two soil samples were removed from incubation and analyzed according to the scheme. The analytical events occurred in the sequence:
- Sample gross weight (for gross moisture record)
- Subsample 1: moisture analysis(by moisture balance)
- Subsample 2: combustion analysis to determine TRR
- Subsample 3: solvent extraction including
LSC Analysis of Extract A TRR content and HPLC/TLC
LSC Analysis of Extract B TRR content and HPLC
Combustion analysis to determine TRR content of PES
- Sampling methods: Randomizing the selection of duplicate samples taken for solvent extraction analysis was done by using the high and low moisture samples remaining in the set after the last water addition. When single samples were taken for analysis (with two subsamples taken for duplicate extractions) selection was made on the basis of highest moisture content among remaining samples.
No special care was taken to equilibrate the soil samples transferred from incubator to laboratory temperature because these temperatures were not appreciably different. Subsampling, however, was done as soon as possible after gross weight was measured to avoid changes in moisture content. Subsample 1 for moisture analysis which allowed up to 6 g per each of one or two determinations was removed first. Subsample 2 for TRR combustion analysis consisted of 3 or 5 portions of about 0.2 g each that were directly weighed into combustion boats. Subsample 3 was taken last and was weighed directly into the extraction vessel. All aspects of these subsample operations and the indicated analyses were easily and quickly accomplished in one to four hours by two technicians. - Soil No.:
- #1
- % Total extractable:
- 71.8
- % CO2:
- 1.36
- Remarks on result:
- other: 10 ppm; on day 181
- Soil No.:
- #1
- % Total extractable:
- 61.9
- % CO2:
- 3.7
- Remarks on result:
- other: 1 ppm; on day 181
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 96.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 181 d
- Remarks on result:
- other: 1 ppm test substance treated samples
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 93.2
- Parameter:
- radiochem. meas.
- Sampling time:
- 181 d
- Remarks on result:
- other: 10 ppm test substance treated samples
- Key result
- Soil No.:
- #1
- DT50:
- 4 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: 1 ppm test substance treated sample; adjusted from 24 °C results
- Key result
- Soil No.:
- #1
- DT50:
- 21 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: 10 ppm test substance treated sample; adjusted from 24 °C results
- Soil No.:
- #1
- DT50:
- 3 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 24 °C
- Remarks on result:
- other: 1 ppm test substance treated sample; based on direct data
- Soil No.:
- #1
- DT50:
- 16 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 24 °C
- Remarks on result:
- other: 10 ppm test substance treated sample, based on direct data
- Transformation products:
- not specified
- Details on transformation products:
- In qualitative terms, all of the known the test substance soil metabolites were observed in virtually all extracts at both applied rates. This included M4, M13, M8, M20, M23, M25 and M5.
M20 was previously thought to always cochromatograph in TLC and HPLC with its isomer, M8. However, in the course of work to characterize the test substance soil residues, it was found that
M20 in fact was separated from M9 with T4 conditions (and others). It was further noted that M20 was coincident with the unknown region initially assigned as UNK-2. While this region might include other species, it appears certain that the UNK-2 region does contain M20. This was supported by both HPLC retention time data and the behavior in solvent partition experiments.
In addition, some species that were previously not examined chromatographically because they remained in the unextracted water-soluble portion of the residue were now visible in the HPLC profile. Some unknown regions in the HPLC profile that attained more than 10% of the TRR (UNK-3 and UNK-5 in 1-ppm treated soil) were characterized. The rise and decline of several metabolites were well displayed.
The parent test chemical declined rapidly and the rate was dose dependent: DT50 for 1 ppm was less than 5 days; for the 10 ppm soil the DT50 was about 18 days.
- M4: This important test substance metabolite was obtained at a higher proportion of the residue with higher test substance applied rate (12.1% with 10 ppm and 5.6% at 1 ppm test substance applied). The highest concentrations were -obtained at 14 to 61 days and clearly declined afterward. The rate of M4 degradation depended on the kinetic model applied to the data. In simplest form and using a short-term, first-order model, the DT50 for M4 at 1 and 10 ppm the test substance, respectively were 21 and 14 days.
- M5: This soil metabolite attained its highest proportion of the residue at 150 to 180 days. Larger
proportions were again seen at the higher application rate (18.9% with 10 ppm and 14.1% with 1 ppm test substance applied). No kinetic analysis on M5 was done.
- M20: This metabolite only exceeded 10% of the residue in 1 ppm test substance treated soil. At 10 ppm, M20 attained 6.1% of the TRR at DAT=28 days and did not require further examination. At 1 ppm , this component did attain 13.2% of the TRR (about 0.13 ppm) at DAT=4 days. The level of M20 declined rapidly thereafter and was not of further concern.
- Other: M13, M8, and M23 did not attain sufficient percentages of the TRR to require more detailed examination.
- UNK-3: Unknown region 3 attained maximum proportion of the residue at or after 150 days after test substance application. At 10 ppm, this component region did not attain 10% of the TRR (9.62 at DAT=181 days). At 1 ppm, UNK-3 appeared to linger near 14 to 15% of the TRR over the interval of 28 to 152 days.
- UNK-5: Unknown region 5 also attained the maximum proportion of the residue at or after 150 days post-test substance application. At 10 ppm, this component region did not attain 10% of the TRR (9.12 at DAT=181 days). At 1 ppm, UNK-5 attained a clear maximum proportion at DAT=152 days (20.72) and declined afterward, multicomponent nature of UNK-5 is also discussed later - Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results is provided in Table 1 – Table 4 in ‘Any other information on results incl. tables’.
- HPLC: Using the solvent A extract HPLC results, 1 ppm samples averaged 91.6% as the test substance in the profile. The average recovery for the amount of 14C injected was 101.8%. All four of the chromatograms obtained with the 1 ppm samples, both initial and later repeats, were included in the final averages. The DAT=0 data with samples of the 10 ppm treated soil were better. These chromatograms showed an average test substance content of 94.3% and average recoveries of 100.2%. These results demonstrated that in both 1- and 10 ppm experiments very little test substance was consumed during soil treatment and chromatography procedures despite the amount of time required to treat the soils and show homogeneity of application, the 1 ppm study and 2 hours in the 10 ppm study were required for this work before subsamples could be taken and extracted for the DAT=0 days analyses. It is further noted that the results remained nearly the same even after the treated soils had been in freezer storage for several months and repeat extractions were performed.
- Storage stability: Frozen stored soil samples were stable for at least one year as evidenced by the foregoing descriptions of samples reanalyzed after more than one year of frozen storage at -40 °C. Extractions and HPLC analyses were repeated for sample days DAT=0, DAT=4, and DAT=7 days of soil treated at 1 ppm and sample day DAT=7 of soil treated at 10 ppm. These samples were reanalyzed because no B solvent extractions had been performed at the time of the original analysis. In all cases very good agreement was obtained for the amounts of the TRR extracted with solvent A. There was also very good agreement among HPLC profiles for the original and repeated solvent A extracts. The extracts themselves were also stable. Profiles in HPLC remained virtually identical as long as the acetone component of the solvent was removed and the methanol concentration was kept low for storage.
- The Total Radioactive Residue: The whole soil TRR at DAT=0 for the 1 ppm treated soil was 46,791 dpm/g (or 1.051 ppm of the test substance) at 7.80% moisture and 92,874 dpm/g (or 10.74 ppm of the test substance) for the 10 ppm treated soil at 6.90% moisture. At exactly 75% of the 1/3 Bar moisture content (11.63% moisture) these concentrations would be 1.015 ppm and 10.28 ppm, respectively. The overall mean TRR (moisture adjusted soil plus accumulated CO2 DPM amounts per 20g) for all samples analyzed through six months for the 1 ppm soil was 100.5 ± 1.8% of the DAT=0 result. The overall mean TRR for the 10 ppm soil (per 10g soil amounts) through six months was 100.5 ± 1.52% of the DAT=0 result.
- Solvent Extraction Results: The DAT=0 extractions provided 93.1% of the 1 ppm TRR in the solvent A extract, 4.6% in the solvent B extract and 2.6% in the PES. At DAT=181 days the distribution was shifted to 49.0, 13.0 and 34.5% for extracts A and B, and the PES, respectively. These six month aging results were adjusted for 3.7% of the 1 ppm TRR that was accumulated as 14CO2. The average recovery for all of the 1 ppm treated soil extractions was 99.4 ± 7.32%. The DAT=0 extractions of the 10 ppm treated soil provided 97.5% of the 10 ppm TRR in the solvent A extract (no solvent B extraction was needed) and 2.5% in the PES. At DAT=181 days the distribution was shifted to 59.9 11.9 and 26.9% for extracts A and B, and the PES, respectively. These six month aging results were adjusted for 1.4% of the 10 ppm TRR that was accumulated as 14CO2. Note also that the 10 ppm PES maximum level of 32.5% was attained at DAT=91days. The average recovery for all of the 10 ppm treated soil extractions was 102.1 ± 4.6%.
- Chromatographic Analysis of the Extracted Residue: The HPLC analyses recoveries were not averaged but the ranges were reported as follows: For 1 ppm treated soil extract A analyses the recoveries ranged from 83.9 to 127.7% of the applied 14C; for the 1 ppm B extract analyses the range was 81.3 to 154.6%. For the 10 ppm treated soil extract A HPLC analyses the recovery range was 92.6 to 119.3%, and for the 10 ppm B extract analyses, 88.9 to 113.8%.
- Mass Spectroscopy Confirmation of M5: All of the profile components were defined by cochromatography with standards using program T4. M4 and M13 were confirmed by virtue of the TLC application needed for quantitation. M5 was selected for added confirmation because it did represent the order of 10% and more of the TRR, so confirmation by mass spectroscopy was applied. Confirmation of M5 was obtained in several forms including matched retention time and mass spectrum compared to the reference standard. Other potential species were excluded in parallel experiments through retention time differences and absence of like mass spectra (for non M5 standards).
- Unknown Characterization: Two regions were of sufficient quantity to require further examination. Unknown region 3 was characterized using HPLC program T6 for DAT=21, 91, and 152 days with solvent A extracts of 1 ppm test substance-treated soil and at DAT=181 days with 10 ppm extracts. In all samples similar results were obtained. Unknown region 3 may be described as containing one major component and several minor components: None of the minor components exceeded 1.6% of the TRR at any time. Over time the major component in the 1 ppm extracts was observed to increase from 8.0% of the TRR at DAT=21 days to 11.5% at DAT=152 days. The major component of the 10 ppm DAT=181 days sample accounted for 7.3% of the TRR. HPLC (T6) recoveries for the UNK.-3 region isolates was 90.6 to 107.4%. Unknown Region 5 was characterized using the HPLC program T1 with an SAX column. Sample days DAT=21 and 152 days of the solvent A extract of 1 ppm test substance treated soil were examined, as was DAT=181 days of the 10 ppm extracts. Unknown region 5 may be described as containing three major components and several minor components: None of the minor components exceeded 1% of the TRR at any time. For the 1 ppm soil extracts, the three major components at DAT=21 days were 1.5, 2.5, and 1.4% of the TRR, while the DAT=152 days sample contained these same components at 5.3, 4.2 and 2.1% of the TRR. The same species in the 10 ppm extract at DAT=181 days were 1.2, 3.4 and 0.5% of the TRR. SAX run recoveries for the UNK-5 region isolates was 90.4 to 140%. It is clear from the characterizations of these unknown regions (3 and 5) that several components were present in each of them. There was only one instance (with the 1 ppm UNK-3 region at 152 days) in which any component in fact exceeded 10% of the TRR. Depending on the dpm per peak definition, the total number of unknown compounds in regions 3 and 5 could range between 5 and 27, for an average of 16.
- Characterization of the PES Fraction: The PES was characterized by way of the analysis of Extract B. Since strong acid conditions( Solvent B) were required to obtain this material, it describes by definition, a part of the soil "bound" residue. The B extract HPLC profile contained similar patterns of component distribution as was seen in extract A. The bound residue was identical in composition with the freely extractable part of the residue (Solvent A), but was less mobile than the extract A portion of the residue.
- Metabolic Pathway: An exact sequence of metabolite interconversions is not known. The steps that are shown are rationalizations based on general principles of chemistry. It is very likely that several paths operate simultaneously and that each may be differently affected by the soil concentration (rate) of the test substance applied. - Conclusions:
- Based on the findings, it was conclude that the degradation of the test substance was rapid. The DT50 was 3 – 16 days at 24 °C (equivalent to 4 - 21 days at 20°C) . It was very dependent on the rate of application and less depend on the kinetics model applied. Degradation of the test substance led to formation of six known metabolites, and to a complex mixture of polar, water soluble unknowns.
- Executive summary:
The rate and pattern of degradation of 14 C-labelled test substance in a sandy loam soil was investigate at 25 °C in the dark under aerobic conditions by following EPA guideline 162-1 and in compliance with GLP criteria. The soil (free of ACN, 75% moisture of the 1/3 bar) was treated with 1 and 10 ppm test substance. A blank formulation was added to the soil while vetting it. Sealed chamber incubation proceeded at 24 ± 1 °C in the dark and included exhaust gas trapping (sodium hydroxide for carbon dioxide). Trapped volatile 14C was analysed and traps replenished at 7 to 30 day intervals allowing test system maintenance and an ongoing record of soil moisture content. At eight time intervals (0, 7, 14, 28, 61, 124, 152, and 181 days for 10 ppm treated soil, and more frequently for the 1 ppm treated soil), soil samples were withdrawn from incubation for total radioactive residue analysis (TRR). The TRR was expressed as the sum of 14C from accumulated CO2 and whole soil combustion and was constant (at constant soil moisture) over the duration of the study.
The mean sample balance (whole soil combustion plus 14CO2) was 100.5 (± 1.8)% for soils treated at 1 ppm and 100.5 (±1.5)% for soils treated at 10 ppm. The mean for extraction recovery (the sum of 14C in Extracts A and B, plus PES) vas 99.3 (± 5.9)% for the 1 ppm soils and 102.1 (± 3.7)% for the 10 ppm soils. In the 10 ppm test substance-application experiment M4 at its maximum accounted for about 12.1% of the TRR on DAT=61 days and declined afterward. M5 increased steadily to a maximum of 18.8% at DAT=181 days. None of the other known metabolites nor any of the unknown regions exceeded 10% of the 10 ppm soil TRR at any time. The largest of these, a component of unknown region 3, attained a maximum of 7.3% at DAT=181 days. A rise and decline was seen for residues of M8 and M20 which represented the next most significant residue components. AT DAT=181 days 1.4% of the 10 ppm TRR had accumulated as 14CO2. At DAT=181 days 6.8% of the 10 ppm TRR remained as the test substance. In the 1 ppm test substance-application experiment M4 at maximum accounted for only 5.6% of the TRR (at DAT=28 days). M5 achieved a maximum value of 14.1% of the TRR at DAT=152 days. M20 attained 13.2% of the TRR at DAT=4 days. Unknown region 3 (a complex mixture) maintained a plateau at about 14.0(± 1)% after DAT=28 days and up until DAT=152 days. Unknown region 5 (also a complex mixture) attained a maximum of about 20.7%of TRR at DAT=152 days and declined thereafter. Only one individual component of either unknown region actually exceeded 10% of the 1 ppm TRR, and this was the major component of UNK-3 which was observed at 11.5% of TRR at DAT=152 days. No other metabolites exceeded 10% of the 1 ppm TRR in this study, although rise and decline was seen, as with the 10 ppm treatment, for residues of M8. At DAT=181 days 3.7% of the 1 ppm TRR had accumulated as 14CO2. At DAT=181 days 3.2% of the 1 ppm TRR remained as the test substance.
Based on the findings, it was conclude that the degradation of the test substance was rapid. The DT50 was 3 – 16 days at 24 °C (equivalent to 4 - 21 days at 20°C) . It was very dependent on the rate of application and less depend on the kinetics model applied. Degradation of the test substance led to formation of six known metabolites, and to a complex mixture of polar, water soluble unknowns.
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 01 Oct 2004 to 13 May 2005
- 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:
- 2002
- Deviations:
- yes
- Remarks:
- The choice of these soils was required by the sponsor, based on the “Instrupao Normativa do IBAMA” (without number and date) which was under public consultation and was not published yet, and are a deviation to the OECD guideline 307.
- GLP compliance:
- yes
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 004
- Soil no.:
- #1
- Soil type:
- clay
- % Clay:
- 46
- % Silt:
- 46
- % Sand:
- 8
- % Org. C:
- 9.6
- pH:
- 4.4
- Bulk density (g/cm³):
- 0.8
- Soil no.:
- #2
- Soil type:
- clay
- % Clay:
- 62
- % Silt:
- 34
- % Sand:
- 4
- % Org. C:
- 2
- pH:
- 4.1
- Bulk density (g/cm³):
- 1.1
- Soil no.:
- #3
- Soil type:
- loamy sand
- % Clay:
- 5
- % Silt:
- 91
- % Sand:
- 4
- % Org. C:
- 0.3
- pH:
- 4.9
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #4
- Soil type:
- clay
- % Clay:
- 40
- % Silt:
- 34
- % Sand:
- 26
- % Org. C:
- 2.8
- pH:
- 5.6
- Bulk density (g/cm³):
- 1.4
- Details on soil characteristics:
- SOIL COLLECTION AND STORAGE
- Geographic location: Gleissolo Melanico Aluminico tipico (GM) soil was sampled from a hygrophyte vegetation area. Argissolo Vermelho Eutrofdrrico chemossolico (PV) soil was sampled from pastures. Latossolo Vermelho Distroférrico tipico (LVdf) and Neossolo Quartzarenico Órtico tipico (RQ) soils were sampled from forest vegetation. The geographic coordinates of the sampling points were 22°35’23” S and 47°35’69” W, 22°45’18” S and 47°53’75” W, 22°40’20” S and 47°37’31” W and 22°37’27” S and 47°36’67” W for GM, RQ, PV and LVdf soils, respectively.
- Pesticide use history at the collection site: No pesticides were ever applied on the four site.
- Soil samples were analyzed for various chemical and physical properties that are considered to be important for the mobility of chemicals in the soil.
- Sampling depth (cm): Between 0- 20 cm
- Soil preparation: Airdried and sieved using a 2 mm mesh - Duration:
- 120 d
- Initial conc.:
- 24.75 mg/kg soil d.w.
- Based on:
- test mat.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Temp.:
- 20 °C
- Humidity:
- 40%
- Details on experimental conditions:
- EXPERIMENTAL DESIGN
- Soil condition: Air dried
- Soil (g/replicate): 60 g
- No. of replication control: 2
- No. of flasks per type pf soil: 20 (Nineteen of those (9 including zero time observation periods, in duplicate) were used to measure the dissipation of the test item).
- Test apparatus: 250 mL Erlenmeyer flasks equipped with a trapping system. The apparatus was formed by eight interconnected Erlenmeyer flasks (250 mL volume).
- Air flow: A vacuum pump was connected at the end of the line which was controlled by timer working 1 h each two hours. The air flow in the apparatus was controlled (10 - 20 mL/min) by needle valve. Every day, the air flow was measured for each apparatus, using a flow meter. The aerobic samples were stored under ventilation with moistened air (flow-rate: 10 - 20 mL/min) in incubation chambers.
PREPARATION OF THE APPLICATION SOLUTION
- Test concentration: The concentration of the test substance employed in this assay was 148.5 µg/60 g soil (maximum used rate at field conditions - MUR = 2475 g a.i./ha), based on the top 10 cm soil layer and considering a density of 1.0 g/cm3.
- Solution A: 20.18 mg of the test substance analytical grade were dissolved in 20 mL of acetonitrile, resulting in a solution with concentration of 1.0 mg/mL.
- Solution B: The 14C-labelled test substance was dissolved in 10 mL of acetonitrile, giving a solution with concentration of 1.97 MBq/mL with 929.24 µg/mL.
- Treatment solution: 11359.6 µL of solution A and 3751.6 µL of solution B were taken and dissolved in 4888.8 µL of acetonitrile, resulting in a solution containing 742.5 µg/mL (0.37 MBq/mL).
- Treatment: The compound was added individually (200 µL), drop wise to the soil surface (each flask) (by means of a syringe) as a solution in acetonitrile. Then, the soil was carefully mixed with a spatula to ensure good mixing and contact of the treatment solution with the soil. In addition, an equivalent volume of test solution was placed in a 10-mL volumetric flask for direct determination of the added radioactivity.
- Moisture maintenance: Yes, at 40 % of maximum water holding capacity.
SAMPLING DETAILS
- Sampling intervals: The measurements of 14CO2 evolution and 14C-labelled organic volatiles, as well as the extractions for characterization of the extractable radioactivity were performed at the following intervals: 0, 1, 3, 7, 14, 28, 60, 90 and 120 days for GM, LVdf, RQ and PV soils. - Soil No.:
- #1
- % Total extractable:
- 36.84
- % Non extractable:
- 42.93
- % CO2:
- 11.3
- % Recovery:
- 91.08
- Remarks on result:
- other: on day 120
- Soil No.:
- #2
- % Total extractable:
- 52.62
- % Non extractable:
- 34.23
- % CO2:
- 10.06
- % Recovery:
- 96.92
- Remarks on result:
- other: on day 120
- Soil No.:
- #3
- % Total extractable:
- 58.89
- % Non extractable:
- 26.17
- % CO2:
- 8.92
- % Recovery:
- 93.98
- Remarks on result:
- other: on day 120
- Soil No.:
- #4
- % Total extractable:
- 48.25
- % Non extractable:
- 34.7
- % CO2:
- 8.31
- % Recovery:
- 91.26
- Remarks on result:
- other: on day 120
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 98.69
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 98.81
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 99.58
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Parent/product:
- parent
- Soil No.:
- #4
- % Degr.:
- 93.16
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Key result
- Soil No.:
- #2
- DT50:
- 4.73 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 6.82 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #4
- DT50:
- 9.45 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Soil No.:
- #1
- DT50:
- 2.96 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: The organic carbon and pH of soil content are not representative of global agriculture. Thus, the adsorption coefficient is not considered as key result.
