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EC number: 217-588-1 | CAS number: 1897-45-6
Biodegradation in water and sediment: simulation tests
Administrative data
Link to relevant study record(s)
- Endpoint:
- biodegradation in water: sediment simulation testing
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 17 Oct 2000 to 13 Dec 2001
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- test procedure in accordance with national standard methods
- Qualifier:
- according to guideline
- Guideline:
- other: BBA Guideline Part IV; 5-1
- Version / remarks:
- December 1990
- Deviations:
- not specified
- Qualifier:
- according to guideline
- Guideline:
- other: OECD Guidelines For the Testing of Chemicals, Draft Proposal For A New Guideline, Aerobic and Anaerobic Transformation in Water-Sediment Systems
- Version / remarks:
- October 1999
- Deviations:
- not specified
- GLP compliance:
- yes
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Inoculum or test system:
- natural water / sediment: freshwater
- Details on source and properties of surface water:
- An overview of the characterisation data for the sediment and water are summarised in Table 1 and Table 2 in 'Any other information on materials and methods incl. tables'.
- Sampling location: The water and sediment sampled from two sources, Emperor Lake and Bury Pond. The Emperor Lake water and sediment were sampled at Chatsworth (Derbyshire, UK). The Bury Pond water and sediment were sampled at Ramsey, Huntingdon (Cambridgeshire, UK).
- Sampling procedure: The surface water was filtered through a 250 µm sieve. Each wet sediment was prepared by sieving to 2 mm to remove any stones or debris, then thoroughly mixed to provide homogenous samples. The sediments were then left to settle at approximately 4 °C in large polypropylene containers. The surface layer of water on the sediment, which formed on standing, was decanted off and discarded.
- Storage conditions: The collected sediment and associated water were stored at ca 4 °C until dispensed into the incubation vessels
- Storage length: Up to 8 days
- Meaurements: The dry matter content of the sediments was determined by drying portions (54 - 68 g for Emperor Lake and 66 - 70 g for Bury Pond) of wet sediment in triplicate, at approximately 103 °C for 48 hours. A sub-sample of each of the 2 mm-sieved wet sediments was taken for characterisation. Approximately 1 litre of each of the 250 µm filtered waters were taken for characterisation. - Details on source and properties of sediment:
- See 'Details on source and properties of surface water'.
- Details on inoculum:
- - Preparation of Water-Sediment Test Systems: The wet sediments were dispensed into cylindrical glass vessels and the associated natural waters were added to a total weight of 200 g. The Emperor Lake test systems contained 73.66 ± 0.05 g wet weight of sediment and the Bury Pond test systems contained 82.14 ± 0.05 g wet weight of sediment. Both wet sediment weights were equivalent to 40 g dry weight. The water-sediment (dry weight) ratios in the vessels were approximately 4: 1 w/w. Throughout the study, water levels were maintained by gravimetric addition, as necessary, of the appropriate surface water. The additional water for this purpose was stored in the dark at < 7 °C.
- Acclimation: The water-sediment systems were acclimatised at ca 20°C for 26 days (Emperor Lake) and 29 days (Bury Pond) prior to treatment with the test substance, to allow equilibration, as determined by the assessment of the redox potential, pH and dissolved oxygen. - Duration of test (contact time):
- >= 100 - <= 103 d
- Initial conc.:
- 30 µg/L
- Based on:
- test mat.
- Remarks:
- nominal initial concentration in the water phase
- Initial conc.:
- 300 µg/L
- Based on:
- test mat.
- Remarks:
- used in an additional experiment to aid metabolite identification only
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Details on study design:
- The actual applied rate of 14C-Labelled test substance to the water- sediment system is provided in Table 3 in 'Any other information on materials and methods incl. tables'.
TEST CONDITIONS
- Test temperature: 20 ± 2 °C
- Preparation of 30 µg/L treatment rate solutions: The radiochemical was received in a concentrated state. The radiochemical was diluted with acetonitrile to give the stock solution (10 mL) contained in a tube. This was then further subjected to serial dilution prior to quantification by LSC. The stock solution contained 16.86 MBq in 10 mL. Following quantification of the stock solution, the solvent was removed under a stream of nitrogen for optimum storage of the radiochemical. Separate application solutions were prepared for each sediment type and for each application rate. Application solutions were prepared so that when applied to the water phase of the water-sediment systems, application rates of 30 µg/L and 300 µg/L were achieved in the surface water of that system. To prepare for the Emperor Lake 30 µg/L application solution, the radiochemical was diluted in acetonitrile (5 mL) to give a fresh stock solution An aliquot of the stock solution (500 µL) was further diluted with 5.5 mL acetonitrile to give a total volume of 6 mL in the application solution. The application solution contained approximately 1.48 MBq of activity. An aliquot of the stock solution was also removed for the 300 µg/L application solution. The remaining stock solution was again concentrated under nitrogen for frozen storage. To prepare the Bury Pond 30 µg/L application solution, the radiochemical (now containing nominally 10.39 MBq ) was diluted in acetonitrile (4 mL) to give a new stock solution. An aliquot of the ‘Bury Pond’ stock solution (770 µL) was further diluted with 6.23 mL acetonitrile to give a total volume of 7 mL in the ‘Bury Pond’ application solution. The application solution contained approximately 1.57 MBq of activity. An aliquot of the stock solution was also removed for the 300 µg/L application solution. The remaining stock solution was again concentrated under nitrogen for frozen storage.
- Application of treatment to the water-sediment systems to achieve 30 µg/L Rate: Immediately prior to application, the water-sediment systems were removed from the air-flow system. The application solution was added to the surface water in each system using a M250 Microman pipette, to achieve an application rate of 30 µg/L in the water. The vessels were carefully agitated, to ensure homogeneity, without disturbing the sediment layer, then, reconnected to the air-flow system, with the exception of the 0 HAT (hours after treatment) samples, which were
analysed immediately. The application volume was 115 µL (29139 Bq) of the 14C-labelled test substance application solution to the Emperor Lake water-sediment systems, to achieve a 30 µg/L application rate. The application volume was 118 µL (26399 Bq) of the 14C-labelled test substance application solution to the Bury Pond water-sediment systems. Aliquots of the application solution were taken immediately prior to, midapplication and immediately after application to the test systems. This was used to determine the homogeneity of the treatment solutions and the actual application rate for each type of water-sediment system. Each aliquot was diluted to 25 mL in acetonitrile and the radioactivity present determined by LSC. To confirm the purity and stability of the application solution, aliquots of the application solution were analysed by TLC and HPLC immediately prior to and after treatment of the test vessels. Water-sediment systems designated for redox potential measurements were treated with non-radiolabelled test substance in water. These applications resulted in the same nominal application rates as for the systems treated with 14C-labelled test substance, i.e. 30 µg/L.
- Preparation of 300 µg/L treatment rate solutions: An exaggerated application rate of ten times the 30 µg/L application rate was required to aid metabolite identification. Separate application solutions were prepared for each sediment type. To prepare the Emperor Lake 300 µg/L application solution, an aliquot of the stock solution (1660 µL) was further diluted with 0.34 mL acetonitrile to give a total volume of 2 mL of the application solution in a plastic scintillation vial. The application solution contained nominally, 4.76 MBq, of activity. The remaining stock solution was again concentrated under nitrogen for frozen storage. To prepare the Bury Pond 300 µg/L application solution, an aliquot of the ‘Bury Pond’ stock solution (2200 µL) was taken. The application solution contained approximately 4.53 MBq of activity. The remaining stock solution was again concentrated under nitrogen for frozen storage.
- Treatment of Water-Sediment Systems to achieve 300 µg/L Rate: Immediately prior to application, the water-sediment systems were removed from the air-flow system. The application solution was added to the surface water in each system using a M250 Microman pipette, to achieve an application rate of 300 µg/L in the surface water. The vessels were carefully agitated, to ensure homogeneity without disturbing the sediment layer, then, reconnected to the air-flow system. The application volume was 119 µL (289850 Bq) of the 14C-labelled test substance application solution to the Emperor Lake water-sediment systems. The application volume was 127 µL (255250 Bq) of the 14C-lablled test substance application solution to the Bury Pond water-sediment systems. Aliquots of the application solution were taken immediately prior to, mid and immediately after treating the test systems. These were used to determine the homogeneity of the treatment solutions and the actual application rate for each water-sediment system type. Each aliquot was diluted to 25 mL in acetonitrile and the radioactivity present determined by LSC. To confirm the purity and stability of the application solution, aliquots of the application solution were analysed by TLC (with the Bioimager) and HPLC immediately prior to and after treatment of the test vessels.
- Aeration: The treated water-sediment vessels were connected to an air-flow system. Moist air flowed over the water surface in the sediment vessels.
- Continuous darkness: Yes
- Microbial assessment: At the start of the study, the Emperor Lake and Bury Pond water-sediment systems were equilibrated for 20 and 16 days respectively, prior to commencing the biomass assessments. At study completion, the final water-sediment system biomass assessments were conducted at 135 days after treatment, for Emperor Lake and 127 days for the Bury Pond samples respectively. The biomass was estimated from the respiratory response following the addition of glucose to selected watersediment systems, based on the method of Anderson and Domsch for soil microbial biomass determinations
TEST SYSTEM
- Culturing apparatus: Cylindrical glass vessels
- Details of trap for CO2 and volatile organics if used: The column effluent gases passed through a foam bung (to trap organic volatiles) and two sodium hydroxide (2M) liquid traps, to capture any mineralised carbon dioxide produced.
SAMPLING
- Water parameter: The redox potential, pH and dissolved oxygen of the water and the redox potential of the sediment were determined from duplicate samples at approximately weekly intervals throughout the equilibration period. These measurements were continued at approximately two weekly intervals during the test incubation period. If the designated vessels gave variable results, then additional samples were used or the measurements were carried out more often, to ensure reequilibration of the systems.
- Application solution: Aliquots of the application solution were taken immediately prior to, mid and immediately after treating the test systems. These were used to determine the homogeneity of the treatment solutions and the actual application rate for each water-sediment system type. Each aliquot was diluted to 25 mL in acetonitrile and the radioactivity present determined by LSC. To confirm the purity and stability of the application solution, aliquots of the application solution were analysed by TLC (with the Bioimager) and HPLC immediately prior to and after treatment of the test vessels.
- water- sediment system: The first sampling took place at 0 HAT (immediately after application) with subsequent sampling taking place at 2, 4, 6, 11 HAT and 1, 3, 7, 14, 43, 76 and 100 days after treatment (DAT) for the Emperor Lake (EL) systems. The first sampling took place at 0 HAT (immediately after application) with subsequent sampling taking place at 2, 4, 6, 11 HAT and 1, 3, 7, 14, 47, 75 and 103 days after treatment (DAT) for the Bury Pond (BP) systems.
- Sampling method: At each sampling interval, duplicate water-sediment vessels were removed from the incubation system. One sample from each time-point was stored frozen for reference purposes. In the case of the 0 HAT (hours after treatment) samples, one was analysed immediately, without being connected to the air-flow system and one replicate was frozen. For these stored systems, the surface water was
aspirated off the sediment and weighed. The remaining sediment and its associated surface water were stored frozen (< -20 °C). All trapping solutions were removed from the air-flow system at each sampling time point and replaced with fresh sodium hydroxide solutions. In the case of 14 DAT BP, the frozen stored replicate was used for method development work on the un-extracted residue. In the case of 7 DAT BP, the analysis replicate was used to generate the aqueous and extract samples for the half life determinations and for the initial comparison co-chromatography with the Emperor Lake samples. Following this analysis, the 7 DAT EL and BP aqueous and extract samples were left in a fridge at 5 °C for a week and storage stability data showed that the samples were not stable over this time. So the frozen, stored 2nd replicate for 7 DAT BP (00JH149/58) was used to provide an aqueous and extract sample for further characterisation by TLC. Fortunately the 7 DAT EL samples had been fully characterised prior to the temporary storage at 5°C.
To minimise degradation, surface water samples (up to 14 DAT) were analysed by HPLC on the sampling day, immediately after they were separated from the sediments and by TLC analysis within two hours. Surface water samples from the remaining time points were analysed by TLC within 2 days of the sampling day. The TLC data was used to provide the quantitative data for this report, while the HPLC analysis provided supporting qualitative data for the presence of the test substance and other metabolites at individual sampling times. Where sediment extracts contained more than 5% of applied activity they were analysed on the sampling day, or in the case of the 3,7 and 14 DAT time points, concentrated in vacuo then analysed within 9 weeks of the sampling day. All the study samples were stored frozen at < -20°C. Some samples were found to have degraded during storage and were not used for further characterisation . Only samples, which gave a qualitatively similar profile after storage to the original analysis, were analysed further.
- Storage stability: Storage stability TLC data for the Bury Pond samples had shown that the samples 4 HAT, 11 HAT, 1 DAT and 3 DAT could not be characterised by solvent system 8B, due to breakdown of thethe test substance in the more basic surface water. Surface water samples after these time points were further characterised in solvent system 8B. In the case of the 7 DAT Bury Pond, the first replicate samples were used in the determination of the half lives. Subsequently these samples were found to have degraded on storage, so the second replicate samples were used for further TLC characterisation. The TLC profiles of the 1st and 2nd replicate samples were qualitatively similar. - Compartment:
- natural water / sediment: freshwater
- % Non extractable:
- 68.9
- % CO2:
- 0.3
- % Recovery:
- 96.3
- Remarks on result:
- other: 100 Days after treatment; Emperor Lake
- Compartment:
- natural water / sediment: freshwater
- % CO2:
- 0.4
- % Other volatiles:
- 67.2
- % Recovery:
- 91.1
- Remarks on result:
- other: 103 Days after treatment; Bury Pond
- Parent/product:
- parent
- Compartment:
- total system
- % Degr.:
- 100
- Parameter:
- radiochem. meas.
- Sampling time:
- 43 d
- Remarks on result:
- other: Emperor Lake
- Parent/product:
- parent
- Compartment:
- total system
- % Degr.:
- 100
- Parameter:
- radiochem. meas.
- Sampling time:
- 47 d
- Remarks on result:
- other: Bury Pond
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 59.4 h
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Emperor Lake; Total System
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 20.1 h
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Bury Pond; Total System
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 59.4 h
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Emperor Lake; Surface Water
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 20.1 h
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Bury Pond; Surface Water
- Other kinetic parameters:
- first order rate constant
- pseudo-first order rate constant
- Transformation products:
- not specified
- Details on transformation products:
- - Radioactive Degradation Products in the Emperor Lake Systems: In the surface water the amount of the test substance decreased from an average value of 88.1% immediately after application, to 1.4% of applied by 14 days. The HPLC traces illustrate how the test substance degraded to M18 and to many minor components with time, in the surface water. TLC analysis showed that the degradation of the test substance was very complex, with the 7 DAT samples showing the largest number of components. The major component was identified asM18, with at least ten minor components also being formed. M18 increased from 2.1% applied to a maximum of 10.1% by 7 days in the Emperor Lake surface water, then further declined to 1.0% by 100 days. The presence of M18 in selected samples was confirmed in the reverse phase TLC solvent system 33. Several compounds were detected at low levels, but unfortunately they could not be resolved in solvent system 8B. A combination of M4 and M24/Na reached a maximum of 4.4% applied by 1 DAT, then declined. A combination of M23 and M9 reached a maximum of 2.0% applied by 7 DAT, then declined. None of the minor unknown components or the streaking on the TLC plate (nondiscrete activity) exceeded 6.5% of applied activity in the Emperor Lake surface water at any time during the study. The polar base line material increased to a maximum of 10.6% at 7 DAT then declined. The complex TLC profile of the sediment extract was very similar to that from the surface water in solvent system 8B. No test substance was detected in the sediment extracts and only traces of M18 were found, that increased from 1% applied at day 3 to a maximum of 1.7% by 14 days after treatment, then declined. The following compounds were detected at very low levels in the sediment. A combination of M4 and M24/Na reached a maximum of 1.0% applied by 3 DAT, then declined . A combination of M23 and M9 reached a maximum of 0.6% applied by 76 DAT, then declined. No single minor component or streaking exceeded 3.7% of applied in the sediment extracts. On a whole system basis (water plus sediment) the test substance could not be detected by 43 days. The amount of M18 increased to 11.5% by 7 DAT then declined to 1.7% applied by 100 days. However as noted before the amount of M18 present is an over estimation due to the cochromatography with Unknown A. M4 and M24/Na reached a combined maximum of 5.1% applied by 7 DAT then declined. M23 and M9 reached a combined maximum of 2.2% applied by 7 DAT. The soil metabolite M5 was not detected. Again no single minor component or streaking exceeded 6.5% of applied activity in the total system.
- Radioactive Degradation Products in the Bury Pond Systems: In the Bury Pond surface water, the amount of the test substance decreased from an average value of 90.3% applied immediately after application, to 0.7% of applied by 14 days. The HPLC traces illustrate how the test substance degraded to M18 and to many minor components with time in the surface water. TLC analysis showed that the degradation of the test substance was very complex with the 7 DAT samples showing the largest number of components. Comparison of the TLC profiles for the 7 DAT Emperor Lake and 7 DAT Bury Pond samples showed them to be qualitatively very similar. The major component was M18, with at least ten minor components also being formed. M18 decreased from 8.9% applied for the 7 DAT surface water sample to 0.6% of applied activity by 47 days. The presence of M18 in the 7 DAT Bury Pond surface water sample was confirmed by reverse phase TLC. Several compounds were detected at low levels, but unfortunately they could not be resolved in solvent system 8B. A combination of M4 and M24/Na reached a maximum of 4.8% applied by 7 DAT, then declined. A combination of M23 and M9 reached a maximum of 1.9% applied by 7 DAT, then declined. None of the minor components or the streaking on the TLC plate (non-discrete activity) exceeded 3.8% of applied in the Bury Pond surface water between 7 days and 47 days after treatment. The base line material increased to a maximum of 21.8% of applied at 14 DAT then declined. The complex TLC profile of the sediment extract w-as very similar to that from the surface water in solvent system 8B. No test substance was detected in the sediment extracts and the amount of M18 formed, remained at approximately 1.5% applied from 7 days to 47 days. By HPLC very low levels of M4 and M9 were detected. By TLC a combination of M4 and M24/Na reached a maximum of 1.4% applied. M23 and M9 reached a combined maximum of 0.4% applied. No single minor component or streaking exceeded 3.1% of applied in the sediment extracts. On a whole system basis (water plus sediment) the test substance was not detected by 47 days. The amount of M18 declined from 10.3% at 7 days after treatment. A combination of M4 and M24/Na reached a maximum of 6.2% applied by day 7, then declined. M23 and M9 reached a combined maximum of 2.2% applied by 7 DAT then declined. M5 was not detected. No single minor component or streaking exceeded 4.5% of applied activity in the total system. - Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results is provided in Table 4 – Table 10 in 'Any other information on results incl. tables'.
- Purity and Homogeneity of the 30 µg/L Application Solution: The radiochemical purity of the application solution, used to treat the sediment water systems, was determined prior to and post application. These data confirmed the stability of the test material through out the application process. The pre and post application values as determined by TLC analysis were averaged to determine the purity for the chemical at the time of application.
The average radiochemical purity of the 14C-labelled test substance applied to the test systems was 98.6% for Emperor Lake systems and 98.9% for Bury Pond respectively. Data from LSC analysis of the solutions confirmed that the solutions remained homogeneous throughout the application.
- Application Rate 30 µg/L: An application rate of 31.2 µg/L (104% of target ) was applied to the Emperor Lake systems and that 30.4 µg/L (101% of target) was applied to the Bury Pond systems.
- Application Rate 300 µg/L: For the exaggerated application rate, 311.6 µg/L (104% of target) was applied to the Emperor Lake systems and 294.0 µg/L (98% of target) was applied to the Bury Pond systems.
- Microbial Biomass Assessments: The biomass assessment showed that the two water-sediment systems were microbially active at the start and the end of the test incubation period.
- Total Recovery of Applied Radioactivity: The total amount of radioactivity recovered from each water-sediment system was calculated from the sum of the activity found in the surface water, the sediment extract, the glass wash of the sediment vessel, the sediment debris (unextracted activity) and the sodium hydroxide traps (14CO2). Radioactivity recovered from the 14C-labelled test substance treatment of Emperor Lake systems was 96.4% of applied at zero hours after treatment (HAT). Recoveries then varied between 90.3% and 97.6% of applied activity, giving an average recovery of 95.2% of applied activity over all sampling points of the study. Radioactivity recovered from the 14C-labelled test substance treatment of Bury Pond systems was 99.4% of applied at zero hours after treatment (HAT). Recoveries then varied between 84.2% and 123.8% (75 DAT) of applied activity, giving an average recovery of 99.7% of applied activity over all sampling points of the study.