- Transformation products:
- not specified
- Details on transformation products:
- M9 was the major metabolite in this study, increasing during incubation time. This metabolite reached at maximum 20.96 % at 90 days of incubation for RQ soil and 7.90 %, 13.38 % and 5.95 % at 120 days of incubation for GM, LVdf and PV soil, respectively. M4 also identified for all soils, from first day of incubation for RQ soil and third day for GM, LVdf and PV soil. M4 was detected in low concentrations, except at 7 days, when it reached values of 3.25 %, 9.14 %, 8.73 % and 5.60 % for GM, LVdf, RQ and PV soil, respectively. Unknown metabolite 1 was detected after 14 days. The percentage of unknown metabolite 1 ranged from 3.42 % to 6.55% in GM soil, 5.01 % to 8.86 % in LVdf, 5.28 % to 8.85% in RQ soil and from 5.81 % to 8.57 % in PV soil. Unknown metabolite 3 was also observed after 14 days of incubation, with percentages ranging from 0.82 % to 1.19 % in GM soil, 2.58 % to 8.40 % in LVdf soil, 2.13 % to 8.42 % in RQ soil and from 0.04 % to 3.73 % in PV soil. Other minor metabolites M1 and M5 , unknown metabolite 2 and unknown metabolite 4 were detected.
- Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results is provided in Table 1 - Table 11 in ‘Any other information on results incl. tables’.
- Microbial Activity: Results showed that soil microbial activity was stimulated by the molecule in GM, LVdf, RQ and PV soils.
- Balance of Radioactivity: Radioactivity recovery ranged from 90.00 % to 98.79 % of the total applied in the GM soil, from 94.74 % to 101.73 % in the LVdf soil, from 91.48% to 103.74 % in the RQ soil and from 90.95 % to 97.85 % in the PV soil.
- 14CO2 Evolution: At the end of the incubation time 120 days, the cumulative percentages of 14CO2 evolved were 11.30 %, 10.06 %, 8.92 % and 8.31 % of the applied radioactivity from GM, LVdf, RQ and PV soils, respectively.
- 14C-labelled organic volatile: No significant organic volatile were observed for any of the studied soils.
- Extraction and Characterization of the Extracted Radioactivity: The extracted radioactivity decreased from 98.79%, 101.13%, 103.74% and 97.85% at the beginning of the study to 36.84%, 52.62%, 58.89% and 48.25% at the end of the experiment, for GM, LVdf, RQ and PV soils, respectively. The test substance was degraded in all studied soils. After 120 days, the percentage of the test substance decreased in the extract from 88.60 to 1.31 % (in GM), from 93.81 to 1.19 %(in LVdf), from 103.16 to 0.42 % (in RQ) and from 97.85 to 6.84 % (in PV). At the end of the test (120 days), the percentage of the test substance in relation to the total radioactivity recovered was 1.31 %, 1.19 %, 0.42 % and 6.84 % for GM, LVdf RQ and PV soils respectively.
- Unextractable Radioactivity: Non-extractable residues increased throughout the incubation period for all four studied soils. They increased from 7.69 %, 6.54 %, 0.38 % and 4.62 % at the beginning of the experiment (1 day after the application of the test substance), to 42.93 %, 34.23 %, 26.17 % and 34.70 %, at the end of the test (120 days) in the GM, LVdf, RQ and PV soils, respectively.
- Organic Matter fractionation: At the end of the incubation time 120 days, the non-extractable fraction was submitted to organic matter fractionation. The major part of the radioactivity of the non-extractable was found in the humin fraction which amounted to 20.27%, 14.18%, 7.64% and 17.33% of the applied radioactivity for GM, LVdf, RQ and PV soils, respectively.
HALF LIVES
Two-compartment model was used to fit the degradation of the test substance in GM, LVdf RQ and PV soils. The half-lives for the test substance in the GM, LVdf, RQ and PV soils were respectively 2.96, 4.73, 6.82 and 9.45 days. - Conclusions:
- Based on the reuslts, the DT50 values for the test substance in the GM, LVdf, RQ and PV soils were respectively 2.96, 4.73, 6.82 and 9.45 days.
- Executive summary:
In the present study, the degradation rate of [14C]-labelled test substance was investigated in four Brazilian agricultural soils incubated under aerobic conditions for a period of up to 120 days. The study was conducted according to OECD TG 307 and in compliance with GLP criteria. The four Brazilian soil types used in the study were as follows: Gleissolo Melanico Aluminico tipico (GM), Latossolo Vermelho Distroferrico tipico (LVdf), Neossolo Quartzarenico Ortico tipico (RQ) and Argissolo Vermelho Eutroferrico chemossdlico (PV). The freshly collected soils were passed through a 2 mm sieve. The test item was applied to 60 g soil samples in Erlenmeyer flasks (250 mL volume) at a concentration of 24.75 mg/kg corresponding to a field application rate of 2475 g a.i./ha assuming an even distribution of the test item in the top 10 cm soil. The experiment was carried out in duplicate. Soil moisture was maintained during the incubation time at 40% of the maximum water holding capacity and the temperature of the incubation dark room was 19 - 21 °C. The exiting air was passed through a trapping system consisting of flasks of ethylene glycol and sodium hydroxide in series. Duplicate samples treated with the test item were taken immediately after treatment (day 0) and after, 1, 3, 7, 14, 28, 60, 90 and 120 days after the test substance application. Soil microbial activity was measured at 0 and 120 days after the application. The samples were submitted to solvent extractions using acetonitrile/water. The combined and concentrated extracts were then analysed by HPLC for the test item and degradation products. A total balance of radioactivity, the nature of extracted radioactivity and pattern of metabolites were established for each sampling interval.
The overall recovery comprising the soil extracts, non-extractable fraction and volatile products ranged from 90.00% to 98.79% in the GM, from 94.74% to 101.13% in the LVdf, from 92.86% to 103.74% in the RQ and from 90.95% to 97.85% of total applied radioactivity in the PV soil. The extractable radioactivity decreased from 98.79%, 101.13%, 103.74% and 97.85%, at the beginning of the study to 36.84%, 52.62%, 58.89% and 48.25% at the end for GM, LVdf, RQ and PV soils, respectively. Non-extractable residues increased throughout the incubation period for all four soils and reached a level of 42.93%, 34.23%, 26.17% and 34.70% for GM, LVdf, RQ and PV soils, respectively, at the end of the study. At the end of incubation period (120 days), the cumulative percentage of 14CO2 evolved in the GM, LVdf, RQ and PV soils were respectively 11.30%, 10.06%, 8.92% and 8.31% of applied radioactivity. No significant organic volatiles were generated during the experimental phase, in any of the four studied soils. The test substance declined from mean levels of between 88.60%, 93.81%, 103.18% and 97.85% of the applied radioactivity on day 0 to 1.31%, 1.19%, 0.42% and 6.84% in soils GM, LVdf, RQ and PV after 120 days of aerobic incubation.
M9 was the major metabolite in this study, increasing during incubation time. This metabolite reached at maximum 20.96 % at 90 days of incubation for RQ soil and 7.90 %, 13.38 % and 5.95 % at 120 days of incubation for GM, LVdf and PV soil, respectively. M4 also identified for all soils, from first day of incubation for RQ soil and third day for GM, LVdf and PV soil. M4 was detected in low concentrations, except at 7 days, when it reached values of 3.25 %, 9.14 %, 8.73 % and 5.60 % for GM, LVdf, RQ and PV soil, respectively. Unknown metabolite 1 was detected after 14 days. The percentage of unknown metabolite 1 ranged from 3.42 % to 6.55% in GM soil, 5.01 % to 8.86 % in LVdf, 5.28 % to 8.85% in RQ soil and from 5.81 % to 8.57 % in PV soil. Unknown metabolite 3 was also observed after 14 days of incubation, with percentages ranging from 0.82 % to 1.19 % in GM soil, 2.58 % to 8.40 % in LVdf soil, 2.13 % to 8.42 % in RQ soil and from 0.04 % to 3.73 % in PV soil. Other minor metabolites M1 and M5, unknown metabolite 2 and unknown metabolite 4 were detected. The half-lives of the test substance in the soils were 2.96, 4.73, 6.82 and 9.45 days for GM, LVdf, RQ and PV soils, respectively.
- Endpoint:
- biodegradation in soil: simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 01 May 2014 to 02 Mar 2015
- 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:
- 2002
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- EPA OPPTS 835.4100 (Aerobic Soil Metabolism)
- Version / remarks:
- 2008
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Test type:
- laboratory
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Soil classification:
- USDA (US Department of Agriculture)
- Year:
- 2 014
- Soil no.:
- #1
- Soil type:
- loam
- % Clay:
- 12
- % Silt:
- 43
- % Sand:
- 45
- % Org. C:
- 2
- pH:
- 7.5
- CEC:
- 10.8 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #2
- Soil type:
- sandy clay loam
- % Clay:
- 25
- % Silt:
- 24
- % Sand:
- 51
- % Org. C:
- 3.3
- pH:
- 5.9
- CEC:
- 18.9 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #3
- Soil type:
- sandy loam
- % Clay:
- 14
- % Silt:
- 21
- % Sand:
- 65
- % Org. C:
- 2.3
- pH:
- 7.5
- CEC:
- 12.1 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Soil no.:
- #4
- Soil type:
- clay loam
- % Clay:
- 29
- % Silt:
- 36
- % Sand:
- 35
- % Org. C:
- 0.8
- pH:
- 7.9
- CEC:
- 21.2 meq/100 g soil d.w.
- Bulk density (g/cm³):
- 1.5
- Details on soil characteristics:
- SOIL COLLECTION AND STORAGE
- Information of geographic location, pesticide use history at the collection site, sampling depth and physico-chemical Properties of Test Soils is provided in Table 1 in 'Any other information on materials and methods incl.tables'.
- Storage conditions: The soils were stored under aerobic conditions in a fridge set to maintain 4 ºC for between 47 and 72 days after arrival at the test facility.
- Soil preparation: Following receipt, the soils were sieved (2 mm) in a fresh state (i.e. not dried) and the moisture content adjusted to close to pF 2. After 47 - 72 days storage, soil samples were weighed into individual 250 mL capacity Duran flasks (134.8 g of nominal weight of Gartenacker soil per flask, 128.1 g of nominal weight of 18 Acres soil per flask, 122.6 g of nominal weight of East Anglia per flask and 117.2 g of nominal weight of Capay soil per flask). A total of 24 test flasks and 8 biomass flasks were prepared for each soil. Soil samples were acclimatised under test conditions for between 5 and 10 days prior to application of the test item.
- Soil No.:
- #1
- Duration:
- 122 d
- Soil No.:
- #2
- Duration:
- 122 d
- Soil No.:
- #3
- Duration:
- 122 d
- Soil No.:
- #4
- Duration:
- 120 d
- Initial conc.:
- 16.89 mg/kg soil d.w.
- Based on:
- test mat.
- Remarks:
- equivalent to 12.665 kg ai/ha
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Soil No.:
- #1
- Temp.:
- 20 ± 2 °C
- Humidity:
- pF2
- Microbial biomass:
- 1.1 (start) and 0.7 (end) % organic carbon
- Soil No.:
- #2
- Temp.:
- 20 ± 2 °C
- Humidity:
- pF
- Microbial biomass:
- 0.6 (start) and 0.6 (end) % organic carbon
- Soil No.:
- #3
- Temp.:
- 20 ± 2 °C
- Humidity:
- pF2
- Microbial biomass:
- 0.5 (start) and 0.7 (end) % organic carbon
- Soil No.:
- #4
- Temp.:
- 20 ± 2 °C
- Humidity:
- pF2
- Microbial biomass:
- 0.8 (start) and 0.9 (end) % organic carbon
- Details on experimental conditions:
- An overview of the experimental design is provided in Table 2 and Table 3 in 'Any other information on materials and methods incl. tables'.
- Radiochemical purity: The radiochemical purity of the stock [14C]-labelled test substance was determined by TLC and HPLC. The radiochemical purity of the [14C]-labelled test substance in the treatment solutions was determined by TLC and HPLC prior to application.
PREPARATION AND APPLICATION OF TREATMENT SOLUTIONS
- Gartenacker, 18 Acres and East Anglia soil treatment solution: A stock solution of the radiolabelled test item was prepared by dissolving a small amount of the supplied [14C]-labelled test substance in acetone (2 mL). The radioactive content was determined as 127.5 MBq. A solution of non-labelled chlorothalonil was prepared by dissolving 200 mg of the test substance in 13 mL of acetone. 1.73 mL of the [14C]-labelled test substance solution was added to the non-labelled solution and ultrasonicated. The solution was concentrated under a gentle stream of N2 gas, to a final volume of ca 13 mL. Concentration and homogeneity were determined by LSC analysis. Specific activity was determined by LSC and HPLC. The radiochemical purity of [14C]-chlorothalonil in the treatment solution was determined by TLC and HPLC prior to application to the soil samples.
- Capay soil treatment solution: A stock solution of the radiolabelled test item was prepared by dissolving a small amount of the supplied [14C]-labelled test substance in acetone (1 mL). The radioactive content was determined as 39.0 MBq. A solution of non-labelled chlorothalonil was prepared by dissolving 70 mg of the test substance in 4 mL of acetone. 0.88 mL of the [14C]-labelled test substance solution was added to 3.62 mL non-labelled solution and ultrasonicated. Concentration and homogeneity were determined by LSC analysis. Specific activity was determined by LSC and HPLC. The radiochemical purity of [14C]-chlorothalonil in the treatment solution was determined by TLC and HPLC prior to application to the soil samples.
- Application of [14C]- labelled test substance: The nominal treatment rate was 16.89 µg/g or 1689 µg per 100 g oven dried soil. The application rate was equivalent to 12665 g a.i./ha assuming a soil incorporation depth of 5cm and a soil bulk density of 1.5 g/cm3.A pipette was used to apply the treatment solution to the samples. Treatment solution (90 - 100 µL; equivalent to 0.1% of the dry soil weight) was applied drop-wise to each sample. Following application, each flask was gently tumbled to incorporate the [14C]-laeblled test substance and then connected to the flow apparatus. Gartenacker, 18 Acres and East Anglia soil samples were treated on 06 June 2014. Capay soil samples were treated on 08 July 2014. To accurately quantify the amount of test item applied to each sample, aliquots of treatment solution (mock doses) were dispensed directly into 10 mL volumetric flasks at regular intervals during treatment. Each mock dose flask was made to volume with acetone and aliquots (3 x 100 µL) taken for LSC analysis. The amount of radioactivity applied to each soil sample was calculated as ca 0.81- 1.04 MBq (equivalent to 1746.4 – 1997.4 µg).
EXPERIMENTAL PROCEDURES
- Incubation of treated soil vessels: The soil flasks were wrapped in foil to eliminate light and incubated in the dark in a temperature controlled room at nominal temperature of 20 ± 2 ºC. The temperature of the room was measured and recorded at regular intervals. To maintain aerobic conditions, moist air was introduced to the test system at a flow rate of one bubble per trap at any time using a vacuum pump. The total weight of each soil sample was recorded prior to test item application. The moisture content of the samples was checked at regular intervals (ca every 1-2 week) by re-weighing the samples. Any weight loss relative to the pF 2 target weights was attributed to soil moisture loss and water was added to restore the original soil sample weight.
- Trapping of volatile products: The effluent gases leaving each soil flask were passed sequentially through a series of traps the first being aqueous NaOH (2M) to trap liberated 14CO2 then an ethylene glycol trap to trap non-specific organic [14C]-volatile compounds.
- Sampling: Duplicate samples were taken for analysis from Gartenacker, 18 Acres and East Anglia soils immediately following application (0 h) and at 6 h, then at 1, 3, 7, 14, 31, 60, 90 and 122 DAT. Duplicate samples were taken for analysis from Capay soil immediately following application (0 h) and at 6 h, then at 1, 3, 7, 14, 30, 59, 91 and 120 DAT. The contents of the 14 CO2 traps (aqueous 2M sodium hydroxide) were sampled and replenished (at 31, 60, 90 and 122 DAT for Gartenacker, 18 Acres and East Anglia soils and at 30, 59, 91 and 120 DAT for Capay soil), the total weight of each trapping solution was measured and duplicate aliquots (ca 0.5 g) analysed by LSC. The ethylene glycol (ethandiol) traps were treated in the same way.
- Sample extraction and analysis: See Table 3 in "Ant other ifnormation on materials and methods incl. tabels" - Soil No.:
- #1
- % Total extractable:
- 49.4
- % Non extractable:
- 31.1
- % CO2:
- 5.5
- % Recovery:
- 86
- Remarks on result:
- other: on day 122
- Soil No.:
- #2
- % Total extractable:
- 55.2
- % Non extractable:
- 28.4
- % CO2:
- 3.6
- % Recovery:
- 87.1
- Remarks on result:
- other: on day 122
- Soil No.:
- #3
- % Total extractable:
- 55.2
- % Non extractable:
- 22.8
- % CO2:
- 7.3
- % Recovery:
- 85.3
- Remarks on result:
- other: on day 122
- Soil No.:
- #4
- % Total extractable:
- 79.5
- % Non extractable:
- 10.2
- % CO2:
- 0.2
- % Recovery:
- 89.8
- Remarks on result:
- other: on day 120
- Parent/product:
- parent
- Soil No.:
- #1
- % Degr.:
- 97
- Parameter:
- radiochem. meas.
- Sampling time:
- 122 d
- Parent/product:
- parent
- Soil No.:
- #2
- % Degr.:
- 98.1
- Parameter:
- radiochem. meas.
- Sampling time:
- 122 d
- Parent/product:
- parent
- Soil No.:
- #3
- % Degr.:
- 98.1
- Parameter:
- radiochem. meas.
- Sampling time:
- 122 d
- Parent/product:
- parent
- Soil No.:
- #4
- % Degr.:
- 83.8
- Parameter:
- radiochem. meas.
- Sampling time:
- 120 d
- Key result
- Soil No.:
- #1
- DT50:
- 11 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #2
- DT50:
- 12 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #3
- DT50:
- 7 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Key result
- Soil No.:
- #4
- DT50:
- 58 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Transformation products:
- not measured
- Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results is provided in Table 4 - Table12 in ‘Any other information on results incl. tables’.
RECOVERY OF RADIOACTIVITY
- Radiochemical Purity: The radiochemical purity of [14C]-labelled test substance were ≥ 95.8% and ≥ 99.4%, respectively. The radiochemical purity of [14C]-labelled test substance in the treatment solution prior to application to the soils was determined as ≥ 99.0% by HPLC and ≥ 99.5% by TLC.
- Treatment Rate: Each soil sample received 0.81 – 1.04 MBq (48,393,900 – 62,319,300 dpm) of [14C]-labelled test substance. This is equivalent to a treatment rate of 17.46 – 19.97 μg a.i./g oven dry soil (which is equivalent to a field application rate of 13098 - 14981 g a.i./ha).
- Mass balance: The overall mass balance was 92.4%, 91.2%, 91.1% and 92.3% AR in Gartenacker, 18 Acres, East Anglia and Capay soils, respectively. Four Gartenacker samples had a mass balance of < 90% (range 84.3% - 89.7% AR). Six 18 Acres samples had a mass balance of < 90% (range 83.6% - 89.9% AR). Six East Anglia samples had a mass balance of < 90% (range 83.8% - 88.9% AR). Six Capay samples had a mass balance of <90% (range 85.8% - 89.2% AR). This is deemed to have no impact on the overall outcomes of the study as the majority of samples had a mass balance > 90% AR and the overall mean recovery for each soil was > 90% AR. Non-extracted residues (bound residues) increased throughout the incubation, reaching a maximum mean of 31.1%, 28.4% and 22.8% AR at 122 DAT in Gartenacker, 18 Acres and East Anglia soils, respectively and a maximum mean of 10.2% AR in Capay soil by 120 DAT.
Mineralization to 14CO2, reached a cumulative maximum mean of 5.5%, 3.6%, 7.3% and 0.2% AR by the end of incubations, for Gartenacker, 18 Acres, East Anglia and Capay soils, respectively. The presence of 14CO2 in Gartenacker and East Anglia sodium hydroxide traps was confirmed by precipitation with BaCl2 in the 122 DAT samples. Radioactivity recovered as non-specific organic [14C]-volatile compounds in the ethylene glycol traps was- Distribution of Radioactive Residues: For all soils, the amount of radioactivity in extracts was high at all time points. The amount of extractable radioactivity across all soil samples decreased with time from a mean of 98.8% at 0 DAT to 59.8% AR by 120 - 122 DAT.
- Radioactive residues in soil extracts: In all soils, unchanged test substance accounted for most of the radioactivity present in the aqueous/organic extracts at 0 DAT but decreased with time. Levels of test substance decreased from a mean of 93.0%, 94.5% and 97.0 at 0 DAT to a mean of 4.6%, 3.0% and 1.9% AR at 122 DAT, in Gartenacker, 18 Acres and East Anglia soils, respectively. Levels of test substance decreased from a mean of 106.2% AR at 0 DAT to a mean of 16.2% AR at 120 DAT, in Capay soil.
DEGT50 VALUES
The degradation rate (DegT50) of the test substance was determined using non-linear regression and a single first order kinetic model (SFO), the DegT50 were 11, 12, 7 and 58 days in Gartenacker, 18 Acres, East Anglia and Capay soils, respectively. SFO kinetics describes the degradation of the test substance very well with a Chisquare (χ2) value less than or equal to 9.3 in all cases and R2 values ranged from 0.96 - 0.99. - Conclusions:
- The DT50 values in Gartenacker, 18 Acres, East Anglia and Capay soils were 11, 12, 7 and 58 days, respectively.
- Executive summary:
The aerobic rate of degradation of [14C]-labelled test substance was investigated in four different soils: Gartenacker (loam, Switzerland), 18 Acres (sandy clay loam, UK), East Anglia (sandy loam, UK) and Capay (clay loam, USA). The study was conducted according to OECD TG 307 and EPA Guideline 835.4100 and was in compliance with GLP criteria. [14C]-labelled test substance was applied at a nominal rate of 16.89 mg/kg dry weight soil, equivalent to a single field application rate of 12665 g a.i./ha (assuming an incorporation depth of 5 cm and a bulk density of 1.5 g/cm3). The soils were incubated under aerobic conditions and maintained in the dark at 20 ± 2°C and a soil moisture of pF 2 for up to 122 days. For Gartenacker, 18 Acres and East Anglia soils, duplicate samples were taken for analysis at 0, 6 h and 1, 3, 7, 14, 31, 60, 90, 122 days after treatment (DAT). For Capay soil, duplicate samples were taken for analysis at 0, 6 h and 1,3, 7, 14, 30, 59, 91, 120 days after treatment (DAT). At each sampling time, samples were extracted twice with acetonitrile:0.3M HCl (4:1 v/v;200 mL) and twice with acetonitrile:1.5M HCl (4:1 v/v; 200 mL). Samples were analysed for extractable test substance and non-extracted residues. Any volatile radioactivity was continuously flushed from the vessels and collected in traps. A mass balance was determined for each sample.
The mean mass balance from all soils was 91.8% (range 83.6 – 107.6% applied radioactivity (AR). A number of samples had a mass balance < 90% AR. This is deemed to have no impact on the overall outcomes of the study, as the majority of samples had a mass balance > 90% AR and the overall mean recovery for each soil was > 90% AR. For all soils, extractability was high at 0 DAT and decreased with time. The amount of extractable radioactivity across all soil samples decreased with time from a mean of 93.9 - 106.5% at 0 DAT to 49.4 - 79.5% AR by 122 DAT. Non-extracted residues (bound residues) increased throughout the incubation, reaching a maximum mean of 31.1%, 28.4% and 22.8% AR at 122 DAT in Gartenacker, 18 Acres and East Anglia soils, respectively and a maximum mean of 10.2% AR in Capay soil by 120 DAT.
Radioactivity recovered as evolved carbon dioxide in NaOH traps reached a cumulative mean of 5.5%, 3.6%, 7.3% and 0.2% AR by the end of incubations, for Gartenacker, 18 Acres, East Anglia and Capay soils, respectively. Radioactivity recovered as non-specific organic [14C]-volatile compounds in the ethylene glycol traps was less than the limit of quantification (< LOQ) in all soils. Unchanged test substance accounted for a mean of 93.0%, 94.5%, 97.0% and 106.2% AR at 0 DAT in Gartenacker, 18 Acres, East Anglia soil and Capay respectively. By 122 DAT (Capay 120 DAT) the levels of parent decreased to 4.6%, 3.0%, 1.9% and 16.2% AR, in Gartenacker, 18 Acres, East Anglia and Capay soils, respectively. The amount of unchanged test substance extracted from the soil decreased over time. The rate of degradation in the 4 soils was estimated using single first order kinetics. Based on the results, the degradation half-lives of [14C]-labelled test substance in Gartenacker, 18 Acres, East Anglia and Capay soils were determined to be 11, 12, 7 and 58 days, respectively.
Referenceopen allclose all
Table 1. Distribution and Recovery of Radioacivity: Marsillargues
Fraction |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
|||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
||
Extract 1(a) |
A |
98.5 |
96.0 |
79.3 |
88.3 |
69.8 |
57.3 |
61.8 |
48.2 |
44.7 |
42.2 |
B |
97.1 |
97.6 |
84.7 |
94.2 |
70.4 |
61.9 |
55.7 |
51.3 |
47.4 |
43.0 |
|
Mean |
97.8 |
96.8 |
82.0 |
91.3 |
70.1 |
59.6 |
58.8 |
49.8 |
46.1 |
42.6 |
|
Extract 2(b) |
A |
2.6 |
1.9 |
1.0 |
2.0 |
2.7 |
3.5 |
3.7 |
2.9 |
2.6 |
2.5 |
B |
3.0 |
1.7 |
2.6 |
2.2 |
2.3 |
2.5 |
4.1 |
2.4 |
2.8 |
3.1 |
|
Mean |
2.8 |
1.8 |
1.8 |
2.1 |
2.5 |
3.0 |
3.9 |
2.7 |
2.7 |
2.8 |
|
Extract 3(b) |
A |
0.2 |
0.3 |
0.6 |
0.4 |
1.2 |
1.5 |
1.2 |
1.8 |
2.8 |
1.5 |
B |
0.2 |
0.4 |
0.3 |
0.2 |
1.2 |
1.5 |
1.2 |
1.4 |
1.7 |
1.6 |
|
Mean |
0.2 |
0.4 |
0.5 |
0.3 |
1.2 |
1.5 |
1.2 |
1.6 |
2.3 |
1.6 |
|
Total Extractable |
Mean |
100.8 |
99.0 |
84.3 |
93.7 |
73.8 |
64.1 |
63.9 |
54.1 |
51.1 |
47.0 |
Non- Extractables(c) |
A |
0.3 |
1.6 |
2.3 |
1.4 |
20.7 |
23.2 |
26.5 |
31.3 |
33.3 |
38.5 |
B |
0.3 |
1.4 |
1.3 |
1.4 |
17.3 |
17.6 |
28.7 |
32.3 |
35.5 |
38.2 |
|
Mean |
0.3 |
1.5 |
1.8 |
1.4 |
19.0 |
20.4 |
27.6 |
31.8 |
34.4 |
38.4 |
|
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.7 |
1.3 |
3.0 |
6.3 |
8.8 |
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.5 |
1.7 |
3.8 |
4.3 |
8.3 |
|
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.6 |
1.5 |
3.4 |
5.3 |
8.6 |
|
Other Volatiles (Orbo Tubes) |
A |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Total % recovery |
A |
101.6 |
99.8 |
83.2 |
92.1 |
94.4 |
86.2 |
94.5 |
87.2 |
89.7 |
93.5 |
B |
100.6 |
101.2 |
88.9 |
98.0 |
91.3 |
84.0 |
91.4 |
91.2 |
91.7 |
94.2 |
|
Mean |
101.1 |
100.5 |
86.1 |
95.1 |
92.9 |
85.1 |
93.0 |
89.2 |
90.7 |
93.9 |
|
Overall Mean ± SD |
92.7 ± 5.5 |
||||||||||
(a) = Acetonitrile:0.3MHCl(8:2,v/v)x 2extractions
(b) = Acetonitrile:1.5M HCl (8:2, v/v)
(c) = Unextracted residue further investigated at 120DATusing reflux and organic matter fractionation NS = Nosample
NA = Not analysed
Table 2. Distribution and Recovery of Radioacivity: 18 Acres
Fraction |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
|||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
||
Extract 1(a) |
A |
99.5 |
97.2 |
85.3 |
93.1 |
67.5 |
66.8 |
54.0 |
59.7 |
50.4 |
45.6 |
B |
99.2 |
97.7 |
95.1 |
93.8 |
76.8 |
62.4 |
58.0 |
52.9 |
50.5 |
49.0 |
|
Mean |
99.4 |
97.5 |
90.2 |
93.5 |
72.2 |
64.6 |
56.0 |
56.3 |
50.5 |
47.3 |
|
Extract 2(b) |
A |
2.8 |
2.9 |
2.7 |
3.6 |
6.5 |
5.8 |
9.3 |
8.4 |
7.9 |
8.4 |
B |
3.4 |
2.9 |
3.6 |
3.6 |
6.3 |
5.3 |
9.6 |
1.6 |
8.0 |
8.4 |
|
Mean |
3.1 |
2.9 |
3.2 |
3.6 |
6.4 |
5.6 |
9.5 |
5.0 |
8.0 |
8.4 |
|
Extract 3(b) |
A |
0.5 |
0.7 |
0.9 |
0.9 |
2.8 |
4.7 |
3.6 |
4.0 |
4.4 |
4.6 |
B |
0.4 |
0.6 |
1.1 |
0.9 |
0.6 |
5.7 |
3.7 |
7.4 |
2.8 |
3.3 |
|
Mean |
0.5 |
0.7 |
1.0 |
0.9 |
1.7 |
5.2 |
3.7 |
5.7 |
3.6 |
4.0 |
|
Total Extractable |
Mean |
103.0 |
101.1 |
94.1 |
98.0 |
80.3 |
75.4 |
69.2 |
67.0 |
62.1 |
59.7 |
Non- Extractables(c) |
A |
0.6 |
1.3 |
1.3 |
2.8 |
14.1 |
17.6 |
24.2 |
21.0 |
30.1 |
27.5 |
B |
0.5 |
1.5 |
1.7 |
2.9 |
13.4 |
18.0 |
24.7 |
26.0 |
30.7 |
30.3 |
|
Mean |
0.6 |
1.4 |
1.5 |
2.9 |
13.8 |
17.8 |
24.5 |
23.5 |
30.4 |
28.9 |
|
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
2.3 |
5.5 |
2.5 |
6.0 |
9.9 |
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.3 |
3.1 |
3.2 |
6.1 |
6.7 |
6.5 |
|
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.2 |
2.7 |
4.4 |
4.3 |
6.4 |
8.2 |
|
Other Volatiles (Orbo Tubes) |
A |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Total % recovery |
A |
103.4 |
102.1 |
90.2 |
100.4 |
91.0 |
97.2 |
96.6 |
95.6 |
98.8 |
96.0 |
B |
103.5 |
102.7 |
101.5 |
101.2 |
97.4 |
94.5 |
99.2 |
94.0 |
98.7 |
97.5 |
|
Mean |
103.5 |
102.4 |
95.9 |
100.8 |
94.2 |
95.9 |
97.9 |
94.8 |
98.8 |
96.8 |
|
Overall Mean ± SD |
98.1 ± 3.8 |
||||||||||
(a) = Acetonitrile:0.3MHCl(8:2,v/v)x 2extractions
(b) = Acetonitrile:1.5M HCl (8:2, v/v)
(c) = Unextracted residue further investigated at 120DATusing reflux and organic matter fractionation NS = Nosample
NA = Not analysed
Table 3. Distribution and Recovery of Radioacivity: Gartenacker
Fraction |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
|||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
||
Extract 1(a) |
A |
91.3 |
84.0 |
86.6 |
82.5 |
65.5 |
62.9 |
54.1 |
47.8 |
40.6 |
40.2 |
B |
92.7 |
88.1 |
87.2 |
83.4 |
68.9 |
63.7 |
56.7 |
48.0 |
39.9 |
42.3 |
|
Mean |
92.0 |
86.1 |
86.9 |
83.0 |
67.2 |
63.3 |
55.4 |
47.9 |
40.3 |
41.3 |
|
Extract 2(b) |
A |
4.3 |
4.2 |
3.4 |
4.1 |
3.6 |
4.2 |
3.8 |
3.8 |
3.3 |
3.6 |
B |
4.3 |
5.2 |
4.2 |
4.4 |
4.7 |
3.8 |
4.6 |
2.0 |
3.5 |
3.7 |
|
Mean |
4.3 |
4.7 |
3.8 |
4.3 |
4.2 |
4.0 |
4.2 |
2.9 |
3.4 |
3.7 |
|
Extract 3(b) |
A |
0.4 |
0.8 |
0.8 |
0.7 |
3.8 |
3.7 |
3.8 |
4.6 |
2.8 |
5.3 |
B |
0.3 |
0.8 |
0.8 |
0.5 |
2.8 |
3.6 |
3.7 |
2.2 |
2.9 |
3.5 |
|
Mean |
0.4 |
0.8 |
0.8 |
0.6 |
3.3 |
3.7 |
3.8 |
3.4 |
2.9 |
4.4 |
|
Total Extractable |
Mean |
96.7 |
91.6 |
91.5 |
87.9 |
74.7 |
71.0 |
63.4 |
54.2 |
46.6 |
49.4 |
Non- Extractables(c) |
A |
0.8 |
3.6 |
4.4 |
12.2 |
22.6 |
25.9 |
30.3 |
29.2 |
29.4 |
32.7 |
B |
0.8 |
3.3 |
4.2 |
9.6 |
21.7 |
26.1 |
29.7 |
34.1 |
31.3 |
34.7 |
|
Mean |
0.8 |
3.5 |
4.3 |
10.9 |
22.2 |
26.0 |
30.0 |
31.7 |
30.4 |
33.7 |
|
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
0.6 |
1.5 |
5.3 |
10.4 |
7.3 |
11.1 |
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.5 |
1.5 |
1.8 |
8.7 |
8.6 |
14.4 |
|
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.6 |
1.5 |
3.6 |
9.6 |
8.0 |
12.8 |
|
Other Volatiles (Orbo Tubes) |
A |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Total % recovery |
A |
96.8 |
92.6 |
95.2 |
99.5 |
96.1 |
98.2 |
97.3 |
95.8 |
83.4 |
92.9 |
B |
98.1 |
97.4 |
96.4 |
97.9 |
98.6 |
98.8 |
96.5 |
95.0 |
86.2 |
98.6 |
|
Mean |
97.5 |
95.0 |
95.8 |
98.7 |
97.4 |
98.5 |
96.9 |
95.4 |
84.8 |
95.8 |
|
Overall Mean ± SD |
95.6 ± 4.1 |
||||||||||
(a) = Acetonitrile:0.3MHCl(8:2,v/v)x 2extractions
(b) = Acetonitrile:1.5M HCl (8:2, v/v)
(c) = Unextracted residue further investigated at 120DATusing reflux and organic matter fractionation NS = Nosample
NA = Not analysed
Table 4.Distribution and Recovery of Radioacivity: White Swan
Fraction |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
|||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
||
Extract 1(a) |
A |
94.3 |
92.3 |
90.2 |
78.0 |
63.0 |
58.1 |
51.9 |
45.9 |
47.6 |
46.8 |
B |
89.8 |
93.3 |
89.2 |
79.4 |
66.8 |
61.4 |
53.7 |
49.3 |
47.3 |
47.6 |
|
Mean |
92.1 |
92.8 |
89.7 |
78.7 |
64.9 |
59.8 |
52.8 |
47.6 |
47.5 |
47.2 |
|
Extract 2(b) |
A |
3.7 |
3.8 |
3.8 |
2.2 |
8.3 |
7.9 |
10.2 |
9.1 |
8.3 |
8.2 |
B |
3.8 |
3.9 |
5.0 |
2.2 |
8.0 |
7.9 |
9.9 |
9.1 |
8.2 |
8.4 |
|
Mean |
3.8 |
3.9 |
4.4 |
2.2 |
8.2 |
7.9 |
10.1 |
9.1 |
8.3 |
8.3 |
|
Extract 3(b) |
A |
0.5 |
0.9 |
0.3 |
1.4 |
3.2 |
3.4 |
2.8 |
3.5 |
3.9 |
3.9 |
B |
1.0 |
0.9 |
0.6 |
2.0 |
2.9 |
3.1 |
2.4 |
3.5 |
4.3 |
3.7 |
|
Mean |
0.8 |
0.9 |
0.5 |
1.7 |
3.1 |
3.3 |
2.6 |
3.5 |
4.1 |
3.6 |
|
Total Extractable |
Mean |
96.7 |
97.6 |
94.6 |
82.6 |
76.2 |
71.0 |
65.5 |
60.2 |
59.9 |
59.3 |
Non-Extractable (c) |
A |
0.3 |
1.0 |
1.6 |
16.0 |
20.3 |
22.5 |
25.2 |
27.6 |
26.3 |
31.1 |
B |
0.4 |
1.1 |
1.1 |
15.7 |
18.7 |
15.1 |
25.1 |
28.5 |
29.8 |
29.7 |
|
Mean |
0.4 |
1.1 |
1.4 |
15.9 |
19.5 |
18.8 |
25.2 |
28.1 |
28.1 |
30.4 |
|
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
0.2 |
0.3 |
0.5 |
0.8 |
1.5 |
2.4 |
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.4 |
0.4 |
1.3 |
2.3 |
2.1 |
|
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.2 |
0.4 |
0.5 |
1.1 |
1.9 |
2.3 |
|
Other Volatiles (Orbo Tubes) |
A |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
NS |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Total % recovery |
A |
98.8 |
98.0 |
95.9 |
97.6 |
95.0 |
92.2 |
90.6 |
86.9 |
87.6 |
92.4 |
B |
95.0 |
99.2 |
95.9 |
99.3 |
96.5 |
87.9 |
91.5 |
91.7 |
92.0 |
91.5 |
|
Mean |
96.9 |
98.6 |
95.9 |
98.5 |
95.8 |
90.1 |
91.1 |
89.3 |
89.9 |
92.0 |
|
Overall Mean ± SD |
93.8 ± 3.9 |
||||||||||
(a) = Acetonitrile:0.3MHCl(8:2,v/v)x 2extractions
(b) = Acetonitrile:1.5M HCl (8:2, v/v)
(c) = Unextracted residue further investigated at 120DATusing reflux and organic matter fractionation NS = Nosample
NA = Not analysed
Table 5.Summary of Characterisation/Idemtification of Radioactive Residues in Soil Extracts: Marsillargues
Component |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
||||||||||||||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
|||||||||||||
Substance |
A |
100.6 |
96.3 |
79.0 |
81.0 |
30.7 |
10.6 |
17.3 |
1.6 |
3.3 |
1.1 |
|||||||||||
B |
99.6 |
97.8 |
85.9 |
91.5 |
31.6 |
16.9 |
4.0 |
2.8 |
1.4 |
1.3 |
||||||||||||
Mean |
100.1 |
97.1 |
82.5 |
86.3 |
31.2 |
13.8 |
10.7 |
2.2 |
2.4 |
1.2 |
||||||||||||
M13 |
A |
ND |
ND |
ND |
ND |
4.5 |
5.0 |
4.3 |
3.5 |
3.1 |
2.7 |
|||||||||||
B |
ND |
ND |
ND |
ND |
4.3 |
5.7 |
4.9 |
4.5 |
4.5 |
2.6 |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
4.4 |
5.4 |
4.6 |
4.0 |
3.8 |
2.7 |
||||||||||||
M20 |
A |
ND |
ND |
ND |
ND |
(a) |
(a) |
1.1 |
(a) |
(a) |
(a) |
|||||||||||
B |
ND |
ND |
ND |
ND |
(a) |
2.4 |
ND |
(a) |
(a) |
(a) |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
(a) |
NA |
0.6 |
(a) |
(a) |
(a) |
||||||||||||
M8 |
A |
ND |
ND |
ND |
0.8 |
3.7 |
3.0 |
2.6 |
2.3 |
2.4 |
2.4 |
|||||||||||
B |
ND |
ND |
ND |
0.7 |
3.8 |
2.5 |
3.1 |
2.5 |
2.5 |
2.5 |
||||||||||||
Mean |
NA |
NA |
NA |
0.8 |
3.8 |
2.8 |
2.9 |
2.4 |
2.5 |
2.5 |
||||||||||||
M21 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.5 |
1.8 |
1.3 |
|||||||||||
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.1 |
2.1 |
1.1 |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
1.3 |
2.0 |
1.2 |
||||||||||||
M4 |
A |
ND |
0.7 |
0.7 |
5.6 |
18.7 |
23.7 |
21.3 |
22.0 |
19.1 |
21.6 |
|||||||||||
B |
ND |
0.7 |
0.8 |
2.6 |
18.0 |
21.0 |
24.5 |
22.4 |
21.8 |
22.4 |
||||||||||||
Mean |
NA |
0.7 |
0.8 |
4.1 |
18.4 |
22.4 |
22.9 |
22.2 |
20.5 |
22.0 |
||||||||||||
M5 |
A |
ND |
ND |
ND |
ND |
3.6 |
5.8 |
6.4 |
7.2 |
3.9 |
3.4 |
|||||||||||
B |
ND |
ND |
ND |
ND |
4.7 |
4.5 |
8.6 |
7.5 |
5.0 |
3.4 |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
4.2 |
5.2 |
7.5 |
7.4 |
4.5 |
3.4 |
||||||||||||
M3 |
A |
ND |
ND |
0.2 |
2.0 |
5.9 |
4.1 |
5.0 |
5.2 |
5.0 |
4.9 |
|||||||||||
B |
ND |
ND |
0.1 |
0.8 |
5.5 |
4.2 |
5.4 |
6.3 |
4.8 |
5.0 |
||||||||||||
Mean |
NA |
NA |
0.2 |
1.4 |
5.7 |
4.2 |
5.2 |
5.8 |
4.9 |
5.0 |
||||||||||||
M2 / M1(b) |
A |
ND |
ND |
ND |
0.5 |
1.0 |
1.8 |
ND |
1.4 |
2.1 |
2.0 |
|||||||||||
B |
ND |
ND |
ND |
0.3 |
0.9 |
1.8 |
1.3 |
1.7 |
1.7 |
1.8 |
||||||||||||
Mean |
NA |
NA |
NA |
0.4 |
1.0 |
1.8 |
0.7 |
1.6 |
1.9 |
1.9 |
||||||||||||
M22 / M3 (b) |
A |
ND |
ND |
ND |
0.5 |
1.3 |
2.3 |
1.4 |
0.7 |
0.8 |
0.6 |
|||||||||||
B |
ND |
ND |
ND |
0.3 |
1.4 |
2.3 |
1.9 |
0.6 |
0.7 |
0.5 |
||||||||||||
Mean |
NA |
NA |
NA |
0.4 |
1.4 |
2.3 |
1.7 |
0.7 |
0.8 |
0.6 |
||||||||||||
M10 |
A |
ND |
ND |
ND |
ND |
1.2 |
1.5 |
1.1 |
1.8 |
1.6 |
1.7 |
|||||||||||
B |
ND |
ND |
ND |
ND |
1.1 |
1.4 |
1.6 |
1.4 |
1.4 |
1.8 |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
1.2 |
1.5 |
1.4 |
1.6 |
1.5 |
1.8 |
||||||||||||
Minor Unknowns(c) |
A |
ND |
ND |
ND |
0.2 |
1.8 |
4.9 |
3.2 |
3.5 |
1.5 |
2.0 |
|||||||||||
B |
ND |
ND |
ND |
<0.1 |
2.2 |
2.9 |
2.5 |
3.5 |
1.7 |
2.4 |
||||||||||||
Mean |
NA |
NA |
NA |
0.1 |
2.0 |
3.9 |
2.9 |
3.5 |
1.6 |
2.2 |
||||||||||||
Origin Bound |
A |
0.6 |
1.0 |
0.4 |
0.2 |
0.1 |
<0.1 |
<0.1 |
0.2 |
0.1 |
<0.1 |
|||||||||||
B |
0.5 |
0.8 |
0.4 |
0.4 |
<0.1 |
0.1 |
<0.1 |
0.1 |
<0.1 |
<0.1 |
||||||||||||
Mean |
0.6 |
0.9 |
0.4 |
0.3 |
0.1 |
0.1 |
<0.1 |
0.2 |
0.1 |
<0.1 |
||||||||||||
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.7 |
1.3 |
3.0 |
6.3 |
8.8 |
|||||||||||
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.5 |
1.7 |
3.8 |
4.3 |
8.3 |
||||||||||||
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.6 |
1.5 |
3.4 |
5.3 |
8.6 |
||||||||||||
Non- Extractable |
A |
0.3 |
1.6 |
2.3 |
1.4 |
20.7 |
23.2 |
26.5 |
31.3 |
33.3 |
38.5 |
|||||||||||
B |
0.3 |
1.4 |
1.3 |
1.4 |
17.3 |
17.6 |
28.7 |
32.3 |
35.5 |
38.2 |
||||||||||||
Mean |
0.3 |
1.5 |
1.8 |
1.4 |
19.0 |
20.4 |
27.6 |
31.8 |
34.4 |
38.4 |
||||||||||||
Extracts not Profiled(d) |
A |
0.2 |
0.3 |
0.6 |
0.4 |
1.2 |
1.5 |
1.2 |
NA |
NA |
NA |
|||||||||||
B |
0.2 |
0.4 |
0.3 |
0.2 |
1.2 |
1.5 |
1.2 |
NA |
NA |
NA |
||||||||||||
Mean |
0.2 |
0.4 |
0.5 |
0.3 |
1.2 |
1.5 |
1.2 |
NA |
NA |
NA |
||||||||||||
Total |
A |
101.7 |
99.9 |
83.2 |
92.6 |
94.4 |
88.1 |
92.7 |
85.2 |
84.3 |
91.0 |
|||||||||||
B |
100.6 |
101.1 |
88.8 |
98.2 |
92.1 |
85.3 |
89.8 |
90.5 |
87.4 |
91.3 |
||||||||||||
Mean |
101.2 |
100.5 |
86.0 |
95.4 |
93.3 |
86.7 |
91.3 |
87.9 |
85.9 |
91.2 |
||||||||||||
(a) = M13 and M20 were not fully resolved in the chromatography systems usedforquantification of residues. Where the component accountedfor > 5%AR,the samples were analysed using Solvent System 3 and the % AR calculatedindividually
(b) = Minor components not fully resolved
(c) = Sumofminorunknowncomponents quantified from solvent system 2
(d) = Radioactivity in extracts accounting for a small % AR which were not subject to chromatography analysis
ND = Notdetected
NA = Not applicableNS = Nosample
Note: Residue summary compiled using a combinationofdatafromSolventSystem1, 2 and3.