- Distribution of Radioactivity: Only trace amounts of carbon dioxide were recovered from the sodium hydroxide traps during the incubation period. In the Emperor Lake system carbon dioxide was only detected from 43 DAT onwards. This reached a maximum of 0.3% applied by 100 DAT for the total cumulative carbon dioxide. A similar situation was found with the Bury Pond system with a maximum of 0.4% applied evolved by 103 DAT for the total cumulative carbon dioxide. The radioactivity in the surface water declined from 92.0% applied immediately after application to 42.0% of applied by 14 days after treatment (DAT) in the Emperor Lake system. In the Bury Pond system the radioactivity declined from 97.2% applied immediately after application to 38.9% of applied by 14 DAT. The extractable radioactivity from the sediment increased very slowly with time for both systems. In the Emperor Lake system, a maximum of 15.3% of activity was present in the sediment extract by day 14, declining to 13.9% by 100 DAT. For the Bury Pond system a maximum of 18.8% of applied activity was found in the sediment extract by 47 DAT, which declined to 12.5% by 103 DAT. The radioactivity became increasingly bound to both sediments with time. At the end of the study, the unextracted residue had reached 68.9% of applied in the Emperor Lake and 67.2% in the Bury Pond systems. The unextracted figure for the 75 DAT sampling was considered to be an outlier as the unextracted residue was increasing with time. Further attempts to fractionate this “unextracted” activity by acid hydrolysis, showed that up to 86% of the recovered activity remained bound to the sediment post hydrolysis. As a result the activity bound to the sediment post hydrolysis is considered to be bio-unavailable.
- Radioactive Residues in Surface Waters and Sediment Extracts: All water samples and sediment extracts containing greater than 5% of the applied radioactivity were analysed by TLC. The TLC data from solvent systems 51 and 49 was used to quantify the amounts of the test substance remaining. These values were averaged for a particular time point to determine the t1/2. Solvent system 49 was used to quantify the unknowm components which chromatographed together at Rf > 0.8. The unknown components increased to a maximum at 7 days after treatment for both systems, then declined. Since the 7 DAT samples for both sediment systems showed the greatest amounts of unknowns, these samples were investigated further. The unknown metabolites in the samples were co-chromatographed with reference standards and the constituent components quantified in solvent system 8B. In this system the amount of reference standard M18 applied to the TLC plates was found to affect the resolution, Rf and accuracy of quantification of the component designated as Unknown A. These metabolites could not be consistently resolved, therefore the amounts of M18 and Unknown A were estimated. This situation represents an over-estimation of the amounts of M18 present throughout the study. Further characterisation was carried out in solvent systems 33 and 10, when reference standards co-eluted in solvent system 8B. If resolution of the minor components was not possible, then their values were estimated from solvent system 8B The total amounts of individual components in the surface water and the sediment extracts were tabulated separately, then the values for the total system were obtained by the summation of the individual components in the two phases.
- DT50 for the test substance in the Surface Waters and Total Water-Sediment Systems: The degradation rate of the test substance was determined using the curve fitting program. This was done by fitting the experimental data to both a simple first order model (SFO) and to a first order multicompartment (FOMC) model. A statistical comparison of the fit of the two curve shapes was then made. It was found that the additional parameter in the FOMC model was not statistically significant at the 10% level, so the simple first order model was adequate. The degradation of the test substance was therefore expressed in terms of a half life (t1/2). which was derived using the SFO model. As the test substance did not partition in to the sediment, the t1 /2 values for the surface water and whole system were identical. The test substance was rapidly dissipated from the surface water and the whole Emperor Lake system with a t1/2 of 59.4 hours. The test substance was rapidly dissipated from the surface water and the whole Bury Pond system with a t1/2 of 20.1 hours. - Validity criteria fulfilled:
- yes
- Conclusions:
- The test substance was rapidly and extensively degraded in natural water sediment systems. It degraded more rapidly in the slightly alkaline sandy clay loam Bury Pond sediment water matrix than in the more acidic sandy loam Emperor Lake system. The DT50 were estimated to be 59 hours and 20 hours for the Emperor Lake and Bury Pond systems, respectively. A single major degradate (> 10% of applied test substance) was formed (M18) by 7 days after treatment. This degradate declined over the remainder of the 100 day study period. Numerous other minor products were also produced showing extensive breakdown of the parent chemical, with only negligible amounts of CO2 evolved from the systems. Of the major soil metabolites, only M9 and M4 were detected and these were at very low levels. A significant amount of radioactivity became bound to the sediment with time and could not be released by harsh extraction. This radioactivity is therefore not believed to be bioavailable.
- Executive summary:
The degradation of 14C-lablled test substance, labelled in the phenyl ring, was investigated in two laboratory incubated natural sediments and their associated waters. Two texturally different sediments, Emperor Lake (sandy loam) and Bury Pond (sandy clay loam) were used. The study was conducted without following guideline but in compliance with GLP criteria.
The water-sediment systems were set up in cylindrical glass vessels. Aeration of the water was achieved by drawing moist air over its surface. The effluent gases from each unit were passed through traps to allow the collection of any volatiles or carbon dioxide, which may have been generated. The test substance was applied to the surface water in each vessel to give a nominal initial concentration of 30µg/L in the water phase. The test systems were incubated in the dark at 20 ± 5 °C for up to 103 days. The distribution of the 14C-lablled test substance and its metabolites was determined at a number of time points, in the surface water and sediment layers after separation of the two phases.
Half lives (t1/2) values for the test substance dissipation in the surface waters were 59.4 hours and 20.1 hours for the Emperor Lake and Bury Pond systems respectively. In the total water-sediment systems, the t1/2 values were identical due to the test substance not partitioning into the sediment phase. Degradation of the test substance was rapid and extensive, with a single major degradate (> 10% of applied test substance) formed in the first 7 days after treatment. This degradate M18 declined over the remainder of the study period. Numerous other minor products were also produced showing extensive breakdown of the parent chemical, with only negligible amounts of CO2 evolved from the systems. A significant amount of radioactivity became bound to the sediment with time and could not be released by harsh extraction. This radioactivity is therefore not believed to be bioavailable.
- Endpoint:
- biodegradation in water: simulation testing on ultimate degradation in surface water
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 27 Oct 2011 to 22 Jan 2015
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 308 (Aerobic and Anaerobic Transformation in Aquatic Sediment Systems)
- Version / remarks:
- adopted 24 April 2002
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- EPA OPPTS 835.4300 (Aerobic Aquatic Metabolism)
- Version / remarks:
- October 2008
- Deviations:
- no
- Qualifier:
- according to guideline
- Guideline:
- EPA OPPTS 835.4400 (Anaerobic Aquatic Metabolism)
- Version / remarks:
- October 2008
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic/anaerobic
- Inoculum or test system:
- natural water / sediment: freshwater
- Details on source and properties of surface water:
- An overview of the sampling dates and the locations is provided in Table 1 in 'Any other information on materials and methods incl. tables'. The characterisation data for the sediment and water are summarised in Table 2 in 'Any other information on materials and methods incl. tables'.
- Sampling location and procedure: The water and sediment sampled from two sources, Swiss Lake and Calwich Abbey. The Swiss Lake water and sediment were sampled at Chatsworth (Derbyshire, UK). The Calwich Abbey water and sediment were sampled at Calwich (Staffordshire, UK). The water was sampled from the lakes using a bucket and subsequently transferred into containers. The sediments were sampled by scoop or bucket and transferred into containers.
- Storage and preparation: After receipt, the water-sediment systems were stored at ca 4°C and prepared for incubation as soon as possible. Prior to characterisation and dispensing, the water was passed through a 0.2 mm sieve and the sediment was passed through a 2 mm sieve.
- Properties of test system: The surface water and sediment samples were characterised under a separate GLP study. The following characterisation data were obtained for each sediment: pH (water and CaCl2), organic matter content (Walkley-Black/Loss on Ignition method), organic carbon content, cation exchange capacity, particle size distribution and textural classification (USDA), water holding capacity and carbonate content. The following characterisation data were obtained for each water sample: pH, electrical conductivity, dissolved organic carbon, total suspended solids, nitrate content and hardness (EDTA titration). Total nitrogen and phosphorus (sediment and water) and phosphate content (water only) was also determined but was excluded from the compliance statement for the characterisation report.
- Microbial biomass: Biomass samples were treated with the equivalent volume of solvent used during application of the test substance. Samples were taken prior to test item application and following the final sampling interval. The microbial biomass of the water-sediment test systems was determined using a fumigation extraction method. At each timepoint, the sediment and water from 4 replicate incubation vessels were transferred to suitable containers. Three of the samples were treated with ethanol free chloroform (prepared by washing 100 mL chloroform with 2 x 40 mL Milli-Q water using a separating funnel) at a rate of 10 µL/g. The treated samples were placed in a chamber containing beakers of soda lime and 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 water-sediment samples and the control sample were extracted with ca 250 mL of 0.5M potassium sulphate by shaking on a flat bed shaker (ca 45 min). Samples were filtered using Buchner apparatus and filter paper. Extracts were stored at ca + 4 ºC prior to total organic carbon (TOC) analysis. - Details on source and properties of sediment:
- See 'Details on source and properties of surface water'.
- Details on inoculum:
- PREPARATION OF THE WATER-SEDIMENT SYSTEM
- Sediment moisture content: The moisture content of the sediments was determined by drying duplicate aliquots in an oven at ca 110 °C overnight. The weight of sediment was recorded before and after drying and the difference in weight attributed to moisture content. The moisture content of the Swiss Lake and Calwich Abbey sediments were determined as 79.1 and 169.9%, respectively, on a dry weight basis.
- Determination of test system target weights: For Swiss Lake, the target weights of sediment and water for the test system were determined using duplicate test vessels. Aliquots of the sediment were weighed into glass cylindrical incubation bottles (7.5 cm diameter) to a height of ca 2.7 cm. With the minimum of disturbance, associated surface water was added to a target height of ca 7.5 cm to provide the target volumetric sediment to water ratio of 1:3. The target weight of fresh sediment per sample was 164.7 g, equivalent to 92.0 g oven dry equivalent. The target weight of water per sample was 359.1 g. For Calwich Abbey, the target weights of sediment and water for the test system were determined using duplicate test vessels. Aliquots of the sediment were weighed into glass cylindrical incubation bottles (8.8 cm diameter) to a height of ca 2.8 cm. With the minimum of disturbance, associated surface water was added to a target height of ca 8.3 cm to provide the target volumetric sediment to water ratio of 1:3. The target weight of fresh sediment per sample was 189.2 g, equivalent to 70.1 g oven dry equivalent. The target weight of water per sample was 571.7 g.
- Preparation of test systems: Aliquots of test sediment were added to incubation bottles of the same dimensions as used to determine the target weights. Appropriate surface water was added to each test vessel taking care to avoid disturbance of the sediment. Bottles were then left to settle before connection to the incubation apparatus. For the aerobic and anaerobic incubation groups, duplicate test vessels were prepared for control measurements. The vessels had a platinum combination electrode placed in situ at the base of the vessel for measuring redox. - Duration of test (contact time):
- 100 d
- Initial conc.:
- 0.33 mg/L
- Based on:
- test mat.