Table 6.Summary of Characterisation/Idemtification of Radioactive Residues in Soil Extracts: 18 Acres
Component |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
|||||||||||||||||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
||||||||||||||||
Substance |
A |
101.8 |
98.5 |
86.6 |
90.7 |
25.0 |
20.1 |
3.5 |
6.2 |
1.8 |
1.1 |
||||||||||||||
B |
102.4 |
99.1 |
96.8 |
90.3 |
37.9 |
12.6 |
4.3 |
1.7 |
1.7 |
1.3 |
|||||||||||||||
Mean |
102.1 |
98.8 |
91.7 |
90.5 |
31.5 |
16.4 |
3.9 |
4.0 |
1.8 |
1.2 |
|||||||||||||||
M13 |
A |
ND |
ND |
ND |
ND |
3.9 |
4.3 |
2.8 |
4.6 |
2.2 |
1.3 |
||||||||||||||
B |
ND |
ND |
ND |
ND |
2.5 |
4.1 |
3.5 |
2.1 |
2.2 |
1.8 |
|||||||||||||||
Mean |
NA |
NA |
NA |
NA |
3.2 |
4.2 |
3.2 |
3.4 |
2.2 |
1.6 |
|||||||||||||||
M20 |
A |
(a) |
(a) |
(a) |
(a) |
(a) |
1.1 |
(a) |
(a) |
(a) |
(a) |
||||||||||||||
B |
(a) |
(a) |
(a) |
(a) |
(a) |
(a) |
(a) |
(a) |
(a) |
(a) |
|||||||||||||||
Mean |
(a) |
(a) |
(a) |
(a) |
(a) |
NA |
(a) |
(a) |
(a) |
(a) |
|||||||||||||||
M8 |
A |
ND |
ND |
ND |
0.4 |
3.4 |
1.9 |
2.7 |
2.8 |
1.9 |
2.2 |
||||||||||||||
B |
ND |
ND |
ND |
0.6 |
2.7 |
2.5 |
2.1 |
2.6 |
1.6 |
4.1 |
|||||||||||||||
Mean |
NA |
NA |
NA |
0.5 |
3.1 |
2.2 |
2.4 |
2.7 |
1.8 |
3.2 |
|||||||||||||||
M21 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.2 |
2.3 |
5.7 |
5.5 |
||||||||||||||
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.3 |
4.5 |
6.0 |
|||||||||||||||
Mean |
NA |
NA |
NA |
NA |
NA |
NA |
1.1 |
1.3 |
5.1 |
5.8 |
|||||||||||||||
M4 |
A |
ND |
0.4 |
0.5 |
2.0 |
14.8 |
16.9 |
13.4 |
16.9 |
9.2 |
7.3 |
||||||||||||||
B |
ND |
0.3 |
0.6 |
2.3 |
16.2 |
19.7 |
18.5 |
14.8 |
10.3 |
9.6 |
|||||||||||||||
Mean |
NA |
0.4 |
0.6 |
2.2 |
15.5 |
18.3 |
16.0 |
15.9 |
9.8 |
8.5 |
|||||||||||||||
M5 |
A |
ND |
ND |
ND |
0.3 |
3.3 |
4.6 |
5.9 |
5.5 |
5.1 |
4.3 |
||||||||||||||
B |
ND |
ND |
ND |
0.2 |
3.0 |
5.1 |
6.4 |
4.8 |
5.0 |
5.3 |
|||||||||||||||
Mean |
NA |
NA |
NA |
0.3 |
3.2 |
4.9 |
6.2 |
5.2 |
5.1 |
4.8 |
|||||||||||||||
M3 |
A |
ND |
ND |
0.2 |
1.6 |
8.3 |
8.5 |
13.2 |
11.5 |
10.0 |
10.0 |
||||||||||||||
B |
ND |
ND |
0.4 |
1.7 |
7.7 |
9.3 |
17.2 |
10.2 |
10.0 |
9.8 |
|||||||||||||||
Mean |
NA |
NA |
0.3 |
1.7 |
8.0 |
8.9 |
15.2 |
10.9 |
10.0 |
9.9 |
|||||||||||||||
M2 / M1(b) |
A |
ND |
ND |
ND |
1.5 |
2.6 |
3.1 |
3.0 |
2.3 |
5.4 |
4.7 |
||||||||||||||
B |
ND |
ND |
ND |
0.2 |
2.5 |
3.5 |
2.5 |
3.9 |
4.9 |
4.2 |
|||||||||||||||
Mean |
NA |
NA |
NA |
0.9 |
2.6 |
3.3 |
2.8 |
3.1 |
5.2 |
4.5 |
|||||||||||||||
M22 / M3(c) |
A |
ND |
ND |
ND |
0.3 |
1.9 |
2.6 |
3.2 |
2.9 |
3.0 |
2.1 |
||||||||||||||
B |
ND |
ND |
ND |
0.2 |
1.8 |
2.8 |
3.2 |
1.8 |
3.1 |
2.7 |
|||||||||||||||
Mean |
NA |
NA |
NA |
0.3 |
1.9 |
2.7 |
3.2 |
2.4 |
3.1 |
2.4 |
|||||||||||||||
M10 |
A |
ND |
ND |
ND |
ND |
2.6 |
3.8 |
6.3 |
4.8 |
5.2 |
5.0 |
||||||||||||||
B |
ND |
ND |
ND |
ND |
2.6 |
4.5 |
4.2 |
5.8 |
5.1 |
4.2 |
|||||||||||||||
Mean |
NA |
NA |
NA |
NA |
2.6 |
4.2 |
5.3 |
5.3 |
5.2 |
4.6 |
|||||||||||||||
Minor Unknowns(d) |
A |
ND |
0.3 |
<0.1 |
1.4 |
6.3 |
6.3 |
7.3 |
9.1 |
7.1 |
8.0 |
||||||||||||||
B |
ND |
0.6 |
0.1 |
2.2 |
7.4 |
6.0 |
6.6 |
10.1 |
6.8 |
7.8 |
|||||||||||||||
Mean |
NA |
0.5 |
0.1 |
1.8 |
6.9 |
6.2 |
7.0 |
9.6 |
7.0 |
7.9 |
|||||||||||||||
Origin Bound |
A |
0.5 |
0.9 |
0.8 |
0.6 |
1.0 |
0.8 |
1.8 |
2.0 |
1.8 |
2.5 |
||||||||||||||
B |
0.2 |
0.7 |
0.9 |
0.4 |
1.0 |
1.1 |
1.5 |
1.5 |
1.3 |
1.6 |
|||||||||||||||
Mean |
0.4 |
0.8 |
0.9 |
0.5 |
1.0 |
1.0 |
1.7 |
1.8 |
1.6 |
2.1 |
|||||||||||||||
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
2.3 |
5.5 |
2.5 |
6.0 |
9.9 |
||||||||||||||
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.3 |
3.1 |
3.2 |
6.1 |
6.7 |
6.5 |
|||||||||||||||
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.2 |
2.7 |
4.4 |
4.3 |
6.4 |
8.2 |
|||||||||||||||
Non- Extractable |
A |
0.6 |
1.3 |
1.3 |
2.8 |
14.1 |
17.6 |
24.2 |
21.0 |
30.1 |
27.5 |
||||||||||||||
B |
0.5 |
1.5 |
1.7 |
2.9 |
13.4 |
18.0 |
24.7 |
26.0 |
30.7 |
30.3 |
|||||||||||||||
Mean |
0.6 |
1.4 |
1.5 |
2.9 |
13.8 |
17.8 |
24.5 |
23.5 |
30.4 |
28.9 |
|||||||||||||||
Extracts not Profiled(e) |
A |
0.5 |
0.7 |
0.9 |
0.9 |
2.8 |
4.7 |
3.6 |
NA |
NA |
NA |
||||||||||||||
B |
0.4 |
0.6 |
1.1 |
0.9 |
0.6 |
5.7 |
3.7 |
NA |
NA |
NA |
|||||||||||||||
Mean |
0.5 |
0.7 |
1.0 |
0.9 |
1.7 |
5.2 |
3.7 |
NA |
NA |
NA |
|||||||||||||||
Total |
A |
103.4 |
102.1 |
90.3 |
102.5 |
90.1 |
98.6 |
98.6 |
94.4 |
94.5 |
91.4 |
||||||||||||||
B |
103.5 |
102.8 |
101.6 |
101.9 |
99.6 |
98.0 |
101.6 |
91.7 |
93.9 |
95.2 |
|||||||||||||||
Mean |
103.5 |
102.5 |
96.0 |
102.2 |
94.9 |
98.3 |
100.1 |
93.1 |
94.2 |
93.3 |
|||||||||||||||
(a) |
= |
M13 and M20 were not fully resolved in the chromatography systems used for quantification |
|
||||||||||||||||||||||
|
|
of residues. Where the component accounted for > 5% AR, the samples were analysed using Solvent |
|
||||||||||||||||||||||
|
|
System 3 and the % AR calculated individually |
|
||||||||||||||||||||||
(b) |
= |
M24 and M1 are unresolved in Solvent System 2, however, HPLC analysis of the 90 |
|
||||||||||||||||||||||
|
|
DAT sample demonstrated that M1 was detected and M2 was below the limit of |
|
||||||||||||||||||||||
|
|
quantification |
|
||||||||||||||||||||||
(c) |
= |
Minor components not fully resolved |
|
||||||||||||||||||||||
(d) |
= |
Sum of minor unknown components quantified from solvent system 2 |
|
||||||||||||||||||||||
(e) |
= |
Radioactivity in extracts accounting for a small % AR which were not subject to chromatography analysis |
|
||||||||||||||||||||||
ND |
= |
Not detected |
|
||||||||||||||||||||||
NA |
= |
Not applicable |
|
||||||||||||||||||||||
NS |
= |
No sample |
|
||||||||||||||||||||||
Note: Residue summary compiled using a combinationofdatafromSolventSystem1, 2 and3.
Table 7.Summary of Characterisation/Idemtification of Radioactive Residues in Soil Extracts: Gartenacker
Component |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
||||||||||||||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
|||||||||||||
Substance |
A |
95.2 |
80.2 |
81.8 |
52.4 |
7.0 |
2.5 |
1.1 |
0.4 |
0.5 |
0.1 |
|||||||||||
B |
96.6 |
86.5 |
83.8 |
59.7 |
11.8 |
2.3 |
1.1 |
0.4 |
0.3 |
0.2 |
||||||||||||
Mean |
95.9 |
83.4 |
82.8 |
56.1 |
9.4 |
2.4 |
1.1 |
0.4 |
0.4 |
0.2 |
||||||||||||
M13 |
A |
ND |
ND |
ND |
5.0 |
8.2 |
7.7 |
5.3 |
1.8 |
1.2 |
1.1 |
|||||||||||
B |
ND |
ND |
ND |
4.3 |
7.9 |
8.0 |
5.8 |
1.9 |
1.1 |
0.9 |
||||||||||||
Mean |
NA |
NA |
NA |
4.7 |
8.1 |
7.9 |
5.6 |
1.9 |
1.2 |
1.0 |
||||||||||||
M20 |
A |
(a) |
(a) |
(a) |
(a) |
2.1 |
0.9 |
ND |
(a) |
(a) |
(a) |
|||||||||||
B |
(a) |
(a) |
(a) |
1.1 |
2.0 |
ND |
ND |
(a) |
(a) |
(a) |
||||||||||||
Mean |
(a) |
(a) |
(a) |
0.6 |
2.1 |
0.5 |
NA |
(a) |
(a) |
(a) |
||||||||||||
M8 |
A |
ND |
0.6 |
1.0 |
1.7 |
2.4 |
2.4 |
2.0 |
1.6 |
1.6 |
1.8 |
|||||||||||
B |
ND |
0.8 |
1.0 |
1.3 |
2.5 |
2.3 |
2.4 |
1.8 |
1.9 |
1.7 |
||||||||||||
Mean |
NA |
0.7 |
1.0 |
1.5 |
2.5 |
2.4 |
2.2 |
1.7 |
1.8 |
1.8 |
||||||||||||
M21 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.2 |
2.0 |
3.2 |
2.3 |
|||||||||||
B |
ND |
ND |
ND |
ND |
ND |
ND |
0.2 |
2.0 |
2.4 |
2.7 |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
NA |
NA |
0.2 |
2.0 |
2.8 |
2.5 |
||||||||||||
M4 |
A |
0.3 |
2.6 |
4.0 |
17.1 |
30.6 |
29.7 |
28.4 |
28.8 |
23.7 |
23.1 |
|||||||||||
B |
0.3 |
2.3 |
4.1 |
14.5 |
33.8 |
29.8 |
29.0 |
27.2 |
23.7 |
26.7 |
||||||||||||
Mean |
0.3 |
2.5 |
4.1 |
15.8 |
32.2 |
29.8 |
28.7 |
28.0 |
23.7 |
24.9 |
||||||||||||
M5 |
A |
ND |
ND |
ND |
1.7 |
6.8 |
7.0 |
3.6 |
1.4 |
1.7 |
0.4 |
|||||||||||
B |
ND |
ND |
ND |
1.6 |
4.6 |
7.2 |
5.0 |
1.1 |
2.2 |
0.3 |
||||||||||||
Mean |
NA |
NA |
NA |
1.7 |
5.7 |
7.1 |
4.3 |
1.3 |
2.0 |
0.4 |
||||||||||||
M3 |
A |
ND |
1.5 |
1.1 |
4.3 |
4.6 |
6.9 |
4.5 |
4.8 |
7.7 |
4.8 |
|||||||||||
B |
ND |
1.1 |
0.1 |
3.8 |
3.2 |
7.1 |
4.7 |
5.3 |
7.0 |
2.7 |
||||||||||||
Mean |
NA |
1.3 |
0.6 |
4.1 |
3.9 |
7.0 |
4.6 |
5.1 |
7.4 |
3.8 |
||||||||||||
M2 / M1(b) |
A |
ND |
0.7 |
ND |
0.2 |
1.4 |
ND |
1.5 |
1.7 |
2.3 |
3.3 |
|||||||||||
B |
ND |
0.4 |
ND |
ND |
0.9 |
ND |
1.5 |
2.2 |
2.5 |
2.7 |
||||||||||||
Mean |
NA |
0.6 |
NA |
0.1 |
1.2 |
NA |
1.5 |
2.0 |
2.4 |
3.0 |
||||||||||||
M22 / M3(c) |
A |
ND |
ND |
ND |
0.9 |
4.3 |
6.6 |
1.8 |
1.0 |
0.5 |
0.7 |
|||||||||||
B |
ND |
ND |
ND |
1.0 |
2.8 |
9.1 |
2.3 |
1.0 |
0.6 |
0.5 |
||||||||||||
Mean |
NA |
NA |
NA |
1.0 |
3.6 |
7.9 |
2.1 |
1.0 |
0.6 |
0.6 |
||||||||||||
M10 |
A |
ND |
ND |
ND |
ND |
1.3 |
2.3 |
1.4 |
1.7 |
2.3 |
3.4 |
|||||||||||
B |
ND |
ND |
ND |
ND |
1.1 |
3.3 |
1.4 |
2.8 |
2.1 |
2.4 |
||||||||||||
Mean |
NA |
NA |
NA |
NA |
1.2 |
2.8 |
1.4 |
2.3 |
2.2 |
2.9 |
||||||||||||
Minor Unknowns(d) |
A |
ND |
1.6 |
2.0 |
2.8 |
4.1 |
9.5 |
3.2 |
1.8 |
3.1 |
6.6 |
|||||||||||
B |
ND |
1.3 |
2.3 |
2.2 |
2.1 |
12.6 |
3.8 |
4.0 |
2.7 |
3.2 |
||||||||||||
Mean |
NA |
1.5 |
2.2 |
2.5 |
3.1 |
11.1 |
3.5 |
2.9 |
2.9 |
4.9 |
||||||||||||
Origin Bound |
A |
0.1 |
1.2 |
ND |
0.1 |
<0.1 |
0.1 |
0.1 |
ND |
0.2 |
0.3 |
|||||||||||
B |
0.1 |
1.0 |
ND |
ND |
<0.1 |
<0.1 |
ND |
<0.1 |
<0.1 |
<0.1 |
||||||||||||
Mean |
0.1 |
1.1 |
NA |
0.1 |
<0.1 |
0.1 |
0.1 |
<0.1 |
0.1 |
0.2 |
||||||||||||
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
0.6 |
1.5 |
5.3 |
10.4 |
7.3 |
11.1 |
|||||||||||
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.5 |
1.5 |
1.8 |
8.7 |
8.6 |
14.4 |
||||||||||||
Mean |
NA |
<0.1 |
<0.1 |
<0.1 |
0.6 |
1.5 |
3.6 |
9.6 |
8.0 |
12.8 |
||||||||||||
Non- Extractable |
A |
0.8 |
3.6 |
4.4 |
12.2 |
22.6 |
25.9 |
30.3 |
29.2 |
29.4 |
32.7 |
|||||||||||
B |
0.8 |
3.3 |
4.2 |
9.6 |
21.7 |
26.1 |
29.7 |
34.1 |
31.3 |
34.7 |
||||||||||||
Mean |
0.8 |
3.5 |
4.3 |
10.9 |
22.2 |
26.0 |
30.0 |
31.7 |
30.4 |
33.7 |
||||||||||||
Extracts not Profiled(e) |
A |
0.4 |
0.8 |
0.8 |
0.7 |
3.8 |
3.7 |
3.8 |
4.6 |
NA |
NA |
|||||||||||
B |
0.3 |
0.8 |
0.8 |
0.5 |
2.8 |
3.6 |
3.7 |
2.2 |
NA |
NA |
||||||||||||
Mean |
0.4 |
0.8 |
0.8 |
0.6 |
3.3 |
3.7 |
3.8 |
3.4 |
NA |
NA |
||||||||||||
Total |
A |
96.8 |
92.8 |
95.1 |
99.1 |
99.8 |
106.7 |
92.5 |
91.2 |
84.7 |
91.7 |
|||||||||||
B |
98.1 |
97.5 |
96.3 |
99.6 |
97.7 |
112.9 |
92.4 |
94.7 |
86.4 |
93.1 |
||||||||||||
Mean |
97.5 |
95.2 |
95.7 |
99.4 |
98.8 |
109.8 |
92.5 |
93.0 |
85.6 |
92.4 |
||||||||||||
(a)= M13 and M20 were not fully resolved in the chromatography systems usedforquantification of residues. Where the component accountedfor > 5%AR,the samples were analysed using Solvent System 3 and the % AR calculatedindividually
(b) = Minor components not fully resolved
(c) = M22 and M3 are unresolved in SolventSystem2, however,HPLCanalysis of selected Gartenacker extracts hasshownthat M25 was below the limitofquantification
(d) = Sum of minor unknown components quantified from solvent system 2
(e) = Radioactivity in extracts accountingfora small % ARwhichwere notsubjectto chromatography analysis
ND = Notdetected NA =Not applicableNS = Nosample
Note: Residue summary compiled using a combinationofdatafromSolventSystem1, 2 and3.
Table 8.Summary of Characterisation/Idemtification of Radioactive Residues in Soil Extracts:White Swan
Component |
Rep |
Percent Applied Radioactivity Recovered at Timepoint (Days) |
|||||||||||||||||||
0 |
3 h |
6 h |
1 |
7 |
14 |
30 |
60 |
90 |
120 |
||||||||||||
Substance |
A |
97.6 |
94.4 |
91.1 |
73.6 |
29.3 |
16.9 |
10.9 |
4.6 |
3.7 |
0.5 |
||||||||||
B |
93.6 |
95.7 |
92.4 |
74.9 |
32.9 |
24.1 |
15.6 |
4.7 |
3.3 |
0.5 |
|||||||||||
Mean |
95.6 |
95.1 |
91.8 |
74.3 |
31.1 |
20.5 |
13.3 |
4.7 |
3.5 |
0.5 |
|||||||||||
M13/ M20(a) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.1 |
1.1 |
3.2 |
||||||||||
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.1 |
1.1 |
3.3 |
|||||||||||
Mean |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
1.1 |
1.1 |
3.3 |
|||||||||||
M8 |
A |
ND |
ND |
ND |
0.6 |
5.3 |
4.4 |
3.5 |
1.9 |
ND |
0.6 |
||||||||||
B |
ND |
ND |
ND |
0.6 |
5.0 |
4.2 |
4.1 |
2.0 |
ND |
0.6 |
|||||||||||
Mean |
NA |
NA |
NA |
0.6 |
5.2 |
4.3 |
3.8 |
2.0 |
NA |
0.6 |
|||||||||||
M21 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.8 |
1.0 |
1.0 |
||||||||||
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.8 |
0.9 |
1.2 |
|||||||||||
Mean |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
0.8 |
1.0 |
1.1 |
|||||||||||
M4 |
A |
0.3 |
ND |
0.6 |
1.1 |
7.4 |
6.6 |
6.5 |
5.9 |
5.1 |
4.8 |
||||||||||
B |
ND |
ND |
0.4 |
1.3 |
9.5 |
8.2 |
7.4 |
5.8 |
4.9 |
5.5 |
|||||||||||
Mean |
0.2 |
NA |
0.5 |
1.2 |
8.5 |
7.4 |
7.0 |
5.9 |
5.0 |
5.2 |
|||||||||||
M5 |
A |
ND |
ND |
ND |
0.3 |
3.4 |
5.5 |
4.9 |
5.9 |
6.8 |
5.8 |
||||||||||
B |
ND |
ND |
ND |
0.3 |
1.6 |
3.1 |
4.6 |
6.0 |
5.9 |
5.9 |
|||||||||||
Mean |
NA |
NA |
NA |
0.3 |
2.5 |
4.3 |
4.8 |
6.0 |
6.4 |
5.9 |
|||||||||||
M3 |
A |
ND |
ND |
ND |
1.7 |
10.8 |
15.7 |
13.1 |
13.9 |
12.9 |
13.4 |
||||||||||
B |
ND |
0.6 |
0.5 |
1.8 |
9.7 |
13.0 |
12.0 |
13.3 |
12.7 |
13.1 |
|||||||||||
Mean |
NA |
0.3 |
0.3 |
1.8 |
10.3 |
14.4 |
12.6 |
13.6 |
12.8 |
13.3 |
|||||||||||
M2 / M1(a) |
A |
ND |
ND |
0.6 |
1.2 |
1.7 |
2.1 |
1.7 |
2.5 |
3.0 |
2.9 |
||||||||||
B |
ND |
<0.1 |
0.1 |
1.3 |
1.7 |
2.3 |
2.9 |
2.9 |
3.4 |
3.2 |
|||||||||||
Mean |
NA |
<0.1 |
0.4 |
1.3 |
1.7 |
2.2 |
2.3 |
2.7 |
3.2 |
3.1 |
|||||||||||
M22 / M3(b) |
A |
ND |
ND |
ND |
ND |
2.5 |
3.6 |
4.4 |
5.5 |
5.7 |
6.0 |
||||||||||
B |
ND |
ND |
ND |
ND |
2.4 |
3.2 |
3.6 |
5.3 |
6.4 |
5.2 |
|||||||||||
Mean |
NA |
NA |
NA |
NA |
2.5 |
3.4 |
4.0 |
5.4 |
6.1 |
5.6 |
|||||||||||
M10 |
A |
ND |
ND |
ND |
ND |
1.3 |
2.3 |
1.9 |
2.8 |
2.0 |
2.7 |
||||||||||
B |
ND |
ND |
ND |
ND |
1.1 |
1.7 |
2.2 |
3.0 |
2.0 |
2.0 |
|||||||||||
Mean |
NA |
NA |
NA |
NA |
1.2 |
2.0 |
2.1 |
2.9 |
2.0 |
2.4 |
|||||||||||
Minor Unknowns(c) |
A |
ND |
0.7 |
0.7 |
2.4 |
10.4 |
19.7 |
9.3 |
11.2 |
10.6 |
12.1 |
||||||||||
B |
ND |
0.3 |
0.1 |
2.2 |
10.3 |
16.9 |
8.6 |
13.8 |
11.0 |
14.0 |
|||||||||||
Mean |
NA |
0.5 |
0.4 |
2.3 |
10.4 |
18.3 |
9.0 |
12.5 |
10.8 |
13.1 |
|||||||||||
Origin Bound |
A |
0.1 |
0.9 |
1.0 |
ND |
1.4 |
2.8 |
2.8 |
2.8 |
4.2 |
2.1 |
||||||||||
B |
ND |
0.7 |
0.8 |
ND |
1.2 |
2.4 |
2.8 |
2.5 |
4.1 |
1.5 |
|||||||||||
Mean |
0.1 |
0.8 |
0.9 |
NA |
1.3 |
2.6 |
2.8 |
2.7 |
4.2 |
1.8 |
|||||||||||
14CO2 |
A |
NS |
<0.1 |
<0.1 |
<0.1 |
0.2 |
0.3 |
0.5 |
0.8 |
1.5 |
2.4 |
||||||||||
B |
NS |
<0.1 |
<0.1 |
<0.1 |
0.1 |
0.4 |
0.4 |
1.3 |
2.4 |
2.1 |
|||||||||||
Mean |
NS |
<0.1 |
<0.1 |
<0.1 |
0.2 |
0.4 |
0.5 |
1.1 |
2.0 |
2.3 |
|||||||||||
Non- Extractable |
A |
0.3 |
1.0 |
1.6 |
16.0 |
20.3 |
22.5 |
25.2 |
27.6 |
26.3 |
31.1 |
||||||||||
B |
0.4 |
1.1 |
1.1 |
15.7 |
18.7 |
15.1 |
25.1 |
28.5 |
29.8 |
29.7 |
|||||||||||
Mean |
0.4 |
1.1 |
1.4 |
15.9 |
19.5 |
18.8 |
25.2 |
28.1 |
28.1 |
30.4 |
|||||||||||
Extracts not Profiled(d) |
A |
0.5 |
0.9 |
0.3 |
1.4 |
3.2 |
3.4 |
2.8 |
3.5 |
NA |
NA |
||||||||||
B |
1.0 |
0.9 |
0.6 |
2.0 |
2.9 |
3.1 |
2.4 |
3.5 |
NA |
NA |
|||||||||||
Mean |
0.8 |
0.9 |
0.5 |
1.7 |
3.1 |
3.3 |
2.6 |
3.5 |
NA |
NA |
|||||||||||
Total |
A |
98.8 |
97.9 |
95.9 |
98.3 |
97.2 |
105.8 |
87.5 |
90.8 |
83.9 |
88.6 |
||||||||||
B |
95.0 |
99.3 |
96.0 |
100.1 |
97.1 |
97.7 |
91.7 |
94.5 |
87.9 |
87.8 |
|||||||||||
Mean |
96.9 |
98.6 |
96.0 |
99.2 |
97.2 |
101.8 |
89.6 |
92.7 |
85.9 |
88.2 |
|||||||||||
(a)= Minor components not fullyresolved
(b) = M22/M3 regions in 60 day to 120 day extract 1, 2 and 3 samples were isolated and found to contain M3. M22 was< LOQ.
(c) = Sumofminorunknowncomponents quantified from solvent system 2; refer APPENDIX 12forindividual quantification. 0-6hunknowncomponents quantified from Solvent System1
(d) = Radioactivity in extracts accounting for a small % AR which were not subject to chromatography analysis
ND = Notdetected
NA =Not applicable
NS = Nosample
Note: Residue summary compiled using a combinationofdatafromSolventSystem1, 2, 3 and4.
Table 9. Bound residue Characterisation: Marsillargues, 120DAT – Bouond residues deermined by combustion = 38,4%
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Reflux Extract |
A |
11.9 |
|
B |
10.7 |
||
Mean |
11.3 |
||
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Organic Matter Fractionation |
Fulvic Acid |
A |
6.9 |
B |
7.3 |
||
Mean |
7.1 |
||
Humic Acid |
A |
ND |
|
B |
ND |
||
Mean |
NA |
||
Humin |
A |
31.6 |
|
B |
30.9 |
||
Mean |
31.3 |
||
Total |
A |
38.5 |
|
B |
38.2 |
||
Mean |
38.4 |
||
ND = Notdetected NA =Notapplicable
Table 10. Bound residue Characterisation: 18 Acres, 120DAT – Bouond residues deermined by combustion = 28.9%
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Reflux Extract |
A |
8.4 |
|
B |
10.3 |
||
Mean |
9.4 |
||
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Organic Matter Fractionation |
Fulvic Acid |
A |
7.2 |
B |
7.4 |
||
Mean |
7.3 |
||
Humic Acid |
A |
4.2 |
|
B |
4.7 |
||
Mean |
4.5 |
||
Humin |
A |
16.1 |
|
B |
18.2 |
||
Mean |
17.2 |
||
Total |
A |
27.5 |
|
B |
30.3 |
||
Mean |
28.9 |
||
Table 11.Bound residue Characterisation: Marsillargues, 120DAT – Bouond residues deermined by combustion = 33.7%
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Reflux Extract |
A |
7.7 |
|
B |
8.7 |
||
Mean |
8.2 |
||
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Organic Matter Fractionation |
Fulvic Acid |
A |
4.0 |
B |
4.2 |
||
Mean |
4.1 |
||
Humic Acid |
A |
ND |
|
B |
ND |
||
Mean |
NA |
||
Humin |
A |
28.7 |
|
B |
30.5 |
||
Mean |
29.6 |
||
Total |
A |
32.7 |
|
B |
34.7 |
||
Mean |
33.7 |
||
Table 12.Bound residue Characterisation: Marsillargues, 120DAT – Bouond residues deermined by combustion = 30,4%
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Reflux Extract |
A |
7.3 |
|
B |
8.3 |
||
Mean |
7.8 |
||
Fraction |
Replicate |
Percent Applied Radioactivity Recovered in Fraction |
|
Organic Matter Fractionation |
Fulvic Acid |
A |
8.0 |
B |
7.7 |
||
Mean |
7.9 |
||
Humic Acid |
A |
3.4 |
|
B |
3.6 |
||
Mean |
3.5 |
||
Humin |
A |
19.7 |
|
B |
18.4 |
||
Mean |
19.1 |
||
Total |
A |
31.1 |
|
B |
29.7 |
||
Mean |
30.4 |
||
Table 13. Summary of DegT50 and DegT90Values
Soil Name |
DegT50 (Days) |
DegT90 (Days) |
Χ2 |
R2 |
Prob>t |
Marsillargues |
4.7 |
15.6 |
9.4 |
0.98 |
7.6 x 10-9 |
18 Acres |
4.7 |
15.5 |
5.8 |
0.99 |
3.0 x 10-11 |
Gartenacker |
1.5 |
5.0 |
6.5 |
0.99 |
1.3 x 10-9 |
White Swan |
5.1 |
17.1 |
10.4 |
0.98 |
5.8 x 10-9 |
SFO = Single first order kinetics (non-linear method) calculated usingCAKEsoftware (Version 1.4) DegT50= Calculated degradation half-life of parent (timetakenfor 50%degradationofparentcompound)
DegT90= Time takenfor90% degradationofparentcompound
χ2 = Chi-square statisticalvalue
R2= Linear regression coefficient relating goodnessoffit as value approaches unity
Prob>t = Statistical probability value related to a statistical t-testcalculation
Table 2. Distribution and Recovery of Radioactivity from the Four Treatment Rates
Treatment Rate (µg/g) |
Recovered Radioactivity (% applied)a Days incubation |
|||||||||
|
0 |
0 |
2 |
7 |
15 |
22 |
34 |
64 |
125 |
|
0.1 |
14CO2 |
na |
na |
1.2 |
1.8 |
7.8 |
9.7 |
11.8 |
17.2 |
22.1 |
Extract 1 |
86.8 |
90.8 |
61.9 |
48.8 |
45.4 |
43.7 |
35.9 |
32.7 |
253 |
|
Extract 2 |
na |
na |
7 |
8.4 |
9.3 |
9.9 |
5 |
4.2 |
9.6 |
|
Foam Bung |
na |
na |
0 |
0 |
0 |
0 |
0 |
0 |
0 |
|
Filter Paper |
na |
na |
na |
na |
na |
1.7 |
na |
na |
na |
|
Unextracted |
12.6 |
10.8 |
24 |
31 |
33 |
33.9 |
35.5 |
413 |
40.2 |
|
TOTAL |
99.4 |
101.6 |
94.1 |
90 |
95.5 |
98.9 |
88.2 |
95.4 |
97.2 |
|
1 |
14CO2 |
na |
na |
3 |
3.7 |
8.2 |
10.2 |
12.4 |
15.9 |
17.2 |
Extract 1 |
93.4 |
94.8 |
75.9 |
55.4 |
50.4 |
44.8 |
46.5 |
36.6 |
25.5 |
|
Extract 2 |
na |
na |
63 |
6.8 |
8.8 |
8.8 |
2.6 |
4.6 |
11.6 |
|
Foam Bung |
na |
na |
0 |
0 |
0 |
0 |
0 |
0 |
0 |
|
Filter Paper |
na |
na |
na |
na |
na |
0.9 |
na |
na |
na |
|
Unextracted |
6.9 |
5.2 |
15.8 |
29.2 |
31.8 |
293 |
34.1 |
36.6 |
43.4 |
|
TOTAL |
1003 |
100 |
98.3 |
95.1 |
99.2 |
94 |
95.6 |
93.7 |
97.7 |
|
10 |
14CO2 |
na |
na |
0 |
0.1 |
1.5 |
2.7 |
46 |
7.7 |
103 |
Extract 1 |
97.9 |
98.6 |
94 |
79.5 |
80.7 |
57.8 |
57.5 |
53.9 |
423 |
|
Extract 2 |
na |
na |
2.4 |
3.7 |
6.6 |
4.8 |
7.6 |
9.7 |
11.5 |
|
Foam Bung |
na |
na |
0 |
0 |
0 |
0 |
0 |
0 |
0 |
|
Filter Paper |
na |
na |
na |
na |
na |
0.5 |
na |
na |
na |
|
Unextracted |
1.9 |
3.1 |
3.2 |
12.3 |
13.4 |
18.9 |
25.7 |
28.9 |
34.2 |
|
TOTAL |
99.8 |
101.7 |
99.6 |
95.6 |
102.2 |
84.7 |
95.4 |
100.2 |
98.3 |
|
25 |
14CO2 |
na |
na |
0 |
0 |
0.5 |
0.9 |
1.7 |
3 |
4.4 |
Extract 1 |
99.8 |
100.7 |
953 |
77.5 |
79.8 |
77.4 |
60.1 |
67.9 |
64.1 |
|
Extract 2 |
na |
na |
2.4 |
3.4 |
5.9 |
6.6 |
6.6 |
8.8 |
7.9 |
|
Foam Bung |
na |
na |
0 |
0 |
0 |
0 |
0 |
0 |
0 |
|
Filter Paper |
na |
na |
2.4 |
3,4 |
5.9 |
6.6 |
6.6 |
8.8 |
7.9 |
|
Unextracted |
na |
na |
na |
na |
na |
0.5 |
na |
na |
na |
|
TOTAL |
102.1 |
102.6 |
99.9 |
88.1 |
97.4 |
99.4 |
85.1 |
100.4 |
96.7 |
|
na - not analysed
a - any summation differences in values within tables result from rounding of numbers within individual calculations
Table 3. Summary of Radioactive Residues in 0.1 µg/g Treatment
|
Distribution of Radioactivity |
|||||
2 |
7 |
15 |
22 |
34 |
125 |
|
The test substance |
7.4 |
3.7 |
2.8 |
2 |
1.6 |
0.9 |
M4 |
11.7 |
12.6 |
12.1 |
11.5 |
7.9 |
5.6 |
M13 |
0.5 |
1.1 |
0.5 |
0.8 |
nd |
0.4 |
M5 |
nd |
nd |
nd |
nd |
nd |
nd |
M8 and M20 |
1.3 |
nd |
nd |
1 |
0.5 |
0.7 |
M23 |
5.9 |
2 |
2.7 |
1.6 |
0.7 |
nd |
M18 |
nd |
nd |
nd |
nd |
nd |
nd |
M24 |
nd |
nd |
nd |
nd |
nd |
nd |
M9 |
8.8 |
10.8 |
12.5 |
8.7 |
5.8 |
12.7 |
M3 |
nc |
nc |
nc |
nc |
nc |
nd |
M10 |
nc |
nc |
nc |
nc |
nc |
3.2 |
M1 |
nc |
nc |
nc |
nc |
nc |
11.9 |
Unknows2 |
1.6 |
3.8 |
2.7 |
5.1 |
3.7 |
0.5 |
Reminder3 |
21.2 |
13.8 |
10.2 |
13.6 |
14.5 |
0 |
Baseline4 |
10.5 |
9.4 |
11.2 |
9.3 |
6.2 |
4.6 |
14CO2 |
1.2 |
1.8 |
7.8 |
9.7 |
11.8 |
22.1 |
Unextracted |
24 |
31 |
33 |
35.6 |
35.5 |
40.2 |
Total |
94.1 |
90 |
95.5 |
98.9 |
88.2 |
102.8 |
nd - Not detected
nc - Not chromatographed
1: Any summation differences in values within tables result from rounding of numbers
within individual calculations
2: Total % of applied of all unknow n compounds
3: This value is calculated as the % remaining after the sum of the baseline, unknowns
and identified components.