- Remarks:
- Swiss
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Details on study design:
- An overview of the study design was provided in Table 3 and Table 4 in 'Any other information on materials and methods incl. tables'.
TEST SOLUTIONS (Swiss Lake)
- Application rate: The field application rate of 1000 g a.i./ha equates to a nominal application of 0.33 µg/mL in each test vessel, assuming a water column depth of 30 cm. Duplicate test flasks were prepared and the volume of water was determined as 431.8 cm3, equivalent to 142 µg of test item per sample.
- Test solution: The stock [14C]-labelled test substance container was washed with acetonitrile and the wash made to a final volume of 8 mL. The homogeneity and radioactivity content of the solution was determined by LSC analysis.
- Application procedure: A pipette was used to apply the treatment solution to the study samples. A 53 µL treatment solution was applied dropwise to each sample. Following application, each flask was reconnected to the flow through apparatus. Acetonitrile was added to each biomass and control sample. To accurately quantify the amount of test item applied to each sample, an additional 7 aliquots of treatment solution were dispensed directly into 10 mL volumetric flasks at regular intervals during each treatment. Each was made up to volume with acetonitrile and aliquots (3 x 100 µL) taken for LSC analysis.
TEST SOLUTIONS (Calwich Abbey)
- Application rate: Duplicate test flasks were prepared and the volume of water was determined as 690.8 cm3, equivalent to 228 µg of test item per sample.
- Test solution: Approximately 18 mg of [14C]-labelled test substance was dispensed into a vial and dissolved in 7 mL acetonitrile. The homogeneity and radioactivity content of the solution was
determined by LSC analysis.
- Application procedure: A pipette was used to apply the treatment solution to the study samples. A 68 µL treatment solution was applied dropwise to each sample. Following application, each flask was reconnected to the flow through apparatus. Acetonitrile was added to each biomass and control sample. To accurately quantify the amount of test item applied to each sample, an additional 7 aliquots of treatment solution were dispensed directly into 10 mL volumetric flasks at regular intervals during each treatment. Each was made up to volume with acetonitrile and aliquots (3 x 100 µL) taken for LSC analysis.
TEST SYSTEM (both Swiss Lake and Calwich Abbey systems )
- Method used to create aerobic conditions: Samples designated for aerobic incubation (Incubation Groups A, B, E, F, I and J) were connected to a flow through apparatus and each bottle was connected to two traps filled with 2M sodium hydroxide for the collection of evolved 14CO2. Moist air was drawn through the test samples using a vacuum pump at a gentle flow rate equivalent to approximately a single bubble present in the sodium hydroxide trap at a time. Samples were wrapped in aluminium foil to exclude light.
- Method used to create anaerobic conditions: Samples designated for anaerobic incubation (Incubation Groups C, D, G, H, K and L) were connected to a flow through apparatus and each bottle was connected to two traps filled with 2M sodium hydroxide for the collection of evolved 14CO2. Moist nitrogen (oxygen free) was introduced to the test samples at a gentle flow rate equivalent to approximately a single bubble present in the sodium hydroxide trap at a time. Samples were wrapped in aluminium foil to exclude light and incubated
- Acclimation: Samples were acclimatised under the relevant incubation conditions for 17-28 days prior to application. Control measurements (% oxygen saturation, redox and pH) were recorded at
regular intervals in the aerobic and anaerobic controls during the acclimatisation period and at each sampling time point during the study. In addition, continuous pH measurements over a 24h period were taken from a representative sample from Incubation Groups I and J.
SAMPLING
- Sampling intervals and procedures are provided in Table 5 “Any other information on materials and methods incl. tables”. - Compartment:
- natural water / sediment: freshwater
- % Total extractable:
- 63.4
- % Non extractable:
- 29.6
- % CO2:
- 0.3
- % Recovery:
- 93.2
- Remarks on result:
- other: Aerobic Swiss Lake; on day 102
- Compartment:
- natural water / sediment: freshwater
- % Total extractable:
- 30.7
- % Non extractable:
- 65.2
- % CO2:
- < 0.1
- % Recovery:
- 95.9
- Remarks on result:
- other: Aerobic Calwich Abbey; on day 102
- Parent/product:
- parent
- Compartment:
- total system
- % Degr.:
- 2
- Parameter:
- radiochem. meas.
- Sampling time:
- 29 d
- Remarks on result:
- other: Aerobic Swiss Lake
- Parent/product:
- parent
- Compartment:
- total system
- % Degr.:
- 3.6
- Parameter:
- radiochem. meas.
- Sampling time:
- 15 d
- Remarks on result:
- other: Aerobic Calwich Abbey
- Key result
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 9 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Aerobic; the total Swiss Lake system
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 3 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Aerobic; the total Calwich Abbey system
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 10 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Aerobic; the water phase of Swiss Lake system
- Compartment:
- natural water / sediment: freshwater
- DT50:
- 3 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: Aerobic; the water phase of Calwich Abbey system
- Other kinetic parameters:
- first order rate constant
- pseudo-first order rate constant
- Transformation products:
- not specified
- Details on transformation products:
- AEROBIC INCUBATION
- Radioactive residues in water phase: For Swiss Lake, levels of the test substance decreased from 82.4% AR at 0 DAT to 1.5% AR at 29 DAT. No test substance was detected from 48 DAT onwards. Two significant radioactive components were detected and co-chromatographed with M18 and M4. These reached maximum levels of 15.7% AR at 29 DAT and 12.9% AR at 7 DAT, respectively. Low levels of radioactive components which co-chromatographed with M8, M17, M13 and M19 were detected and reached maximums of 1.0%, 2.8%, 2.5% and 2.0% AR, respectively. Three metabolites, which did not co-chromatograph with reference standards, were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 6.7% AR at 29 DAT and 7.1% AR and 3.6% AR at 102 DAT, respectively. For Calwich Abbey, levels of the test substance decreased from 84.9% AR at 0 DAT to 3.6% AR at 14 DAT. No test substance was detected from 29 DAT onwards. Two significant radioactive components were detected and co-chromatographed with M18 and M4. These reached maximum levels of 34.2% AR at 14 DAT and 44.5% AR at 7 DAT, respectively. Lower levels of radioactive components which co-chromatographed with M8,M17 M13 and M19 were detected and reached maximums of 5.4%, 3.6%, 1.5% and 7.1% AR, respectively. Three metabolites, which did not co-chromatograph with reference standards, were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 6.2% AR at 29 DAT, 2.6% AR at 46 DAT and 1.0% AR at 102 DAT, respectively.
- Radioactive residues in sediment extracts: For Swiss Lake, levels of the test substance increased from 7.3% AR at 0 DAT to 8.5% AR at 3 h, before decreasing to 0.5% AR at 29 DAT. No test substance l was detected from 48 DAT onwards. Two significant radioactive components were detected and co-chromatographed with M18 and M4, reaching maximum levels of 11.6% AR at 29 DAT and 6.3% AR at 29 DAT, respectively. Low levels of radioactive components which cochromatographed with M8, M13 and M19 were detected and reached maximums of 1.3%, 0.6% and 0.7% AR, respectively. Three metabolites, which did not cochromatograph with reference standards, were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 0.2% AR and 17.9% AR at 102 DAT and 7.1% AR at 29 DAT, respectively. For Calwich Abbey, levels of the test substance decreased from 4.8% AR at 0 DAT to 2.1% AR at 7 DAT. No test substance was detected from 14 DAT onwards. Two radioactive components were detected and co-chromatographed with M18 and M4 and reached maximum levels of 6.4% AR at 7 DAT and 4.2% AR at 60 DAT, respectively. Radioactive components which co-chromatographed with M8, M17 and M19 were also detected and reached maximums of 3.3% AR at 29 DAT, 9.0% AR at 14 DAT and 8.0% AR at 14 DAT, respectively. Three metabolites which did not co-chromatograph with reference standards were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 1.1% AR at 46 DAT and 3.1% AR and 2.2% AR at 102 DAT, respectively.
- Radioactive residues in the total system: For Swiss Lake, levels of the test substance decreased from 89.6% AR at 0 DAT to 2.0% AR at 29 DAT. No test substance was detected from 48 DAT onwards. Two significant radioactive components were detected and co-chromatographed with M18 and M4. These reached maximum levels of 26.2% AR at 29 DAT and 11.4% AR at 29 DAT, respectively. Low levels of radioactive components which co-chromatographed with M8, M17, M13 and M19 were detected and reached maximums of 1.4%, 2.8%, 2.7% and 2.0% AR, respectively. Three metabolites, which did not co-chromatograph with reference standards, were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 6.7% AR at 29 DAT, 24.9% AR at 102 DAT and 7.1% AR at 29 DAT, respectively. For Calwich Abbey, levels of the test substance decreased from 89.6% AR at 0 DAT to 3.6% AR at 14 DAT. No test substance was detected from 29 DAT onwards. Four significant radioactive components were detected and co-chromatographed with M18, M17, M19 and M4. These reached maximum levels of 36.3% AR at 14 DAT, 11.7% AR at 14 DAT, 9.5% AR at 29 DAT and 46.5% AR at 7 DAT, respectively. Lower levels of radioactive components which co-chromatographed with M8 and M13 were detected and reached maximums of 7.3% AR at 46 DAT and 1.5% AR at 14 DAT, respectively. Three metabolites which did not co-chromatograph with reference standards were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 6.3% AR at 29 DAT and 5.2% AR and 3.2% AR at 102 DAT, respectively.
AEROBIC INCUBATION
- Radioactive residues in water phase: For Swiss Lake, levels of the test substance decreased from 86.9% AR at 0 DAT to 0.7% AR at 29 DAT. No test substance was detected from 48 DAT onwards. Three significant radioactive components were detected and co-chromatographed with M18, M19 and M4. These reached maximum levels of 35.2% AR at 29 DAT, 8.7% AR at 15 DAT and 6.1% AR at 29 DAT, respectively. Radioactive components which co-chromatographed with M8,M17 and M13 were detected and reached maximums of 0.8%, 2.7% and 4.0% AR, respectively. Three metabolites, which did not co-chromatograph with reference standards, were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2. These reached maximum levels of 7.4% AR at 48 DAT, 4.7% AR and 6.3% AR at 102 DAT, respectively. For Calwich Abbey, levels of the test substance decreased from 88.4% AR at 0 DAT to 6.4% AR at 14 DAT. No test substance was detected from 29 DAT onwards. Three significant radioactive components were detected and co-chromatographed with M4,M18 and M8. These reached maximum levels of 38.8% AR at 14 DAT, 9.2% AR at 46 DAT and 5.8% AR at 102 DAT, respectively. Lower levels of radioactive components which cochromatographed with M13, M17 and M19 were detected and reached maximums of 6.8% AR at 46 DAT, 2.2% AR at 14 DAT and 2.6% AR at 7 DAT, respectively. Three metabolites, which did not co-chromatograph with reference standards, were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2. These reached maximum levels of 5.1% AR at 29 DAT, 12.5% AR at 60 DAT and 4.6% AR at 102 DAT, respectively.