4: Radioactivity remaining at or very close to the origin of the TLC plate
Table 4. Summary of Radioactive Residues in 1 µg/g Treatment
|
Distribution of Radioactivity |
|||||
2 |
7 |
15 |
22 |
34 |
125 |
|
The test substance |
30.1 |
4.3 |
2.4 |
1.8 |
1.1 |
0.6 |
M4 |
14.1 |
16.7 |
17.9 |
14.8 |
13.3 |
5.6 |
M13 |
1.4 |
1.4 |
1.5 |
1 |
0.6 |
0.4 |
M5 |
nd |
nd |
nd |
nd |
nd |
0.2 |
M8 and M20 |
1.00 |
1.2 |
1.1 |
0.7 |
0.8 |
0.4 |
M23 |
6.5 |
3.5 |
0.9 |
1.2 |
1.5 |
nd |
M18 |
nd |
nd |
nd |
nd |
nd |
nd |
M24 |
nd |
nd |
nd |
nd |
nd |
nd |
M9 |
4.2 |
8.5 |
96 |
9.6 |
8.7 |
9.7 |
M3 |
nc |
nc |
nc |
nc |
nc |
nd |
M10 |
nc |
nc |
nc |
nc |
nc |
2.7 |
M1 |
nc |
nc |
nc |
nc |
nc |
6.9 |
Unknows2 |
1.8 |
0.9 |
3.2 |
3.8 |
5.3 |
1.8 |
Reminder3 |
12.5 |
14.9 |
12.5 |
11.9 |
9.8 |
3.9 |
Baseline4 |
10.6 |
10.8 |
10.1 |
8.8 |
8 |
4.9 |
14CO2 |
0.3 |
3.7 |
8.2 |
10.2 |
12.4 |
17.2 |
Unextracted |
15.8 |
29.2 |
31.8 |
30.2 |
34.1 |
43.4 |
Total |
98.3 |
95.1 |
99.2 |
94.00 |
95.6 |
97.7 |
nd - Not detected
nc - Not chromatographed
1: Any summation differences in values within tables result from rounding of numbers
within individual calculations
2: Total % of applied of all unknow n compounds
3: This value is calculated as the % remaining after the sum of the baseline, unknowns
and identified components.
4: Radioactivity remaining at or very close to the origin of the TLC plate
Table 5. Summary of Radioactive Residues in 10 µg/g Treatment
|
Distribution of Radioactivity |
|||||
2 |
7 |
15 |
22 |
34 |
125 |
|
The test substance |
83.0 |
42.2 |
45.7 |
21.3 |
5.6 |
1 |
M4 |
4.5 |
13.9 |
16.2 |
14.5 |
18.4 |
14.3 |
M13 |
0.6 |
1.4 |
1.7 |
1.6 |
1.4 |
0.6 |
M5 |
nd |
nd |
nd |
3.3 |
4.6 |
5.4 |
M8 and M20 |
0.3 |
1.8 |
1.2 |
0.9 |
1 |
1.0 |
M23 |
0.8 |
2.9 |
2.4 |
2.1 |
2.1 |
nd |
M18 |
nd |
nd |
nd |
nd |
nd |
nd |
M24 |
nd |
nd |
nd |
nd |
nd |
nd |
M9 |
0.5 |
3.5 |
4.1 |
4.5 |
7.7 |
10.1 |
M3 |
nc |
nc |
nc |
nc |
nc |
nd |
M10 |
nc |
nc |
nc |
nc |
nc |
0.6 |
M1 |
nc |
nc |
nc |
nc |
nc |
1.4 |
Unknows2 |
nd |
1.4 |
1.00 |
2.1 |
4.6 |
5.3 |
Reminder3 |
4.1 |
9.4 |
9.7 |
6.7 |
10.5 |
9.2 |
Baseline4 |
2.6 |
6.7 |
5.3 |
6.1 |
9.2 |
4.9 |
14CO2 |
0 |
0.1 |
1.5 |
2.7 |
4.6 |
10.3 |
Unextracted |
3.2 |
12.3 |
13.4 |
18.9 |
25.7 |
34.2 |
Total |
99.6 |
95.6 |
102.2 |
84.7 |
95.4 |
98.3 |
nd - Not detected
nc - Not chromatographed
1: Any summation differences in values within tables result from rounding of numbers
within individual calculations
2: Total % of applied of all unknow n compounds
3: This value is calculated as the % remaining after the sum of the baseline, unknowns
and identified components.
4: Radioactivity remaining at or very close to the origin of the TLC plate
Table 6. Summary of Radioactive Residues in 25 µg/g Treatment
|
Distribution of Radioactivity |
|||||
2 |
7 |
15 |
22 |
34 |
125 |
|
The test substance |
89.7 |
58.3 |
49.9 |
41.7 |
27.9 |
30.4 |
M4 |
3.3 |
9.7 |
14 |
16.4 |
14.5 |
14.7 |
M13 |
0.2 |
1 |
1.5 |
1.7 |
1.5 |
0.9 |
M5 |
nd |
nd |
nd |
4.6 |
3.7 |
4.2 |
M8 and M20 |
0.2 |
0.8 |
1.4 |
1.6 |
0.9 |
0.6 |
M23 |
0.4 |
1.8 |
2.2 |
2.6 |
2 |
nd |
M18 |
nd |
nd |
nd |
nd |
nd |
nd |
M24 |
nd |
nd |
nd |
nd |
nd |
nd |
M9 |
0.3 |
1.1 |
2.8 |
3.9 |
4.1 |
6 |
M3 |
nc |
nc |
nc |
nc |
nc |
0.9 |
M10 |
nc |
nc |
nc |
nc |
nc |
1.8 |
M1 |
nc |
nc |
nc |
nc |
nc |
4.4 |
Unknows2 |
0.2 |
0.6 |
1.3 |
0.5 |
2.4 |
4.3 |
Reminder3 |
2.3 |
4.8 |
7.5 |
8.9 |
5.1 |
0 |
Baseline4 |
1.1 |
2.8 |
5.1 |
2.6 |
4.6 |
4 |
14CO2 |
0 |
0 |
0.5 |
0.9 |
1.7 |
4.4 |
Unextracted |
2.2 |
7.2 |
11.2 |
14 |
16.7 |
20.3 |
Total |
99.9 |
88,1 |
97.4 |
99.4 |
85.1 |
96.9 |
nd - Not detected
nc - Not chromatographed
1: Any summation differences in values within tables result from rounding of numbers
within individual calculations
2: Total % of applied of all unknow n compounds
3: This value is calculated as the % remaining after the sum of the baseline, unknowns
and identified components.
4: Radioactivity remaining at or very close to the origin of the TLC plate
Table 2. Distribution and recovery of Radioactivity
Soil # |
Soil type |
|
Recovered Radioactivity (% applied) Days after treatment |
|
|
|
|
0 |
120 |
1 |
18 Acres |
Extract 1 |
92.6 |
38.8 |
Extract 2 |
na |
9.4 |
||
Foam Bung |
na |
na |
||
Carbon Sieves |
na |
na |
||
Accumulated CO2 |
na |
13.5 |
||
Unextracted |
5.7 |
33.1 |
||
Total |
98.3 |
94.8 |
||
2 |
Chamberlain's Farm |
Extract 1 |
96.6 |
30.7 |
Extract 2 |
na |
3.1 |
||
Foam Bung |
na |
na |
||
Carbon Sieves |
na |
na |
||
Accumulated CO2 |
na |
23.8 |
||
Unextracted |
4.0 |
39.9 |
||
Total |
100.6 |
97.5 |
||
3 |
ERTC |
Extract 1 |
96.0 |
49.5 |
Extract 2 |
na |
11.4 |
||
Foam Bung |
na |
na |
||
Carbon Sieves |
na |
na |
||
Accumulated CO2 |
na |
6.3 |
||
Unextracted |
1.5 |
23.7 |
||
Total |
97.5 |
90.9 |
||
4 |
Munster |
Extract 1 |
98.8 |
41.4 |
Extract 2 |
na |
14.9 |
||
Foam Bung |
na |
na |
||
Carbon Sieves |
na |
na |
||
Accumulated CO2 |
na |
11.8 |
||
Unextracted |
0.3 |
25.7 |
||
Total |
99.1 |
93.8 |
||
na: not analysed
Table 3. Summary of Radioactive Residues in 18 Acres Soil
|
Distribution of Radioactivity (% applied)a Days Incubation |
|||||||||
|
0 |
6hr |
1 |
3 |
7 |
14 |
30 |
58 |
92 |
120 |
The test substance |
88.8 |
68.8 |
41.8 |
14.3 |
6.5 |
2.2 |
2.0 |
1.1 |
0.5 |
1.2 |
M4 |
nd |
2.7 |
5.0 |
7.9 |
8.1 |
5.3 |
4.7 |
3.3 |
2.1 |
1.9 |
M13 |
nd |
nd |
1.1 |
1.7 |
1.6 |
1.1 |
0.8 |
0.6 |
nd |
nd |
M5 |
nd |
nd |
nd |
1.1 |
3.6 |
4.1 |
1.9 |
1.6 |
1.1 |
1.1 |
M8 |
nd |
nd |
2.5 |
3.0 |
0.5 |
3.0 |
1.7 |
0.8 |
0.2 |
nd |
M20b |
nd |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
M9 |
nd |
1.6 |
2.1 |
7.3 |
14.1 |
12.7 |
12.1 |
10.3 |
5.3 |
6.5 |
M10 |
nd |
nd |
0.4 |
1.1 |
2.0 |
2.4 |
2.8 |
4.0 |
3.8 |
2.4 |
M1 |
nd |
nd |
1.1 |
1.0 |
1.8 |
2.3 |
3.6 |
5.6 |
6.6 |
6.1 |
Unknownsc |
nd |
6.9 |
12.4 |
14.4 |
12.9 |
8.3 |
9.1 |
9.5 |
10.6 |
7.7 |
Baselined |
nd |
1.5 |
3.4 |
1.5 |
2.3 |
2.9 |
4.2 |
5.2 |
2.3 |
5.5 |
14CO2 |
nd |
nd |
nd |
0.6 |
2.7 |
5.1 |
8.4 |
11.3 |
12.5 |
13.5 |
Unextracted |
6.3 |
11.0 |
20.5 |
29.2 |
36.4 |
36.3 |
28.7 |
32.0 |
29.4 |
33.1 |
nd: Not detected
cc: Co-chromatographed with another reference compound
a Any summation differences in values within tables result from rounding of numbers within individual calculations
b Reference compound 6 co-chromatographed in all three solvent systems
c Total % of applied of all unknown compounds, where no single compound was > 10% of applied dose
d Radioactivity remaining at or very close to the origin of the TLC plate
Table 4. Summary of Radioactive Residues in Chamberlain’s Farm Soil
|
Distribution of Radioactivity (% applied)a Days Incubation |
|||||||||
|
0 |
6hr |
1 |
3 |
7 |
14 |
30 |
58 |
92 |
120 |
The test substance |
92.8 |
49.3 |
14.4 |
4.4 |
1.1 |
0.7 |
2.1 |
0.3 |
0.3 |
0.2 |
M4 |
nd |
14.6 |
24.5 |
23.1 |
25.3 |
21.9 |
22.2 |
17.0 |
17.3 |
14.5 |
M13 |
nd |
1.7 |
2.1 |
2.0 |
1.5 |
0.9 |
nd |
nd |
nd |
nd |
M5 |
nd |
nd |
nd |
nd |
3.4 |
4.3 |
3.2 |
2.8 |
nd |
2.3 |
M8 |
nd |
nd |
3.2 |
0.3 |
0.3 |
cc |
0.8 |
0.1 |
nd |
nd |
M20b |
nd |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
M9 |
nd |
2.9 |
3.5 |
5.8 |
5.8 |
4.6 |
3.9 |
2.8 |
1.8 |
1.9 |
M10 |
nd |
nd |
1.1 |
1.8 |
1.9 |
1.9 |
1.9 |
1.6 |
2.9 |
2.8 |
M1 |
nd |
nd |
nd |
nd |
0.6 |
1.0 |
1.6 |
2.5 |
3.2 |
3.8 |
Unknownsc |
nd |
3.7 |
8.5 |
16.8 |
10.9 |
3.3 |
4.3 |
2.0 |
5.6 |
2.5 |
Baselined |
nd |
nd |
1.5 |
nd |
0.7 |
nd |
nd |
nd |
0.2 |
1.2 |
14CO2 |
nd |
nd |
0.1 |
1.0 |
4.6 |
10.2 |
16.7 |
19.2 |
21.9 |
23.8 |
Unextracted |
4.0 |
14.2 |
21.5 |
26.2 |
35.1 |
35.9 |
29.0 |
33.4 |
32.1 |
39.9 |
nd: Not detected
cc: Co-chromatographed with another reference compound
a Any summation differences in values within tables result from rounding of numbers within individual calculations
b Reference compound 6 co-chromatographed in all three solvent systems
c Total % of applied of all unknown compounds, where no single compound was > 10% of applied dose
d Radioactivity remaining at or very close to the origin of the TLC plate
Table 5. Summary of Radioactive Residues in ERTC Soil
|
Distribution of Radioactivity (% applied)a Days Incubation |
|||||||||
|
0 |
6hr |
1 |
3 |
7 |
14 |
30 |
58 |
92 |
120 |
The test substance |
92.2 |
84.7 |
53.0
|
17.7 |
8.6 |
4.8 |
2.1 |
1.8 |
1.6 |
1.7 |
M4 |
nd |
4.7 |
11.6 |
20.8 |
13.8 |
15.5 |
15.3 |
14.5 |
12.5 |
5.4 |
M13 |
nd |
nd |
nd |
1.0 |
1.2 |
2.3 |
1.6 |
1.6 |
1.2 |
0.4 |
M5 |
nd |
nd |
0.5 |
1.4 |
2.8 |
5.1 |
6.0 |
5.2 |
4.1 |
2.6 |
M8 |
nd |
nd |
0.6 |
2.0 |
2.1 |
1.7 |
1.1 |
1.0 |
1.0 |
1.2 |
M20b |
nd |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
M9 |
nd |
1.4 |
2.1 |
4.5 |
4.4 |
7.4 |
12.3 |
8.1 |
7.8 |
8.8 |
M10 |
nd |
nd |
nd |
1.3 |
1.2 |
2.3 |
4.4 |
5.2 |
8.3 |
12.4 |
M1 |
nd |
nd |
nd |
nd |
1.0 |
nd |
1.4 |
1.7 |
1.7 |
2.0 |
Unknownsc |
nd |
5.1 |
11.6 |
16.2 |
12.4 |
11.4 |
13.7 |
11.6 |
12.9 |
12.2 |
Baselined |
nd |
1.3 |
1.6 |
7.4 |
3.6 |
3.9 |
6.6 |
2.9 |
4.5 |
3.9 |
14CO2 |
nd |
nd |
nd |
nd |
0.3 |
1.0 |
2.2 |
4.8 |
6.3 |
6.3 |
Unextracted |
1.5 |
3.5 |
8.7 |
14.7 |
20.8 |
19.6 |
17.2 |
23.2 |
18.9 |
23.7 |
nd: Not detected
cc: Co-chromatographed with another reference compound
a Any summation differences in values within tables result from rounding of numbers within individual calculations
b Reference compound 6 co-chromatographed in all three solvent systems
c Total % of applied of all unknown compounds, where no single compound was > 10% of applied dose
d Radioactivity remaining at or very close to the origin of the TLC plate
Table 6. Summary of Radioactive Residues in Munster Soil
|
Distribution of Radioactivity (% applied)a Days Incubation |
|||||||||
|
0 |
6hr |
1 |
3 |
7 |
14 |
30 |
58 |
92 |
120 |
The test substance |
95.6 |
85.2 |
61.9 |
29.5 |
11.8 |
3.5 |
0.9 |
1.4 |
0.9 |
1.1 |
M4 |
nd |
1.8 |
4.1 |
6.3 |
5.1 |
4.6 |
4.3 |
3.7 |
2.8 |
2.0 |
M13 |
nd |
nd |
nd |
nd |
1.8 |
1.6 |
1.2 |
1.4 |
0.8 |
0.5 |
M5 |
nd |
nd |
0.6 |
2.6 |
9.3 |
12.8 |
13.2 |
11.3 |
6.5 |
7.2 |
M8 |
nd |
nd |
0.7 |
3.2 |
4.0 |
1.6 |
0.4 |
0.7 |
0.3 |
nd |
M20b |
nd |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
cc |
M9 |
nd |
2.1 |
2.3 |
6.5 |
6.9 |
11.7 |
7.3 |
10.7 |
8.1 |
10.5 |
M10 |
nd |
nd |
nd |
1.2 |
2.0 |
3.9 |
3.8 |
3.2 |
6.4 |
5.9 |
M1 |
nd |
nd |
0.8 |
nd |
1.5 |
nd |
1.6 |
2.1 |
2.6 |
3.2 |
Unknownsc |
nd |
5.2 |
10.5 |
13.9 |
15.1 |
9.9 |
14.8 |
10.5 |
13.4 |
10.6 |
Baselined |
nd |
1.8 |
0.3 |
8.6 |
5.3 |
7.0 |
6.8 |
9.3 |
9.6 |
7.1 |
14CO2 |
nd |
nd |
nd |
0.1 |
0.8 |
2.1 |
5.3 |
8.3 |
10.4 |
11.8 |
Unextracted |
0.3 |
3.6 |
9.9 |
13.4 |
24.7 |
24.8 |
21.9 |
22.9 |
22.6 |
25.7 |
nd: Not detected
cc: Co-chromatographed with another reference compound
a Any summation differences in values within tables result from rounding of numbers within individual calculations
b Reference compound 6 co-chromatographed in all three solvent systems
c Total % of applied of all unknown compounds, where no single compound was > 10% of applied dose
d Radioactivity remaining at or very close to the origin of the TLC plate
Table 7. Degradation of the test substance
Soil type |
Rate of Degradation (days) |
|||
SFO |
FOMC |
|||
DT50 |
DT90 |
DT50 |
DT90 |
|
18 Acres |
1.0 |
3.4 |
0.9 |
5.1 |
Chamberlain's Farm |
0.3 |
1.0 |
0.3 |
1.5 |
ERTC |
1.3 |
4.3 |
1.2 |
5.6 |
Munster |
1.9 |
6.1 |
1.6 |
7.8 |
Table 1. Residue Summary PO (10 ppm) Soil Samples - Total [(aveExt A)+(aveExt B)] - Adjusted % of TRR in Extracts
Sample |
Total profile |
Test substance |
M4 |
M13 |
M8 |
M23 |
M5 |
M20 |
Region UNK-3 |
Region UNK-5 |
Sum of all unknowns |
Total extractable |
Day 0 |
RexA+ExtB |
91.99 |
0.12 |
0.12 |
0.08 |
0.09 |
0.07 |
0.12 |
0.11 |
0.03 |
4.13 |
97.5% |
Day 7 |
RexA+ExtB |
63.64 |
5.28 |
0 |
4.15 |
1.1 |
0.47 |
4.74 |
1.46 |
0.71 |
9.01 |
89.4% |
Day 21 |
RexA+ExtB |
40.18 |
8.51 |
2.85 |
6.99 |
1.94 |
3.43 |
4.53 |
4.03 |
2 |
13.73 |
83.0% |
Day 28 |
RexA+ExtB |
32.03 |
8.25 |
4.17 |
6.78 |
1.97 |
4.9 |
6.07 |
5.17 |
3.12 |
17.02 |
82.6% |
Day 61 |
RexA+ExtB |
19.08 |
12.11 |
2.64 |
8.87 |
3.38 |
11.1 |
3.85 |
7.52 |
4.45 |
17.71 |
80.0% |
Day 91 |
RexA+ExtB |
7.43 |
8.8 |
0.81 |
9.74 |
3.08 |
13.05 |
3.81 |
8.42 |
5.57 |
17.54 |
66.7% |
Day 124 |
RexA+ExtB |
0.71 |
8.84 |
2.38 |
8.32 |
3.78 |
15.82 |
2.86 |
9.1 |
7.72 |
19.91 |
71.6% |
Day 181 |
RexA+ExtB |
6.8 |
6.18 |
5.52 |
5.35 |
3.96 |
10 |
2.94 |
9.64 |
9.09 |
21.17 |
71.8% |
Note: Unknown regions 1, 4, and 6 are excluded from this table because their individual amounts did not exceed 10% of the TRR.
Table 2. Residue Summary PO (1 ppm) Soil Samples - Total [(aveExt A)+(aveExt B)] - Adjusted % of TRR in Extracts
Sample |
Total profile |
Test substance |
M4 |
M13 |
M8 |
M23 |
M5 |
M20 |
Region UNK-3 |
Region UNK-5 |
Sum of all unknowns |
Total extractable |
Day 0 |
RexA+ExtB |
89.02 |
0.65 |
0.65 |
0.54 |
0.55 |
0.14 |
1.69 |
0.41 |
0.33 |
3.59 |
97.70% |
Day 4 |
RexA+ExtB |
36.53 |
5.09 |
2.73 |
4.86 |
2.56 |
1.58 |
13.24 |
5.12 |
4.71 |
17.91 |
85.90% |
Day 7 |
RexA+ExtB |
25.34 |
5.55 |
0.66 |
7.16 |
2.18 |
4.35 |
9.23 |
9.27 |
5.62 |
21.58 |
76.70% |
Day 14 |
RexA+ExtB |
20.92 |
5.61 |
0.76 |
6.84 |
3.35 |
7.92 |
7.77 |
11.82 |
8.2 |
27.84 |
82.80% |
Day 21 |
RexA+ExtB |
18.47 |
5.51 |
1.87 |
5.59 |
2.88 |
9.49 |
6.53 |
13.74 |
9.69 |
29.63 |
79.50% |
Day 28 |
RexA+ExtB |
15.5 |
5.57 |
2.03 |
4.28 |
3.08 |
10.07 |
4.95 |
14.27 |
10.79 |
31.68 |
78.40% |
Day 61 |
RexA+ExtB |
9.05 |
4.95 |
0.83 |
4.21 |
3.58 |
12.12 |
3.64 |
14.39 |
14.53 |
34.79 |
74.80% |
Day 91 |
RexA+ExtB |
5.56 |
3.84 |
1.44 |
3.35 |
2.58 |
10.96 |
3.87 |
12.7 |
14.16 |
33.13 |
66.50% |
Day 124 |
RexA+ExtB |
5.5 |
3.23 |
0.4 |
3.82 |
2.87 |
12.45 |
2.62 |
13.15 |
16.98 |
33.37 |
65.20% |
Day 152 |
RexA+ExtB |
2.7 |
3.62 |
0.17 |
3.6 |
2.94 |
14.07 |
2.62 |
14.99 |
20.66 |
38.8 |
69.40% |
Day 181 |
RexA+ExtB |
3.23 |
2.9 |
0.89 |
3.16 |
2.93 |
11.6 |
3.34 |
12.19 |
18.39 |
32.88 |
61.90% |
Note: Unknown regions 1, 4, and 6 are excluded from this table because their individual amounts did not exceed 10% of the TRR.
Table 3. Extraction Summary - Percent Distribution - 10 ppm Soil Samples
Sample |
Recovered DPM per sample |
% of DPM as Extract A |
% of DPM as Extract B |
n/ ExtB |
% of DPM as PES |
Cumulative % TRR as CO2 |
Day 0-1 |
966,452 |
97.30% |
nd |
0 |
2.70% |
|
Day 0-2 |
962,174 |
97.80% |
nd |
0 |
2.20% |
na |
Day 7-1 |
925,060 |
84.50% |
3.40% |
1 |
12.10% |
|
Day 7-2 |
911,588 |
86.30% |
3.40% |
1 |
10.30% |
|
Day 7-R1 |
466,185 |
83.10% |
5.10% |
2 |
11.70% |
|
Day 7-R2 |
439,004 |
86.60% |
3.50% |
3 |
9.90% |
0.03% |
Day 21-1 |
913,895 |
74.00% |
8.10% |
3 |
17.70% |
|
Day 21-2 |
852,422 |
76.40% |
9.10% |
3 |
14.30% |
0.17% |
Day 28-1 |
827,949 |
78.30% |
5.30% |
3 |
16.10% |
|
Day 28-2 |
821,129 |
75.90% |
5.50% |
3 |
18.30% |
0.27% |
Day 61-1 |
865,317 |
71.30% |
8.30% |
3 |
19.80% |
|
Day 61-2 |
878,430 |
72.30% |
8.10% |
3 |
19.00% |
0.58% |
Day 91-1 |
1,023,318 |
56.60% |
7.90% |
3 |
34.70% |
|
Day 91-2 |
939,499 |
60.80% |
8.00% |
3 |
30.30% |
0.81% |
Day 124-1 |
951,180 |
61.10% |
10.50% |
3 |
27.40% |
|
Day 124-2 |
946,567 |
63.20% |
8.60% |
3 |
27.20% |
1.05% |
Day 181-1 |
1,336,099 |
58.90% |
12.80% |
3 |
26.90% |
|
Day 181-2 |
1,341,964 |
60.80% |
11.00% |
3 |
26.80% |
1.36% |
Table 4. Extraction Summary - Percent Distribution - 1 ppm Soil Samples
Sample |
Recovered DPM per sample |
% of DPM as Extract A |
% of DPM as Extract B |
n/ ExtB |
% of DPM as PES |
Cumulative % TRR as CO2 |
Day 0-1 |
968,551 |
92.7% |
nd |
0 |
7.3% |
|
Day 0-2 |
959,348 |
94.1% |
nd |
1 |
5.9% |
|
Day 0-R1 |
695,820 |
94.0% |
3.7% |
3 |
2.3% |
|
Day 0-R2 |
747,974 |
91.6% |
5.5% |
3 |
2.9% |
na |
Day 4-1 |
828.766 |
79.3% |
nd |
0 |
20.6% |
|
Day 4-2 |
862,990 |
75.2% |
nd |
0 |
24.7% |
|
Day 4-R1 |
594,020 |
79.0% |
8.5% |
3 |
12.3% |
|
Day 4-R2 |
602,542 |
72.1% |
10.5% |
3 |
17.3% |
0.10% |
Day 7-1 |
874,662 |
72.2% |
5.9% |
1 |
21.7% |
|
Day 7-2 |
891,562 |
71.1% |
5.0% |
1 |
22.9% |
|
Day 7-R1 |
238,410 |
71.3% |
5.2% |
3 |
23.2% |
0.2% |
Day 14-1 |
813,007 |
71.6% |
12.1% |
3 |
15.7% |
|
Day 14-2 |
834,480 |
71.7% |
10.1% |
3 |
17.7% |
0.5% |
Day 21-1 |
847,660 |
69.0% |
11.6% |
3 |
18.7% |
|
Day 21-2 |
840,850 |
60.8% |
17.7% |
3 |
20.7% |
0.8% |
Day 28-1 |
904,709 |
62.8% |
14.6% |
3 |
21.8% |
|
Day 28-2 |
886,381 |
67.7% |
11.7% |
3 |
19.6% |
1.0% |
Day 61-1 |
846,777 |
59.3% |
13.7% |
3 |
25.3% |
|
Day 61-2 |
855,612 |
64.4% |
12.3% |
3 |
21.6% |
1.7% |
Day 91-1 |
680,903 |
60.7% |
11.5% |
3 |
25.6% |
|
Day 91-2 |
823,998 |
51.1% |
9.7% |
3 |
36.9% |
2.3% |
Day 124-1 |
667,024 |
53.0% |
12.4% |
3 |
31.0% |
|
Day 124-2 |
720,930 |
54.30% |
10.0% |
3 |
32.1% |
2.8% |
Day 152-1 |
669,364 |
59.0% |
11.3% |
3 |
25.7% |
|
Day 152-2 |
674.528 |
58.5% |
11.1% |
3 |
29.2% |
3.2% |
Day 181-1 |
750.969 |
45.0% |
14.1% |
3 |
36.5% |
|
Day 181-2 |
762,601 |
52.1% |
11.8% |
3 |
32.4% |
3.7% |
Table 1. Radioactive mass balance: Extracts, Mineralization, volatilization and Unextracted percentages for the total radioactivity applied in the Gleissolo Melanico Aluminico tipico (GM) soil.
Sampling time (days) |
Extract1 |
Extract 2 |
Sum of extracted radioactivity |
14CO2 |
14C-labelled organic volatile |
Unextracted radioactivity |
Total recovery |
% of applied |
|||||||
0 |
88.47 |
10.31 |
98.79 |
nd |
nd |
nd |
98.79 |
1 |
75.97 |
11.27 |
87.24 |
0.01 |
0.01 |
7.69 |
94.94 |
3 |
58.2 |
11.27 |
69.46 |
0.23 |
0.02 |
25.6 |
95.32 |
7 |
45.01 |
11.2 |
56.2 |
0.83 |
0.03 |
32.93 |
90.00 |
14 |
39.77 |
15.15 |
54.92 |
1.8 |
0.03 |
34.45 |
91.2 |
28 |
36.71 |
14.34 |
51.05 |
5.01 |
0.02 |
34.12 |
90.19 |
60 |
26.83 |
13.12 |
39.95 |
8.95 |
0.01 |
42.47 |
91.38 |
90 |
28.3 |
11.38 |
39.68 |
10.55 |
0.01 |
42.23 |
92.47 |
120 |
24.67 |
12.17 |
36.84 |
11.3 |
< LD |
42.93 |
91.08 |
nd: not determined
LD: Limit of Detection = 8*10^4 µg/mL
Table 2. Radioactive mass balance: Extracts, Mineralization, volatilization and Unextracted percentages for the total radioactivity applied in the Latossolo Vermelho Distroferrico tipico (LVdf) soil.
Sampling time (days) |
Extract1 |
Extract 2 |
Sum of extracted radioactivity |
14CO2 |
14C-labelled organic volatile |
Unextracted radioactivity |
Total recovery |
% of applied |
|||||||
0 |
93.72 |
7.41 |
101.13 |
nd |
nd |
nd |
101.13 |
1 |
83 |
7.81 |
90.82 |
0.01 |
0.01 |
6.54 |
97.38 |
3 |
73.88 |
11.32 |
85.2 |
0.1 |
0.1 |
11.46 |
96.86 |
7 |
62.44 |
11.44 |
73.88 |
0.87 |
0.1 |
21.06 |
95.9 |
14 |
55.98 |
14.46 |
70.43 |
2.21 |
0.08 |
22.02 |
94.74 |
28 |
45.49 |
13.75 |
59.24 |
4.95 |
0.06 |
32.46 |
96.71 |
60 |
43.66 |
13.37 |
57.03 |
7.02 |
0.02 |
32.96 |
97.03 |
90 |
41.24 |
14.51 |
55.75 |
9.31 |
0.01 |
33.75 |
98.82 |
120 |
39.95 |
12.67 |
52.62 |
10.06 |
< LD |
34.23 |
96.92 |
nd: not determined
LD: Limit of Detection = 8*10^4 µg/mL
Table 3. Radioactive mass balance: Extracts, Mineralization, volatilization and Unextracted percentages for the total radioactivity applied in the Neossolo Quartzarenico Ortico tipico (RQ) soil.
Sampling time (days) |
Extract1 |
Extract 2 |
Sum of extracted radioactivity |
14CO2 |
14C-labelled organic volatile |
Unextracted radioactivity |
Total recovery |
% of applied |
|||||||
0 |
99.58 |
4.16 |
103.74 |
nd |
nd |
nd |
103.74 |
1 |
89.63 |
10.67 |
100.3 |
0.01 |
< LD |
0.38 |
100.7 |
3 |
90.71 |
2.27 |
92.98 |
0.16 |
0.2 |
1.36 |
94.7 |
7 |
76.05 |
4.85 |
80.9 |
0.79 |
0.35 |
12.89 |
94.94 |
14 |
65.13 |
5.77 |
70.9 |
2.27 |
0.16 |
18.16 |
91.48 |
28 |
60.41 |
5.3 |
65.71 |
5.05 |
0.02 |
25.62 |
96.4 |
60 |
54.47 |
6.08 |
60.55 |
6.46 |
0.56 |
25.3 |
92.86 |
90 |
53.28 |
6.1 |
59.38 |
8.06 |
< LD |
25.94 |
93.39 |
120 |
51.21 |
7.69 |
58.89 |
8.92 |
< LD |
26.17 |
93.98 |
nd: not determined
LD: Limit of Detection = 8*10^4 µg/mL
Table 4. Radioactive mass balance: Extracts, Mineralization, volatilization and Unextracted percentages for the total radioactivity applied in the Argissolo Vermelho Eutroferrico chemossolico (PV) soil.
Sampling time (days) |
Extract1 |
Extract 2 |
Sum of extracted radioactivity |
14CO2 |
14C-labelled organic volatile |
Unextracted radioactivity |
Total recovery |
% of applied |
|||||||
0 |
87.06 |
10.79 |
97.85 |
nd |
nd |
nd |
97.85 |
1 |
84.69 |
2.43 |
87.11 |
0.02 |
0.01 |
4.62 |
91.76 |
3 |
72.49 |
10.43 |
82.93 |
0.14 |
0.01 |
11.12 |
94.2 |
7 |
62.31 |
10.55 |
72.86 |
0.71 |
0.01 |
17.37 |
90.95 |
14 |
55.89 |
12.18 |
68.07 |
1.95 |
0.01 |
21.35 |
91.38 |
28 |
47.31 |
12.06 |
59.37 |
4.51 |
0.01 |
33.79 |
97.67 |
60 |
44.12 |
9.82 |
53.93 |
5.88 |
0.01 |
33.05 |
92.86 |
90 |
41.21 |
14.76 |
55.97 |
7.41 |
< LD |
34.03 |
97.42 |
120 |
38.08 |
10.17 |
48.25 |
8.31 |
< LD |
34.7 |
91.26 |
nd: not determined
LD: Limit of Detection = 8*10^4 µg/mL
Table 5. Characterization of Radioactivity in the Gleissolo Melanico Aluminico tipico (GM) soil.
Sampling time (days) |
The test substance |
M1 |
M9 |
M4 |
M5 |
Unknown metabolite 1 |
Unknown metabolite 2 |
Unknown metabolite 3 |
Unknown metabolite 4 |
Unknowns |
% of applied |
||||||||||
0 |
88.6 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
10.18 |
1 |
76.58 |
0.00 |
0.09 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
10.56 |
3 |
49.91 |
0.08 |
0.34 |
2.79 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
16.33 |
7 |
22.09 |
0.19 |
2.53 |
3.25 |
0.07 |
0.00 |
0.00 |
0.00 |
0.00 |
28.06 |
14 |
19.41 |
0.27 |
5.54 |
0.12 |
0 |
4.57 |
7.66 |
1.19 |
0.63 |
15.53 |
28 |
4.04 |
0.08 |
1.13 |
0.27 |
9.75 |
6.55 |
7.63 |
0.00 |
0.42 |
21.17 |
60 |
3.71 |
0.19 |
3.82 |
0.16 |
4.79 |
5.97 |
0.43 |
0.00 |
1.2 |
19.68 |
90 |
2.39 |
1.31 |
7.78 |
0.71 |
1.39 |
4.12 |
0.64 |
1.78 |
0.25 |
19.31 |
120 |
1.31 |
1.15 |
7.9 |
0.03 |
4.3 |
3.42 |
0.26 |
0.82 |
0.1 |
17.56 |
Unknowns: Sum of unknowns peaks and unresolved radioactivity.
Table 6. Characterization of Radioactivity in the Latossolo Vermelho Distroferrico tipico (LVdf) soil.
Sampling time (days) |
The test substance |
M1 |
M9 |
M4 |
M5 |
Unknown metabolite 1 |
Unknown metabolite 2 |
Unknown metabolite 3 |
Unknown metabolite 4 |
Unknowns |
% of applied |
||||||||||
0 |
93.81 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
7.31 |
1 |
77.15 |
0.06 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
13.61 |
3 |
66.03 |
0.00 |
1.14 |
3.88 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
14.16 |
7 |
35.55 |
0.00 |
6.93 |
9.14 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
22.26 |
14 |
18.26 |
0.33 |
7.39 |
0.20 |
0.92 |
6.95 |
3.49 |
8.40 |
0.36 |
24.13 |
28 |
5.32 |
0.47 |
10.61 |
1.40 |
6.00 |
8.86 |
0.62 |
2.58 |
5.67 |
17.71 |
60 |
4.08 |
1.44 |
10.47 |
0.09 |
2.04 |
7.42 |
0.33 |
6.78 |
0.93 |
23.46 |
90 |
2.40 |
2.80 |
9.20 |
0.17 |
2.89 |
5.01 |
0.37 |
4.66 |
0.02 |
28.22 |
120 |
1.19 |
3.95 |
13.38 |
0.60 |
4.22 |
5.50 |
0.21 |
4.80 |
0.30 |
18.48 |
Unknowns: Sum of unknowns peaks and unresolved radioactivity.
Table 7. Characterization of Radioactivity in the Neossolo Quartzarenico 6rtico tipico (RQ) soil.
Sampling time (days) |
The test substance |
M1 |
M9 |
M4 |
M5 |
Unknown metabolite 1 |
Unknown metabolite 2 |
Unknown metabolite 3 |
Unknown metabolite 4 |
Unknowns |
% of applied |
||||||||||
0 |
103.16 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.58 |
1 |
98.76 |
0.00 |
0.00 |
0.30 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
1.25 |
3 |
91.98 |
0.00 |
0.00 |
0.23 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.77 |
7 |
48.96 |
0.00 |
6.52 |
8.73 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
16.70 |
14 |
9.09 |
0.05 |
10.67 |
0.79 |
0.83 |
8.85 |
2.01 |
8.42 |
0.27 |
29.93 |
28 |
8.70 |
0.35 |
10.71 |
0.16 |
2.60 |
8.45 |
2.07 |
8.83 |
0.40 |
23.44 |
60 |
3.69 |
0.22 |
11.33 |
0.25 |
2.94 |
7.23 |
0.51 |
5.03 |
0.38 |
28.97 |
90 |
1.38 |
2.27 |
20.96 |
0.33 |
2.90 |
7.08 |
0.34 |
2.13 |
0.14 |
21.85 |
120 |
0.42 |
0.90 |
15.35 |
0.34 |
7.39 |
5.28 |
0.34 |
4.63 |
0.15 |
24.09 |
Unknowns: Sum of unknowns peaks and unresolved radioactivity.
Table 8. Characterization of Radioactivity in the Argissolo Vermelho Eutrofdrrico chemossdlico (PV) soil.
Sampling time (days) |
The test substance |
M1 |
M9 |
M4 |
M5 |
Unknown metabolite 1 |
Unknown metabolite 2 |
Unknown metabolite 3 |
Unknown metabolite 4 |
Unknowns |
% of applied |
||||||||||
0 |
97.85 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
1 |
86.91 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
0.20 |
3 |
76.69 |
0.00 |
0.00 |
3.20 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
3.04 |
7 |
57.46 |
0.00 |
1.46 |
5.60 |
0.00 |
0.00 |
0.00 |
0.00 |
0.00 |
8.35 |
14 |
40.84 |
0.00 |
1.34 |
0.26 |
0.43 |
7.02 |
1.64 |
3.73 |
0.60 |
12.21 |
28 |
25.84 |
0.04 |
3.21 |
0.12 |
1.52 |
8.57 |
2.38 |
4.30 |
0.25 |
13.13 |
60 |
18.36 |
0.09 |
3.20 |
0.29 |
1.39 |
6.69 |
0.81 |
3.93 |
0.29 |
18.88 |
90 |
7.59 |
1.67 |
5.43 |
0.14 |
3.43 |
7.36 |
0.57 |
0.04 |
0.05 |
29.68 |
120 |
6.84 |
1.08 |
5.65 |
0.42 |
3.30 |
5.81 |
0.62 |
0.13 |
0.13 |
24.28 |
Unknowns: Sum of unknowns peaks and unresolved radioactivity.
Table 10. Partition of the no-extractable fraction (humin, humic acid and fulvic acid) after 120 days of incubation from GM, LVdf, RQ and PV soils (Percentage for the total applied radioactivity).
Soils |
% of applied (120 days) |
||
Humin |
Humin acid |
Fulvic acid |
|
GM |
20.27 |
7.99 |
3.39 |
LVdf |
14.18 |
1.69 |
10.95 |
RQ |
7.64 |
1.42 |
7.60 |
PV |
17.33 |
3.27 |
9.29 |
Table 11. Parameters of the Two Compartments Model for the test substance dissipation, and half-life and DT90 for Chlorothalonil in the Gleissolo Melanico Aluminico tipico (GM), Latossolo Vermelho Distroferrico tipico (LVdf), Neossolo Quartzarenico Ortico tipico (RQ) and Argissolo Vermelho Eutrofi&rrico chemossolico (PV) soils.
Soil |
Parameters of the Two Compartments Model |
R2 |
DT50 |
DT90 |
|||
C1a |
C2b |
K1c |
K2d |
||||
% |
% |
/days |
/days |
||||
GM |
18.759 |
71.907 |
0.031 |
0.265 |
0.99 |
2.96 |
21.23 |
LVdf |
86.253 |
6.055 |
0.141 |
0.01 |
0.99 |
4.73 |
20.03 |
RQ |
102.186 |
8.608 |
0.116 |
0.116 |
0.97 |
6.82 |
20.63 |
PV |
57.067 |
39.689 |
0.137 |
0.015 |
0.99 |
9.45 |
89.79 |
a. Maximum concentration remaining in the soil in the side one.
b. Maximum concentration remaining in the soil in the side two.
c. Rate constant for soil degradation of the test item in the side one.
d. Rate constant for soil degradation of the test item in the side two
Table 4. Distribution and Recovery of Radioactivity: Gartenacker
[14C]-labelled test substance |
Rep |
% of Applied Radioactivity in Sample at Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
31 |
60 |
90 |
122 |
||
Extract 1 (a) |
A |
88.7 |
NS |
87.4 |
86.0 |
80.2 |
72.9 |
65.5 |
64.3 |
55.7 |
44.6 |
B |
89.7 |
90.1 |
87.3 |
80.7 |
80.8 |
73.6 |
68.9 |
69.1 |
56.1 |
43.1 |
|
Mean |
89.2 |
90.1 |
87.4 |
83.4 |
80.5 |
73.3 |
67.2 |
66.7 |
55.9 |
43.9 |
|
Extract 2 (b) |
A |
4.7 |
NS |
5.3 |
5.3 |
7.0 |
5.7 |
5.8 |
5.3 |
4.6 |
6.5 |
B |
4.7 |
5.0 |
4.8 |
4.9 |
6.6 |
6.2 |
5.5 |
4.9 |
4.2 |
4.5 |
|
Mean |
4.7 |
5.0 |
5.1 |
5.1 |
6.8 |
6.0 |
5.7 |
5.1 |
4.4 |
5.5 |
|
Total Extractables |
A |
93.4 |
NS |
92.7 |
91.3 |
87.2 |
78.6 |
71.3 |
69.6 |
60.3 |
51.1 |
B |
94.4 |
95.1 |
92.1 |
85.6 |
87.4 |
79.8 |
74.4 |
74.0 |
60.3 |
47.6 |
|
Mean |
93.9 |
95.1 |
92.4 |
88.5 |
87.3 |
79.2 |
72.9 |
71.8 |
60.3 |
49.4 |
|
Non-Extractables |
A |
0.3 |
NS |
1.1 |
3.8 |
2.4 |
15.0 |
21.0 |
19.6 |
25.1 |
31.2 |
B |
0.3 |
0.1 |
1.3 |
5.0 |
2.8 |
13.7 |
18.0 |
26.4 |
25.7 |
31.0 |
|
Mean |
0.3 |
0.1 |
1.2 |
4.4 |
2.6 |
14.4 |
19.5 |
23.0 |
25.4 |
31.1 |
|
Alkaline Traps (as 14CO2) |
A |
NA |
NS |
< 0.1 |
< 0.1 |
0.1 |
0.2 |
1.2 |
3.1 |
4.0 |
5.3 |
B |
NA |
< LOQ |
< 0.1 |
< 0.1 |
0.1 |
< LOQ |
1.1 |
0.3 |
4.4 |
5.7 |
|
Mean |
- |
- |
< 0.1 |
< 0.1 |
0.1 |
0.1 |
1.2 |
1.7 |
4.2 |
5.5 |
|
Other Volatiles |
A |
NA |
NS |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
B |
NA |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Total % recovery (c) |
A |
93.7 |
NS |
93.8 |
95.1 |
89.7 |
93.8 |
93.5 |
92.3 |
89.4 |
87.6 |
B |
94.7 |
95.2 |
93.4 |
90.6 |
90.3 |
93.5 |
93.5 |
100.7 |
90.4 |
84.3 |
|
Mean |
94.2 |
95.2 |
93.6 |
92.9 |
90.0 |
93.7 |
93.5 |
96.5 |
89.9 |
86.0 |
|
Gartenacker: Overall Mean ± SD |
92.4 ± 3.5 |
||||||||||
(a) samples extracted twice with acetonitrile:0.3M HCl (4:1 v/v)
(b) samples extracted twice with acetonitrile:1.5M HCl (4:1 v/v)
(c) six samples had a mass balance < 90%. This is deemed to have no impact on the overall outcomes of the study.