- Radioactive residues in sediment extracts: For Swiss Lake, levels of the test substance increased from 6.9% AR at 0 DAT to 10.6% AR at 6 h, before decreasing to 0.1% AR at 29 DAT. No test substance was detected from 48 DAT onwards. Radioactive components which co-chromatographed with M8,M18 and M4 were detected and reached a maximum of 3.4% AR at 102 DAT, 5.0% AR at 29 DAT and 2.7% AR at 61 DAT, respectively. Three metabolites which did not cochromatograph with reference standards were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 0.9% AR at 48 DAT and 4.3% AR and 6.0% AR at 102 DAT, respectively. For Calwich Abbey, levels of the test substance increased from 3.5% AR at 0 DAT to 3.6% AR at 1 h, before decreasing to 3.4% AR at 6 h. No test substance was detected from 1 DAT onwards. Radioactive components were detected and co-chromatographed with M8,M17 and M18. These reached maximum levels of 6.7% AR at 60 DAT, 12.8% AR at 29 DAT and 10.8% AR at 29 DAT, respectively. Radioactive components which cochromatographed with M19 and M4 were detected and reached maximums of 6.3% AR at 14 DAT and 3.3% AR at 46 DAT. Two metabolites which did not co-chromatograph with reference standards were detected at 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 2.4% AR at 60 DAT and 4.5% AR at 102 DAT, respectively.
- Radioactive residues in the total system: For Swiss Lake, levels of the test substance decreased from 93.8% AR at 0 DAT to 0.8% AR at 29 DAT. No test substance was detected from 48 DAT. Three significant radioactive components were detected and co-chromatographed with M18, M19 and M4. These reached maximum levels of 40.2% AR at 29 DAT, 8.7% AR at 15 DAT and 10.1% AR at 29 DAT, respectively. Radioactive components which co-chromatographed with M8, M17 and M13 were detected and reached maximums of 3.4% AR at 102 DAT, 2.9% AR at 48 DAT, and 4.0% AR at 48 DAT, respectively. Three metabolites which did not co-chromatograph with reference standards were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 8.2% AR at 48 DAT and 9.0% AR and 12.3% AR at 102 DAT, respectively. For Calwich Abbey, levels of the test substance decreased from 91.9% AR at 0 DAT to 6.4% AR at 14 DAT. No test substance was detected from 29 DAT onwards. Radioactive components were detected and co-chromatographed with M8, M18,M19 and M4. These reached maximum levels of 10.9% AR at 102 DAT, 14.1% AR at 29 DAT, 41.4% AR at 14 DAT, 8.4% AR at 14 DAT and 12.4% AR at 48 DAT, respectively. A radioactive component which co-chromatographed with M13 was detected and reached a maximum level of 6.8% AR at 46 DAT. Three metabolites which did not co-chromatograph with reference standards were detected at 38, 40 and 44 minutes when samples were analysed using HPLC Method 2, these reached maximum levels of 5.1% AR at 29 DAT, 14.9% AR at 60 DAT and 9.0% AR at 102 DAT, respectively. - Evaporation of parent compound:
- no
- Volatile metabolites:
- yes
- Remarks:
- See 'Any other information in results incl tables' and 'Details on transformation products'.
- Residues:
- yes
- Remarks:
- See 'Any other information in results incl tables' and 'Details on results'.
- Details on results:
- An overview of the results is provided in Table 6 – Table 16 in 'Any other information on results incl. tables'.
- Microbial Biomass: Biomass results indicated healthy microflora at study initiation. Microbial biomass for Swiss Lake at initiation was 282.4 and 237.1 mg carbon/kg (1.5% and 1.2% organic carbon) of sediment for aerobic and anaerobic incubations, respectively. Microbial biomass for Calwich Abbey at initiation was 266.4 and 202.2 mg carbon/kg (0.5% and 0.4% organic carbon) of sediment for aerobic and anaerobic incubations, respectively. Measurements at the end of the incubation period (100 DAT) demonstrated that the test systems remained viable throughout the study. Microbial biomass for Swiss Lake at termination was 204.2 and 209.6 mg carbon/kg (1.1% and 1.1% organic carbon) of sediment for aerobic and anaerobic incubations, respectively. Microbial biomass for Calwich Abbey at termination was 274.4 and 218.7 mg carbon/kg (0.6% and 0.4% organic carbon) of sediment for aerobic and anaerobic incubations, respectively.
- Radiochemical Purity: The radiochemical purity of the [14C]-labelled test substance in the treatment solutions was determined by HPLC and TLC immediately prior to application (> 97.4%) and after application (> 96.0%).
- Reflux extraction: Reflux extraction with acetonitrile:1.5M hydrochloric acid (4:1, v/v) was performed on selected 102 DAT samples where unextractable residues contained >10% AR following initial solvent extraction. This procedure liberated a maximum range of 3.6-5.6% AR across all water-sediment systems. No further analysis was carried out on these samples.
- Organic matter fractionation: Further characterization of selected bound residues by OMF demonstrated that the majority of 14C was associated with the humin fraction (≤ 47.1% AR). Small amounts of 14C were associated with the humic acid (≤ 8.7% AR) and with the fulvic acid fraction (≤ 9.9% AR).
- Proposed degradation pathway: Degradation of the test substance was complex and involved numerous reactions: Oxidative dichlorination; Cyano hydrolysis; Reductive dichlorination; Reaction with cysteine/glutathione with further metabolism and ring closure; Oxidative cleavage of the glutathione conjugate to form the sulphate; Sulphur oxidation.
AEROBIC INCUBATION
- Mass balance: 95.2 to 99.7% of applied radioactivity was recovered at 0 DAT. The overall recovery range for all samples was ranging from 84.9 to 102.1% of applied radioactivity.
- Swiss Lake: Mean 92.6% (Four samples had an overall recovery < 90% (range 84.9 – 89.2%))
- Calwich Abbey: Mean 96.8 % (A single sample had an overall recovery < 90% (89.3%))
- Volatile degradation products: Radioactivity recovered as evolved 14CO2 throughout the study was low. Small amounts of radioactivity were evolved as volatile products throughout the course of the study. The mean values of 14CO2 evolved at end of study were 0.3% for Swiss Lake system and 0.1% for Calwich Abbey system. No trapping of other volatiles was conducted on the aerobic incubation groups.
ANAEROBIC INCUBATION
- Mass balance: 95.2 to 99.9% of applied radioactivity at 0 DAT. The overall recovery range for all samples was ranging from 88.1 to 100.4% of applied radioactivity (A single Swiss Lake sample had an overall recovery < 90% (88.1%)).
- Swiss Lake: Mean 93.4 %
- Calwich Abbey: Mean 97.8 %
- Volatile degradation products: Radioactivity recovered as evolved 14CO2 throughout the study was low. The mean value of 14CO2 evolved at end of study was ≤ 0.1% for both Swiss Lake system and Calwich Abbey system. No radioactivity was recovered in the catalytic converter traps indicating that 14C-methane was not produced.
DT50 OF THE TEST SUBSTANCE IN THE WATER-SEDIMENT SYSTEMS
The dissipation of [14C]-labelled test substance from the water column and degradation rate (DegT50 and DegT90) of the test substance in the test system was determined using non-linear regression and a single first order kinetic model. SFO kinetics describes the dissipation and degradation of the test substance well with a Chi-square (χ2) error value of less than or equal to 8.0. The rate of dissipation of the test substance from the water column for Swiss Lake was 10 and 5 days for aerobic and anaerobic incubations, respectively. The corresponding values for Calwich Abbey were 3 and 4 days, respectively. The degradation (DegT50) of the test substance in the total test system (sum of surface water and sediment extract) was 9 and 4 days for Swiss Lake aerobic and anaerobic incubations, respectively. The corresponding values for Calwich Abbey were 3 and 4 days, respectively. As the test substance does not partition readily into the sediment, the kinetics of the total system are therefore not greatly affected by the inclusion of the sediment phase. - Validity criteria fulfilled:
- yes
- Conclusions:
- Based on the findings, the DT50 values of the Swiss Lake system in aerobic condition were calculated to be 10 and 9 days for the surface water and total system, respectively. The DT50 values of the Calwich Abbey system in aerobic condition for both surface water and total system were 3 days. The major transformation products in the aerobic water-sediment systems were M8, M17 and M19 (all >5% AR in Calwich Abbey), and M18 and M4 (>5% AR in both Calwich Abbey and Swiss Lake).
- Executive summary:
The rate and route of degradation of [14C]-labelled test substance was investigated in 2 dissimilar water-sediment systems, Swiss Lake (sandy loam) and Calwich Abbey (silt loam), at a dose rate of 0.33 mg/kg and after incubation at 20°C in the dark under aerobic and anaerobic conditions. The study was conducted in according to OECD TG 308 and in compliance with GLP criteria. Volatile radioactivity was continuously flushed from the vessels and collected in traps. For each test system, duplicate samples were taken for analysis at 11 intervals, up to 100 days.
The mean mass balance from all aerobic samples was in the range 88.1 - 100.0% AR. The mean mass balance from all anaerobic samples was in range 90.1 - 99.9% AR. Under aerobic conditions the major transformation products of substance were found to be M17, M18, M19 and M4, which reached maximum levels of 11.7%, 36.3%, 9.5% and 46.5% AR, respectively. Minor degradates M8 and M13 were also detected reaching maximums of 7.3% and 2.5% AR, respectively. Under anaerobic conditions the major transformation products of substance were found to be M17, M18, M19, M8 and M4, which reached maximum levels of 14.1%, 41.4%, 8.7%, 10.9% and 12.4% AR, respectively. M13 was also detected reaching a maximum of 6.8% AR. In addition, a number of discrete unknown metabolites were also observed under aerobic and anaerobic conditions, each individual not exceeding 5% of applied radioactivity. Under aerobic conditions, 14CO2 reached maximum levels of 0.3% AR in Swiss Lake samples and <0.1% AR in Calwich Abbey samples. Under anaerobic conditions, 14CO2 were <0.1% AR in both sediments.
Under aerobic conditions, the DT50 value of the water column was 10 and 3 days for Swiss Lake and Calwich Abbey, respectively. The DegT50 values of the total systems were 9 days (Swiss Lake) and 3 days (Calwich Abbey). Under anaerobic conditions, the DT50 value of the water column was 5 and 4 days for Swiss Lake and Calwich Abbey, respectively. The DegT50 values of the total systems were 4 days (Swiss Lake) and 4 days (Calwich Abbey). As substance does not partition readily into the sediment, the kinetics of the total system are therefore not greatly affected by the inclusion of the sediment phase.
- Endpoint:
- biodegradation in water: simulation testing on ultimate degradation in surface water
- Type of information:
- experimental study
- Adequacy of study:
- key study
- Study period:
- 04 Nov 2013 to 26 Mar 2015
- Reliability:
- 1 (reliable without restriction)
- Rationale for reliability incl. deficiencies:
- guideline study
- Qualifier:
- according to guideline
- Guideline:
- OECD Guideline 309 (Aerobic Mineralisation in Surface Water - Simulation Biodegradation Test)
- Version / remarks:
- April 2004
- Deviations:
- no
- GLP compliance:
- yes (incl. QA statement)
- Radiolabelling:
- yes
- Oxygen conditions:
- aerobic
- Inoculum or test system:
- natural water: freshwater
- Details on source and properties of surface water:
- Sampling details and properties of the water are provided in Table 1 and Table 2 in 'Any other information on materials and methods incl. tables'.
- Details on collection: Sampled at Calwich Abbey Lake, Staffordshire, England.
- Collection procedure: The water was scooped from the lake and passed through a 100 µm (high rate) or 212 µm (low rate) sieve into a 20 L bottle - Duration of test (contact time):
- >= 60 - <= 65 d
- Initial conc.:
- 10 µg/L
- Based on:
- test mat.
- Initial conc.:
- 50 µg/L
- Based on:
- test mat.
- Parameter followed for biodegradation estimation:
- CO2 evolution
- radiochem. meas.
- Details on study design:
- Detailed information of experimental design and sampling is provided in Table 3 - Table 5 in 'Any other information on materials and methods incl. tables'.
PREPARTION OF TEST SYSTEM
- Surface water: Aliquots (100 mL) of the surface water were dispensed into pre-labelled glass vessels (250 mL). These vessels labelled with the study number and a code representing the incubation group. Sterile samples were prepared by autoclaving vessels containing surface water on two separate occasions separated by 24 h. Sterile in-line air filters (0.2 µm PTFE) were attached to the inlet and outlet tubing connected to sterile control vessels to maintain sterility.
- Radiochemical purity: The radiochemical purity of the stock [14C]-labelled test substance was determined by HPLC and TLC. The radiochemical purity of [14C]-labelled test substance in the treatment solutions was determined by HPLC and TLC immediately prior to application.
- Preparation of treatment solutions: For the low rate and low rate sterile controls, ca 0.599 mg of [14C]-labelled test substance was dispensed into a vial and dissolved in 25 mL acetonitrile. The homogeneity and radioactivity content of the solution was determined by LSC analysis. For the high rate and accompanying sterile controls, ca 5 mg of [14C]-labelled test substance was dispensed into a vial and dissolved in 5 mL acetonitrile. The homogeneity and radioactivity content of the solution was determined by LSC analysis. The low rate phase sodium benzoate treatment solution was prepared by taking 100 µL of [14C]-benzoic acid and concentrating to near dryness. This sample was reconstituted in 175 µL of 1 mM sodium hydroxide and made to a final volume of 2 mL with Milli-Q water. Duplicate aliquots were taken for LSC. A subsample (1 mL) was diluted to give a final concentration of 10.0 µg/L and the radioactivity content determined by LSC. The high rate phase sodium benzoate treatment solution was prepared by adding 250 µL of Milli-Q water to a trace amount of [14C]-Sodium benzoate. Triplicate aliquots were taken for LSC and the concentration determined as 10.6 µg/L.
- Application of [14C]-labelled test substance: A pipette was used to apply the test item treatment solution to the study samples. Treatment solution (1 mL for low rate and 7 µL for high rate) was applied to each sample. Following application, each flask was reconnected to the flow through apparatus. To accurately quantify the amount of test item applied to each sample, additional aliquots (1 mL or 7 µL as appropriate) of treatment solution were dispensed and taken for LSC analysis.
- Application of [14C]-sodium benzoate: A pipette was used to apply the sodium benzoate treatment solution to the control samples. Treatment solution (1 mL for low rate and 8 µL for high rate) was applied to each sample. Following application, each flask was reconnected to the flow through apparatus. To accurately quantify the amount of test item applied to each sample, an additional 2 aliquots (1 mL or 8 µL as appropriate) of treatment solution were dispensed during dosing and taken for LSC analysis.
TEST SYSTEM
- Culturing apparatus: Glass flask
- Number of culture flasks/concentration: 2
- Method used to create aerobic conditions: Moist air bubbled through system
- Method used to trap CO2 & organic volatiles: Two traps filled with 2M NaOH for 14CO2
SAMPLING
- Sampling method used per analysis type: At each sampling interval, duplicate samples from each incubation group were removed for analysis. The recovery of radioactivity in liquid samples was determined by LSC analysis. Surface water samples were analysed directly by TLC or HPLC.
- Structure assignment: Structural assignment for parent substance and its metabolites was made by co-chromatography with authenticated reference standards in HPLC or TLC. - Reference substance:
- benzoic acid, sodium salt
- Compartment:
- natural water: freshwater
- % Recovery:
- 96.4
- Remarks on result:
- other: 10 µg/L test concentration
- Compartment:
- natural water: freshwater
- % Recovery:
- 95
- Remarks on result:
- other: 50 µg/L test concentration
- Parent/product:
- parent
- Compartment:
- water
- % Degr.:
- 100
- Parameter:
- radiochem. meas.
- Sampling time:
- 5 d
- Remarks on result:
- other: 10 µg/L test concentration
- Parent/product:
- parent
- Compartment:
- water
- % Degr.:
- 100
- Parameter:
- radiochem. meas.
- Sampling time:
- 60 d
- Remarks on result:
- other: 50 µg/L test concentration
- Key result
- Compartment:
- natural water: freshwater
- DT50:
- 6 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: 50 µg/L test concentration
- Compartment:
- natural water: freshwater
- DT50:
- 0.4 d
- Type:
- (pseudo-)first order (= half-life)
- Temp.:
- 20 °C
- Remarks on result:
- other: 10 µg/L test concentration
- Other kinetic parameters:
- pseudo-first order rate constant
- Transformation products:
- not specified
- Details on transformation products:
- For the low rate, levels of the test substance decreased from 67.4% AR at 0 DAT to 4.7% AR at 2 DAT. No test substance was detected from 5 DAT onwards. Two significant radioactive components were detected and co-chromatographed with M13 and M4. M13 reached a maximum level of 6.3% AR at 60 DAT, whilst M4 reached a maximum level of 79.9% AR at 29 DAT, decreasing to 71.9% AR at 60 DAT. Origin bound material reached a maximum of 11.1% AR at 5 DAT. The majority of the origin bound material was shown experimentally to be the metabolite M4 (mean of 10.4% AR) A maximum of 4.8% AR (29 DAT) was recovered in the apparatus wash. Levels of 14CO2 reached a maximum level of 10.8% AR at 60 DAT. For the high rate, levels of the test substance decreased from 91.5% AR at 0 DAT to 1.6% AR at 60 DAT. Three significant radioactive components were detected and co-chromatographed with M18, M13 and M4. M18 reached a maximum level of 32.1% AR at 60 DAT. M13 reached a maximum level of 13.9% AR at 60 DAT, whilst M4 reached a maximum level of 12.2% AR at 5 DAT, decreasing to 7.2% AR at 60 DAT. A maximum of 9.8% AR (30 DAT) was recovered in the apparatus wash and the majority was confirmed as the test substance, M13 or M4. In addition a number of discrete unknown degradates were observed, none exceeding 5.7% AR at a single timepoint. As these components were not detected in the low rate samples, no further characterisation work was carried out. Levels of 14CO2 reached a maximum level of 1.2% AR at 60 DAT. In low rate sterile samples, sampled at 65 DAT, the test substance accounted for 3.3% AR, showing that the rate of degradation was slower but qualitatively similar to the non-sterile test samples. Two radioactive components were detected which co-chromatographed with M4 and M13. M4 accounted for 76.4% AR, whilst M13 accounted for 1.1% AR. Origin bound material, likely M4, accounted for 7.7% AR. Unidentified products accounted for 2.4% AR. Levels of 14CO2 accounted for 0.3% AR. For the high rate sterilised samples, the mean level of parent compound was 22.4% AR 59 DAT. The metabolites M4 and M13 accounted for 8.9% AR and 3.4% AR in the sterile samples, respectively at 59 DAT. Three components were detected at greater than 5% AR (up to 11.9% AR) which were not detected in low rate samples, therefore no further characterisation work was carried out. In addition a number of discrete unknown degradates were observed, none exceeding 4.5% AR. 14CO2 accounted for 0.4% AR at 59 DAT. Apparatus wash accounted for 4.5% AR.
- Evaporation of parent compound:
- not specified
- Volatile metabolites:
- yes
- Residues:
- yes
- Details on results:
- An overview of the results is provided in Table 6 – Table 11 in 'Any other information on results incl. tables'.
- Treatment Rate: Separate treatment solutions were prepared for low and high rate test systems. Each low rate sample received 0.2 µCi, (0.008 MBq) at a specific activity 210.8 µCi/mg, equivalent to 1.0 µg per sample. Each high rate sample received 1.3 µCi (0.05 MBq), equivalent to 6.4 µg per sample.
- Radiochemical Purity: The radiochemical purity of the [14C]-labelled test substance in the treatment solutions was determined by HPLC and TLC immediately prior to application and was > 95.1%.
- Volatile degradation products: Radioactivity recovered as evolved 14CO2 throughout the study was low. Small amounts of radioactivity were evolved as volatile products throughout the course of the study. The mean 14CO2 evolved at end of study at low rate dose group, high rate dose group, Sterile Low Rate and Sterile High Rate was 10.8%, 1.2%, 0.3% and 0.4%, respectively.
- Origin Bound Material: The majority of the origin bound material was confirmed as M4 (8.7 - 12.0% AR). Two minor components were detected and neither accounted for greater than 0.6% AR.