NS: no sample, sample lost during sampling. Calculations based on single replicate
NA: not applicable
<LOQ: below limit of quantification
Table 5. Distribution and Recovery of
Radioactivity: 18 Acres
[14C]-labelled test substance |
Rep |
% of Applied Radioactivity in Sample at Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
31 |
60 |
90 |
122 |
||
Extract 1 (a) |
A |
92.3 |
92.2 |
90.7 |
84.0 |
81.4 |
70.4 |
62.4 |
54.1 |
51.1 |
46.9 |
B |
93.0 |
88.6 |
87.7 |
85.6 |
79.7 |
67.8 |
65.0 |
57.2 |
57.2 |
45.3 |
|
Mean |
92.7 |
90.4 |
89.2 |
84.8 |
80.6 |
69.1 |
63.7 |
55.7 |
54.2 |
46.1 |
|
Extract 2 (b) |
A |
3.2 |
3.0 |
3.6 |
4.3 |
5.7 |
7.4 |
9.0 |
7.1 |
6.9 |
9.4 |
B |
2.9 |
3.0 |
3.6 |
3.8 |
6.0 |
7.3 |
8.6 |
7.0 |
8.0 |
8.7 |
|
Mean |
3.1 |
3.0 |
3.6 |
4.1 |
5.9 |
7.4 |
8.8 |
7.1 |
7.5 |
9.1 |
|
Total Extractables |
A |
95.5 |
95.2 |
94.3 |
88.3 |
87.1 |
77.8 |
71.4 |
61.2 |
58.0 |
56.3 |
B |
95.9 |
91.6 |
91.3 |
89.4 |
85.7 |
75.1 |
73.6 |
64.2 |
65.2 |
54.0 |
|
Mean |
95.7 |
93.4 |
92.8 |
88.9 |
86.4 |
76.5 |
72.5 |
62.7 |
61.6 |
55.2 |
|
Non-Extractables |
A |
0.2 |
1.1 |
1.2 |
2.6 |
5.7 |
13.7 |
17.7 |
22.6 |
23.3 |
26.5 |
B |
0.2 |
0.6 |
1.5 |
4.2 |
4.7 |
14.4 |
20.6 |
22.2 |
23.2 |
24.5 |
|
Mean |
0.2 |
0.9 |
1.4 |
3.4 |
5.2 |
14.1 |
19.2 |
22.4 |
23.3 |
28.4 |
|
Alkaline Traps (as 14CO2) |
A |
NA |
< LOQ |
< 0.1 |
0.1 |
0.3 |
0.6 |
1.5 |
2.3 |
2.8 |
2.1 |
B |
NA |
< 0.1 |
< 0.1 |
<0.1 |
0.2 |
0.4 |
<0.1 |
4.9 |
1.0 |
5.1 |
|
Mean |
- |
< 0.1 |
< 0.1 |
0.1 |
0.3 |
0.5 |
0.8 |
3.6 |
1.9 |
3.6 |
|
Other Volatiles |
A |
NA |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
B |
NA |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Total % recovery |
A |
95.7 |
96.3 |
95.5 |
91.0 |
93.1 |
92.1 |
90.6 |
86.1 |
84.1 |
84.9 |
B |
96.1 |
92.2 |
92.8 |
93.6 |
91.6 |
89.9 |
94.2 |
91.3 |
89.4 |
83.6 |
|
Mean |
95.9 |
94.3 |
94.2 |
92.3 |
92.4 |
91.0 |
92.4 |
88.7 |
86.8 |
87.1 |
|
18 Acres: Overall Mean ± SD |
91.2 ± 3.9 |
||||||||||
(a) samples extracted twice with acetonitrile:0.3M HCl (4:1 v/v)
(b) samples extracted twice with acetonitrile:1.5M HCl (4:1 v/v)
(c) six samples had a mass balance < 90%. This is deemed to have no impact on the overall outcomes of the study.
NS: no sample, sample lost during sampling. Calculations based on single replicate
NA: not applicable
< LOQ: below limit of quantification
Table 6. Distribution and Recovery of
Radioactivity: East Anglia
[14C]-labelled test substance |
Rep |
% of Applied Radioactivity in Sample at Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
31 |
60 |
90 |
122 |
||
Extract 1 (a) |
A |
93.3 |
NS |
85.3 |
82.5 |
76.2 |
70.4 |
63.3 |
53.6 |
52.8 |
42.9 |
B |
99.4 |
89.2 |
86.2 |
85.6 |
78.8 |
71.2 |
64.6 |
59.2 |
52.5 |
44.9 |
|
Mean |
96.4 |
89.2 |
85.8 |
84.1 |
77.5 |
70.8 |
64.0 |
56.4 |
52.7 |
43.9 |
|
Extract 2 (b) |
A |
2.5 |
NS |
3.4 |
4.1 |
6.5 |
7.5 |
9.9 |
10.1 |
8.7 |
11.2 |
B |
2.7 |
2.8 |
3.4 |
3.8 |
7.5 |
7.8 |
9.6 |
9.0 |
8.5 |
11.4 |
|
Mean |
2.6 |
2.8 |
3.4 |
4.0 |
7.0 |
7.7 |
9.8 |
9.6 |
8.6 |
11.3 |
|
Total Extractables |
A |
95.8 |
NS |
88.7 |
86.6 |
82.7 |
77.9 |
73.2 |
63.7 |
61.5 |
54.1 |
B |
102.1 |
92.0 |
89.6 |
89.4 |
86.3 |
79.0 |
74.2 |
68.2 |
61.0 |
56.3 |
|
Mean |
99.0 |
92.0 |
89.2 |
87.9 |
84.5 |
78.5 |
73.7 |
66.0 |
61.3 |
55.2 |
|
Non-Extractables |
A |
0.9 |
NS |
2.3 |
4.5 |
4.0 |
12.2 |
16.4 |
19.9 |
18.1 |
22.2 |
B |
0.4 |
3.2 |
3.5 |
5.9 |
6.3 |
12.3 |
16.8 |
18.2 |
19.6 |
23.4 |
|
Mean |
0.7 |
3.2 |
2.9 |
5.2 |
5.2 |
12.3 |
16.6 |
19.1 |
18.9 |
22.8 |
|
Alkaline Traps (as 14CO2) |
A |
NA |
NS |
< 0.1 |
< 0.1 |
0.1 |
0.5 |
1.7 |
5.3 |
4.5 |
7.5 |
B |
NA |
< LOQ |
< LOQ |
< 0.1 |
0.2 |
0.1 |
0.8 |
4.5 |
5.7 |
7.0 |
|
Mean |
- |
- |
< 0.1 |
< 0.1 |
0.2 |
0.3 |
1.3 |
4.9 |
4.9 |
7.3 |
|
Other Volatiles |
A |
NA |
NS |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
B |
NA |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Total % recovery |
A |
96.7 |
NS |
91.0 |
91.1 |
86.8 |
90.6 |
91.3 |
88.9 |
84.1 |
83.8 |
B |
102.5 |
95.2 |
93.1 |
95.3 |
92.8 |
91.4 |
91.8 |
90.9 |
86.3 |
86.7 |
|
Mean |
99.6 |
95.2 |
92.1 |
93.2 |
89.8 |
91.0 |
91.6 |
89.9 |
85.2 |
85.3 |
|
East Anglia: Overall Mean ± SD |
91.1 ± 4.5 |
||||||||||
(a) samples extracted twice with acetonitrile:0.3M HCl (4:1 v/v)
(b) samples extracted twice with acetonitrile:1.5M HCl (4:1 v/v)
(c) six samples had a mass balance < 90%. This is deemed to have no impact on the overall outcomes of the study.
NS: no sample, sample lost during sampling. Calculations based on single replicate
NA: not applicable
< LOQ: below limit of quantification
Table 7. Distribution and Recovery of
Radioactivity: Capay
[14C]-labelled test substance |
Rep |
% of Applied Radioactivity in Sample at Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
30 |
59 |
91 |
120 |
||
Extract 1 (a) |
A |
103.3 |
91.2 |
87.1 |
86.4 |
84.9 |
86.4 |
80.3 |
77.5 |
68.7 |
73.0 |
B |
102.3 |
86.9 |
88.3 |
85.0 |
90.0 |
82.9 |
81.8 |
77.5 |
70.7 |
69.8 |
|
Mean |
102.8 |
89.1 |
87.7 |
85.7 |
87.5 |
84.7 |
81.1 |
77.5 |
69.7 |
71.4 |
|
Extract 2 (b) |
A |
4.2 |
2.7 |
3.9 |
4.6 |
4.1 |
3.7 |
5.0 |
5.5 |
7.0 |
8.0 |
B |
3.2 |
3.0 |
3.7 |
4.4 |
4.9 |
4.2 |
6.4 |
6.4 |
6.4 |
8.1 |
|
Mean |
3.7 |
2.9 |
3.8 |
4.5 |
4.5 |
4.0 |
5.7 |
5.9 |
6.7 |
8.1 |
|
Total Extractables |
A |
107.5 |
93.9 |
91.0 |
91.0 |
89.0 |
90.1 |
85.3 |
83.0 |
75.7 |
81.0 |
B |
105.5 |
89.9 |
92.0 |
89.4 |
94.9 |
87.1 |
88.2 |
83.9 |
77.1 |
77.9 |
|
Mean |
106.5 |
91.9 |
91.5 |
90.2 |
92.0 |
88.6 |
86.8 |
83.5 |
76.4 |
79.5 |
|
Non-Extractables |
A |
0.1 |
0.2 |
0.8 |
0.7 |
1.3 |
2.5 |
3.8 |
5.3 |
9.9 |
10.1 |
B |
0.1 |
0.2 |
0.4 |
1.0 |
1.5 |
3.0 |
4.6 |
5.0 |
9.9 |
10.2 |
|
Mean |
0.1 |
0.2 |
0.6 |
0.9 |
1.4 |
2.8 |
4.2 |
5.2 |
9.9 |
10.2 |
|
Alkaline Traps (as 14CO2) |
A |
NA |
< 0.1 |
< 0.1 |
< 0.1 |
< 0.1 |
< 0.1 |
0.1 |
0.1 |
0.2 |
0.1 |
B |
NA |
< 0.1 |
< 0.1 |
< 0.1 |
< 0.1 |
0.1 |
0.1 |
0.1 |
0.1 |
0.2 |
|
Mean |
- |
< 0.1 |
< 0.1 |
< 0.1 |
< 0.1 |
0.1 |
0.1 |
0.1 |
0.2 |
0.2 |
|
Other Volatiles |
A |
NA |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
B |
NA |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
< LOQ |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Total % recovery |
A |
107.6 |
94.1 |
91.8 |
91.7 |
90.3 |
92.6 |
89.2 |
88.4 |
85.8 |
91.2 |
B |
105.6 |
90.1 |
92.4 |
90.4 |
96.4 |
90.2 |
92.9 |
89.0 |
87.1 |
88.3 |
|
Mean |
106.6 |
92.1 |
92.1 |
91.1 |
93.4 |
91.4 |
91.1 |
88.7 |
86.5 |
89.8 |
|
Capay: Overall Mean ± SD |
92.3 ± 5.5 |
||||||||||
(a) samples extracted twice with acetonitrile:0.3M HCl (4:1 v/v)
(b) samples extracted twice with acetonitrile:1.5M HCl (4:1 v/v)
(c) six samples had a mass balance < 90%. This is deemed to have no impact on the overall outcomes of the study.
NS: no sample, sample lost during sampling. Calculations based on single replicate
NA: not applicable
< LOQ: below limit of quantification
Table 8. Summary of Characterisation /
Identification of Radioactive Residues in Soil Extracts: Gartenacker
Components |
Replicate |
Component as % AR at Each Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
31 |
60 |
90 |
122 |
||
The test substance |
A |
94.5 |
94.0 |
89.6 |
77.5 |
63.7 |
39.2 |
15.9 |
6.2 |
1.5 |
3.0 |
B |
94.5 |
90.3 |
84.8 |
80.4 |
61.2 |
33.4 |
20.5 |
11.1 |
3.1 |
2.9 |
|
Mean |
94.5 |
92.2 |
87.2 |
79.0 |
62.5 |
36.3 |
18.2 |
8.7 |
2.3 |
3.0 |
|
Table 9. Summary of Characterisation / Identification of Radioactive Residues in Soil Extracts: 18 Acres
Components |
Replicate |
Component as % AR at Each Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
31 |
60 |
90 |
122 |
||
The test substance |
A |
93.7 |
NS |
78.5 |
66.2 |
45.0 |
25.2 |
8.6 |
2.9 |
1.1 |
1.9 |
B |
100.3 |
88.8 |
80.7 |
70.1 |
50.1 |
24.6 |
6.3 |
3.9 |
1.3 |
1.9 |
|
Mean |
97.0 |
88.8 |
79.6 |
68.2 |
47.6 |
24.9 |
7.5 |
3.4 |
1.2 |
1.9 |
|
Table 10. Summary of Characterisation
/ Identification of Radioactive Residues in Soil Extracts: East Anglia
Components |
Replicate |
Component as % AR at Each Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
31 |
60 |
90 |
122 |
||
The test substance |
A |
93.7 |
NS |
78.5 |
66.2 |
45.0 |
25.2 |
8.6 |
2.9 |
1.1 |
1.9 |
B |
100.3 |
88.8 |
80.7 |
70.1 |
50.1 |
24.6 |
6.3 |
3.9 |
1.3 |
1.9 |
|
Mean |
97.0 |
88.8 |
79.6 |
68.2 |
47.6 |
24.9 |
7.5 |
3.4 |
1.2 |
1.9 |
|
Table 11. Summary of Characterisation
/ Identification of Radioactive Residues in Soil Extracts: Capay
Components |
Replicate |
Component as % AR at Each Timepoint (DAT) |
|||||||||
0 |
6 h |
1 |
3 |
7 |
14 |
30 |
59 |
91 |
120 |
||
The test substance |
A |
106.9 |
92.3 |
89.2 |
88.6 |
84.2 |
74.3 |
66.2 |
48.8 |
39.3 |
18.7 |
B |
105.4 |
89.6 |
89.8 |
86.3 |
89.0 |
78.0 |
62.7 |
49.1 |
37.8 |
13.6 |
|
Mean |
106.2 |
91.0 |
89.5 |
87.5 |
86.6 |
76.2 |
64.5 |
49.0 |
38.6 |
16.2 |
|
Table 12. Summary of DegT50
and DegT90 Values
Soil |
SFO |
|||||
DegT50 [days] |
DegT90 [days] |
K |
χ2 |
R2 |
Prob > t |
|
Gartenacker |
11 |
35 |
0.0655 |
9.25 |
0.9741 |
4.629E-08 |
18 Acres |
12 |
39 |
0.0585 |
4.73 |
0.9936 |
1.886E-13 |
East Anglia |
7 |
24 |
0.0946 |
4.89 |
0.9941 |
2.486E-13 |
Capay |
58 |
194 |
0.0119 |
6.05 |
0.9572 |
2.603E-11 |
SFO: Single first order kinetics (non-linear method) calculated using a software
DegT50: Calculated degradation half-life of parent (time taken for 50% degradation of parent compound)
DegT90: Time taken for 90% degradation of parent compound
K: Rate Constant
χ2: Chi-square statistical value
R2:Linear regression coefficient relating goodness of fit as value approaches unity
Prob > t: Statistical probability value related to a statistical t-test calculation
Description of key information
Geometric mean DT50 in soil = 4.2 d, 20 °C, OECD TG 307 (or similar), Green 2015; Wicksted 2015; Tornisielo 2006; and EPA 162 -1, Gibbings & Bramley 2000; Bramley & Gibbings 2001; Duane 1995
Key value for chemical safety assessment
- Half-life in soil:
- 4.2 d
- at the temperature of:
- 20 °C
Additional information
DT50 values for the substance in soil under aerobic standard test conditions
USDA/Name/Origin |
OC [%] / pH (water) |
T [°C] / Moisture [%] |
DT50 [d] (Kinetic model in original report) |
Author / Year |
Marsillargues / Silty Clay/ France |
1.0 / 7.8 |
20 ± 2 /22.71 |
4.7 (SFO) |
Green / 2015 |
18 Acres / Sandy Clay loam / UK |
2.3 / 6.0 |
20 ± 2 /29.78 |
4.7 (SFO) |
Green / 2015 |
Gartenacker / Loam / Switzerland |
2.6 / 7.0 |
20 ± 2 / 38.95 |
1.5 (SFO) |
Green / 2015 |
White Swan / Loam/Silt loam / USA |
1.7 / 5.9 |
20 ± 2 / 36.6 |
5.1 (SFO) |
Green / 2015 |
18 Acres / Loam / UK |
4.5 / 6 |
20 / - |
1(SFO) |
Bramley & Gibbings / 2001 |
Chamberlain's Farm / Loamy sand / UK |
3.2 / 7.5 |
20 / - |
0.3 (SFO) |
Bramley & Gibbings / 2001 |
ERTC / Sandy loam / USA |
1.3 / 6.7 |
20 / -
|
1.3 (SFO) |
Bramley & Gibbings / 2001 |
Munster / Loamy sand / Germany |
2.6 / 5.6 |
20 / -
|
1.9 (SFO) |
Bramley & Gibbings / 2001 |
Gartenacker/ Loam / Switzerland |
2 / 7.5 |
20 ± 2 / 34.8
|
11 (SFO) |
Wicksted / 2015 |
18 Acres/ Sandy clay loam/ UK |
3.3 / 5.9 |
20 ± 2 / 28.1
|
12 (SFO) |
Wicksted / 2015 |
East Anglia / Sandy loam/ UK |
2.3 / 7.5 |
20 ± 2 / 22.6
|
7 (SFO) |
Wicksted / 2015 |
Capay / Clay loam/ USA |
0.8 / 7.9 |
20 ± 2 / 17.2
|
58 (SFO) |
Wicksted / 2015 |
Capay / Clay / USA |
2 / 4.1 |
20 / 40 |
4.73 (SFO) |
Tornisielo / 2006 |
Capay / Loamy sand / USA |
0.3 / 4.9 |
20 / 40
|
6.82 (SFO) |
Tornisielo / 2006 |
Capay / Clay / USA |
2.8 / 5.6 |
20 / 40 |
9.45 (SFO) |
Tornisielo / 2006 |
18 Acres / Sandy clay loam/ UK |
5.0 (% OM) / 6.5 |
20 / - |
0.53 (Treatment rate 0.1µg/g) |
Bramley & Gibbings / 2000 |
18 Acres / Sandy clay loam/ UK |
5.0 (% OM) / 6.5 |
20 / - |
1.2 (Treatment rate 1µg/g) |
Bramley & Gibbings / 2000 |
18 Acres / Sandy clay loam/ UK |
5.0 (% OM) / 6.5 |
20 / -
|
9.7 (Treatment rate 10µg/g) |
Bramley & Gibbings / 2000 |
18 Acres / Sandy clay loam/ UK |
5.0 (% OM) / 6.5 |
20 / -
|
17.1 (Treatment rate 25µg/g) |
Bramley & Gibbings / 2000 |
PO soil / Loamy sand/ USA |
2.6 (% OM) / 5.1 |
24 / 74.5
|
4.9 (SFO) (Treatment rate1 ppm) |
Duane / 1995 |
PO soil / Loamy sand/ USA |
2.6 (% OM) / 5.1 |
24 / 74.7
|
18 (SFO) (Treatment rate 10 ppm) |
Duane / 1995 |
Geomean
|
|
|
4.3 |
|
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.