- Apparatus Wash: High Rate apparatus washes containing > 5% AR were analysed using HPLC Method 1. In the 3 h high rate replicate A apparatus wash sample (12.5% AR), the test substance accounted for 9.9% AR. A component which co-chromatographed with M13 was detected and accounted for 2.1% AR. At 30 DAT in the high rate replicate A apparatus wash sample (11.2% AR), the test substance accounted for 1.3% AR. A component which co-chromatographed with M4 was detected and accounted for 1.5% AR. At 30 DAT in the high rate replicate B apparatus wash sample (8.4% AR), the test substance accounted for 2.2% AR. A component which co-chromatographed with M4 was detected and accounted for 1.6% AR. At 60 DAT the high rate replicate A apparatus wash sample (6.1% AR), the test substance accounted for 1.5% AR. A component which co-chromatographed with M4 was detected and accounted for 0.7% AR. At 60 DAT the high rate replicate B apparatus wash sample (6.9% AR), the test substance accounted for 1.7% AR. A component which co-chromatographed with M4 was detected and accounted for 0.4% AR. A number of discrete unknown degradates were also observed in the 30 and 60 DAT samples, none of which accounted for greater than 1.8% AR.
- Confirmation of known degradates: Structural assignment for unchanged test substance, M18, M13 and M4 was by co-chromatography using HPLC method 2
- DegT50 and DegT90 of the test substance in Surface Water Systems: The degradation rate (DegT50 and DegT90) of the test substance in the test system was determined using non-linear regression and a single first order kinetic model (SFO). SFO kinetics describes the degradation of the test substance well with a Chi-square (χ2) error value of less than or equal to 10.7%. The degradation (DegT50) of the test substance in surface water was 0.4 and 6 days for the low and high rate incubations, respectively.
- Proposed Degradation Pathway: Degradation of the test substance involved:
> Oxidative dechlorination.
> Conversion of the nitrile group to an amide
> Cysteine/glutathione conjugation and further metabolism and ring closure - Results with reference substance:
- Reference and solvent controls showed that the degradation of [14C]-sodium benzoate to [14C]-carbon dioxide during the low rate experiment (maximum CO2 of 84.5% and 81.1% AR at 65 DAT in reference and solvent controls, respectively) indicated a viable microbial population was established. Reference and solvents controls for the high rate showed a maximum of 25.8% and 101.8% AR as CO2 at 59 DAT, respectively, however there was inefficient trapping of CO2 in some of control samples resulting in low mass balance. Despite the low mass balance the data demonstrated that the water had a viable microbial population and was suitable for use in the experiment.
- Validity criteria fulfilled:
- yes
- Conclusions:
- The DT50 values were calculated to be 0.4 and 6 days for the low and high rate incubations, respectively. M4 and M13 were the major degradation products detected in the low rate samples, reaching mean maximums of 79.9% AR (29 DAT) and 6.3% AR (60 DAT), respectively. M4, M13 and M18 were the major degradation products detected in the high rate samples, reaching mean maximums of 12.2% AR (5 DAT), 13.9% AR (60 DAT) and 32.1% AR (60 DAT), respectively. For the sterilised samples, the test substance degraded slower than in non-sterile samples with 3.3% and 22.4% AR remaining at 65 and 59 DAT for low and high rates, respectively.
- Executive summary:
The extent of mineralisation rate and the rate and route of degradation of [14C]-labelled test substance was investigated in surface water at ca 20 ± 2°C. The study was conducted in according to OECD TG 309 and in compliance with GLP criteria. [14C]-labelled test substance was applied to the water at nominal rates of 10 and 50 µg/L (low and high, respectively). The systems were incubated under aerobic conditions and maintained in the dark at ca 20°C for 60 days. Volatile radioactivity was continuously flushed from the vessels and collected in traps. For each test system, duplicate samples were taken for analysis at 8 intervals. Sterilised test systems were also treated with the test substance at the low and high application rates. For the low rate one set of duplicate samples were taken for analysis at 65 days. For the high rate one set of duplicate samples were taken for analysis at 59 days. At each sampling time, the quantity of radioactivity in the water was determined by liquid scintillation counting (LSC). A mass balance was determined for each sample. Separate reference control samples (treated with [14C]-sodium benzoate at 10 µg/L) of surface water were prepared and incubated alongside the test samples to determine whether a viable microbial population was present in the test system. Blank control samples were similarly incubated to allow water quality measurements at each sampling interval.
The mean mass balance for the low and high test concentration surface water samples was 95.7% applied radioactivity (AR) with ranges of 92.7% to 99.5% AR and 86.8% to 102.0% AR, respectively. For the high test concentration, four samples had a mass balance < 90% (range 86.1% to 88.2% AR). This was deemed to have no effect on the overall outcomes of the study and the loss was postulated to be a result of adsorption of test item and/or related components to apparatus. The mass balances for the sterilised incubation groups were 92.8% and 94.1% AR for the low and high rate samples, respectively. A single sample in the high rate samples had a mass balance 76.7% AR which was postulated to be the result of a treatment error and was excluded from calculations. t the low rate, the degradation of the test substance was rapid with mean levels decreasing from 67.4% AR at 0 DAT (days after treatment) to 4.7% AR at 2 DAT, with no test substance detected from 5 DAT onwards. The major degradate of the test substance was found to be M4 which reached a maximum of 79.9% AR in low rate samples at 29 DAT, decreasing to 71.9% AR at 60 DAT. M13 was detected and reached a maximum level of 6.3% AR at 60 DAT. For the low rate, 14CO2 contributed 10.8% AR at 60 DAT. At the high rate, degradation was slower with the test substance accounting for 91.5% at 0 DAT and decreased to 1.6% AR at 60 DAT. M4 reached a maximum of 12.2% AR at 5 DAT and decreased to 7.2% AR at 60 DAT. M13 was detected and reached a maximum level of 13.9% AR at 60 DAT in high rate samples. M18 increased from 3.9% AR at 5 DAT to 32.1% AR at 60 DAT. For the high rate, 14CO2 contributed 1.2% AR at 60 DAT. In addition a number of discrete unknown degradates were observed, none exceeding 5.7% AR at a single timepoint. For the low rate sterilised samples, the mean level of parent compound was 3.3% AR at 65 DAT. M4 and M13 accounted for 76.4% AR and 1.1% AR in the sterile samples, respectively. A mean of 2.4% AR was recovered as unassigned products with 7.7% AR remaining origin bound on the TLC, which was determined to be mainly M4. 14CO2 accounted for 0.3% AR at 65 DAT. Apparatus wash accounted for 1.5% AR. For the high rate sterilised samples, the mean level of parent compound was 22.4% AR 59 DAT. The metabolites M4 and M13 accounted for 8.9% AR and 3.4% AR in the sterile samples, respectively at 59 DAT. Three components were detected at greater than 5% AR (up to11.9% AR) which were not detected in low rate samples, therefore no further work was carried out. In addition a number of discrete unknown degradates were observed, none exceeding 4.5% AR. 14CO2 accounted for 0.4% AR at 59 DAT. Apparatus wash accounted for 4.5% AR. Reference and solvent controls showed that the degradation of [14C]-sodium benzoate to [14C]-carbon dioxide during the low rate experiment (maximum CO2 of 84.5% and 81.1% AR at 65 DAT in reference and solvent controls, respectively) indicated a viable microbial population was established. Reference and solvents controls for the high rate showed a maximum of 25.8% and 101.8% AR as CO2 at 59 DAT, respectively. The mass balance for the reference controls was low, however, it is postulated that there was incomplete capture of CO2 throughout the incubation period. The degradation (DegT50) of the test substance in surface water was 0.4 and 6 days for the low and high rate incubations, respectively.
Referenceopen allclose all
Table 4. Recovery of Radioactivity (14C-labelled test substance Equivalents)
a. Emperor Lake Sediment-Water Systems
|
% applied radioactivity |
||||||||||
0 HAT |
2 HAT |
4 HAT |
6 HAT |
1 DAT |
3 DAT |
7 DAT |
14 DAT |
43 DAT |
76 DAT |
100 DAT |
|
Sediment vessel |
1 |
3 |
5 |
7 |
9 |
11 |
13 |
15 |
17 |
21 |
23 |
Surface water |
92 |
92.8 |
95.7 |
90.9 |
91.1 |
88.8 |
74.6 |
60.1 |
42 |
12.9 |
13 |
Acetonitrile extract |
2.9 |
0.8 |
0.9 |
3.9 |
3.7 |
3.3 |
8.3 |
10.2 |
15.3 |
14.8 |
13.9 |
Vessel glasswash |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.1 |
1 |
2 |
0.1 |
1 |
0.1 |
CO2(analysis day) |
n.d |
n.d |
n.d |
n.d |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.1 |
0.1 |
CO2(cumulative) |
n.d |
n.d |
n.d |
n.d |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.2 |
0.3 |
Unextracted activity |
1.5 |
1.3 |
0.8 |
2.7 |
2.8 |
3.2 |
9.8 |
22.3 |
32.9 |
63.1 |
68.9 |
Total recovery |
96.4 |
94.9 |
97.4 |
97.5 |
97.6 |
95.4 |
93.7 |
94.6 |
90.3 |
92.1 |
96.3 |
b. Bury Pond Sediment-Water Systems
|
% applied radioactivity |
||||||||||||
0 HAT |
2 HAT |
4 HAT |
6 HAT |
11 HAT |
1 DAT |
3 DAT |
7 DAT |
7 DAT |
14 DAT |
47 DAT |
75 DAT |
103 DAT |
|
Sediment vessel |
43 |
45 |
47 |
49 |
51 |
53 |
55 |
57 |
58 |
59 |
61 |
63 |
65 |
Surface water |
97.2 |
96.3 |
93.4 |
95.9 |
94.3 |
91.3 |
78 |
78.7 |
67.3 |
38.9 |
15.7 |
8.7 |
10.7 |
Acetonitrile extract |
0.9 |
1.5 |
1.9 |
1.4 |
1.7 |
2.1 |
6.1 |
12.6 |
13.4 |
17.3 |
18.8 |
12.9 |
12.5 |
Vessel glasswash |
0.1 |
0.1 |
0.1 |
0.1 |
0.6 |
0.2 |
0.6 |
0.4 |
0.0 |
0.0 |
0.0 |
0.3 |
0.1 |
CO2(analysis day) |
n.d |
n.d |
n.d |
n.d |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.1 |
0.1 |
0.2 |
CO2(cumulative) |
n.d |
n.d |
n.d |
n.d |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.0 |
0.1 |
0.2 |
0.4 |
Unextracted activity |
1.2 |
2.7 |
4.0 |
2.2 |
4.0 |
5.6 |
12.5 |
14.1 |
3.5 |
38.4 |
65.3 |
101.6 |
67.2 |
Total recovery |
99.4 |
100.6 |
99.4 |
99.6 |
100.6 |
99.2 |
97.2 |
105.8 |
84.2 |
94.6 |
100 |
123.8 |
91.1 |
n.d - not done
HAT- hours after treatment
DAT-days after treatment
Table 5. Quantification of the test substance Remaining in the water-sediment system By TLC
a. Emperor Lake Aquatic Sediment Systems
Solvent system 51 |
Solvent system 49 |
Average |
||
0 HAT |
Surface water |
87.6 |
88.5 |
88.1 |
Total System |
87.6 |
88.5 |
88.1 |
|
2 HAT |
Surface water |
88.4 |
88.4 |
88.4 |
Total System |
88.4 |
88.4 |
88.4 |
|
4 HAT |
Surface water |
88.2 |
88.4 |
88.3 |
Total System |
88.2 |
88.4 |
88.3 |
|
6 HAT |
Surface water |
80.2 |
82.5 |
81.4 |
Total System |
80.2 |
82.5 |
81.4 |
|
11 HAT |
Surface water |
77.3 |
82.4 |
79.9 |
Total System |
77.3 |
82.4 |
79.9 |
|
1 DAT |
Surface water |
68.4 |
71.8 |
70.1 |
Total System |
68.4 |
71.8 |
70.1 |
|
3 DAT |
Surface water |
39.0 |
40.9 |
40.0 |
Total System |
39.0 |
40.9 |
40.0 |
|
7 DAT |
Surface water |
8.0 |
11.5 |
9.8 |
Total System |
8.0 |
11.5 |
9.8 |
|
14 DAT |
Surface water |
1.0 |
1.7 |
1.4 |
Total System |
1.0 |
1.7 |
1.4 |
|
43 DAT |
Surface water |
0.0 |
0.0 |
0.0 |
Total System |
0.0 |
0.0 |
0.0 |
b. Bury Pond Aquatic Sediment Systems
|
|
Solvent system 51 |
Solvent system 49 |
Average |
0 HAT |
Surface water |
90.2 |
90.4 |
90.3 |
Total System |
90.2 |
90.4 |
90.3 |
|
2 HAT |
Surface water |
82.0 |
85.7 |
83.9 |
Total System |
82.0 |
85.7 |
83.9 |
|
4 HAT |
Surface water |
61.1 |
65.2 |
63.2 |
Total System |
61.1 |
65.2 |
63.2 |
|
6 HAT |
Surface water |
79.0 |
83.0 |
81.0 |
Total System |
79.0 |
83.0 |
81.0 |
|
11 HAT |
Surface water |
49.7 |
52.9 |
51.3 |
Total System |
49.7 |
52.9 |
51.3 |
|
1 DAT |
Surface water |
43.2 |
42.8 |
43 |
Total System |
43.2 |
42.8 |
43 |
|
3 DAT |
Surface water |
4.8 |
5.4 |
5.1 |
Total System |
4.8 |
5.4 |
5.1 |
|
7 DAT 1st replicate |
Surface water |
3.5 |
2.4 |
3.0 |
Total System |
3.5 |
2.4 |
3.0 |
|
14 DAT |
Surface water |
0.7 |
0.6 |
0.7 |
Total System |
0.7 |
0.6 |
0.7 |
|
47 DAT |
Surface water |
0.0 |
0.0 |
0.0 |
Total System |
0.0 |
0.0 |
0.0 |
Table 6. Characterisation of the Radioactivity in the Emperor Lake Sediment and Water in TLC Solvent System 8B
Analysis Time |
1 DAT |
3 DAT |
7 DAT |
14 DAT |
43 DAT |
76 DAT |
100 DAT |
Surface Water |
% Applied |
||||||
Test substance |
68.5 |
40.1 |
8.6 |
0 |
0 |
0 |
0 |
Unknown A |
2.1 |
1.5 |
1.1 |
||||
M18 |
2.1 |
5.7 |
10.1 |
7.3 |
1.4 |
0.7 |
1 |
M4 & M24/Na |
4.4 |
3.3 |
4.2 |
2.5 |
0.8 |
0.5 |
0.4 |
M23 & M9 |
0.3 |
1.0 |
2.0 |
0.9 |
1.0 |
0.7 |
0.7 |
Baseline |
3.8 |
7.8 |
10.6 |
5.5 |
5.4 |
2.3 |
3.4 |
Remainder |
9.7 |
16.7 |
24.6 |
23.8 |
10.3 |
7.6 |
7.5 |
Surface Water total |
88.8 |
74.6 |
60.1 |
42.1 |
20.4 |
12.9 |
13 |
Sediment extract |
% Applied |
||||||
Unknown A |
0.5 |
1.2 |
2.2 |
1.8 |
1.2 |
||
M18 |
1 |
1.4 |
1.7 |
0.9 |
0.6 |
0.7 |
|
M4 & M24/Na |
1.0 |
0.9 |
0.9 |
0.6 |
0.7 |
0.6 |
|
M23 & M9 |
0.2 |
0.2 |
0.3 |
0.5 |
0.6 |
0.5 |
|
Baseline |
0.3 |
0.6 |
0.6 |
0.3 |
1.0 |
0.7 |
|
Remainder |
3.3 |
5.5 |
7 |
10.3 |
10.4 |
10 |
10.1 |
Loss on concentration |
0.2 |
0.3 |
|||||
Sediment extract total |
3.3 |
8.2 |
10.6 |
15.3 |
14.9 |
14.7 |
13.8 |
Extracts from 3 DAT to 14 DAT were concentrated. The 7 DAT extract increased by 0.5% on concentration, which is already included in the total recovery .
Baseline: radioactivity remaining at or close to the origin of the TLC plate
DAT - days after treatment
Remainder consists of streaking (non-discrete activity) or minor unknowns as below (The remainder for the 1 DAT extract was quantified by LSC only):
Analysis time |
Surface water |
Sediment extract |
||
Minimum number of unknowns |
No single Component |
Minimum number |
No single Component |
|
1 DAT |
2 |
3.1 |
(fraction not analysed) |
3.3 |
3 DAT |
2 |
6.5 |
3 |
2.1 |
7 DAT |
3 |
6.3 |
3 |
1.8 |
14 DAT |
2 |
4.7 |
3 |
3.7 |
43 DAT |
3 |
2.1 |
3 |
2.8 |
76 DAT |
3 |
1.9 |
3 |
2.4 |
100 DAT |
2 |
1.7 |
2 |
3.6 |
Table 7. Characterisation of the Radioactivity in the Emperor Lake total system in Solvent System 8B
Analysis Time |
1 DAT |
3 DAT |
7 DAT |
14 DAT |
43 DAT |
76 DAT |
100 DAT |
Surface Water |
% Applied |
||||||
Test substance |
68.5 |
40.1 |
8.6 |
0.0 |
0.0 |
0.0 |
0.0 |
Unknown A |
|
|
|
0.5 |
3.7 |
2.9 |
1.2 |
M18 |
2.1 |
6.7 |
11.5 |
9 |
2.3 |
1.3 |
1.7 |
M4 & M24/Na |
4.4 |
4.3 |
5.1 |
3.4 |
1.4 |
1.2 |
1.00 |
M23 & M9 |
0.3 |
1.2 |
2.2 |
1.2 |
1.5 |
1.3 |
1.2 |
Baseline |
3.8 |
8.1 |
11.2 |
6.1 |
5.7 |
3.3 |
4.1 |
Remainder |
9.7 |
22.2 |
31.6 |
34.1 |
20.7 |
17.6 |
17.6 |
Unanalysed fraction |
3.3 |
|
|
|
|
|
|
Loss on concentration |
|
0.2 |
* |
0.3 |
|
|
|
Vessel-glasswash |
0.1 |
1 |
2 |
0.1 |
0.2 |
1 |
0.1 |
14CO2 from analysis day |
0 |
0,0 |
0 |
0 |
0.1 |
0.1 |
0.1 |
14CO2 (Cumulative) |
0 |
0.0 |
0 |
0 |
0.1 |
0.2 |
0.3 |
Unextracted |
3.2 |
9.8 |
22.3 |
32.9 |
60.4 |
63.1 |
68.9 |
Total recovery |
95.4 |
93.6 |
95 |
90.4 |
96.1 |
92.0 |
96.2 |
*7 DAT extract increased by 0.5% of applied on concentration, which is already included in the total recovery
DAT: Days after treatment
Remainder consists of streaking (non-discrete activity) or minor unknowns as below:
Analysis time |
Surface water amd sediment extract |
|
Minimum number of unknowns |
No single Component |
|
1 DAT |
2 |
3.1 |
3 DAT |
5 |
6.5 |
7 DAT |
6 |
6.3 |
14 DAT |
6 |
4.7 |
43 DAT |
6 |
2.8 |
76 DAT |
6 |
2.4 |
100 DAT |
4 |
3.6 |
Table 8 . Characterisation of the Radioactivity in the Bury Pond Sediment and Water
Analysis Time |
7 DAT |
14 DAT |
47 DAT |
Surface Water |
% Applied |
||
Test substance |
0.0 |
0.0 |
0.0 |
Unknown A |
0.0 |
0.0 |
1.2 |
M18 |
8.9 |
2.2 |
0.6 |
M4 & M24/Na |
4.8 |
0.4 |
0.9 |
M23 & M9 |
1.9 |
0.8 |
0.3 |
Baseline |
21.2 |
21.8 |
5.6 |
Remainder |
30.5 |
13.7 |
7.1 |
Surface Water total |
67.3 |
38.9 |
15.7 |
Sediment extract |
% Applied |
||
Unknown A |
0.0 |
1.3 |
2.6 |
M18 |
1.4 |
1.5 |
1.4 |
M4 & M24/Na |
1.4 |
0.4 |
1.4 |
M23 & M9 |
0.3 |
0.3 |
0.4 |
Baseline |
0.2 |
2.7 |
0.5 |
Remainder |
10.1 |
10.6 |
12.6 |
Sediment extract total |
13.4 |
16.8 |
18.9 |
Base line: radioactivity remaining at or close to the origin of the TLC plate
DAT - days after treatment
Remainder consists of streaking (non-discrete activity) or minor unknowns as below:
Analysis time |
Surface water |
Sediment extract |
||
Minimum number of unknowns |
No single Component |
Minimum number |
No single Component |
|
7 DAT |
3 |
4.5 |
3 |
3.1 |
14 DAT |
4 |
3.8 |
2 |
2.3 |
47 DAT |
2 |
2.2 |
3 |
3.1 |
Table 9. Characterisation of Radioactivity In the Bury Pond Total System in Solvent System 8B
Analysis Time |
7 DAT |
14 DAT |
47 DAT |
% Applied |
|||
Test substance |
0.0 |
0.0 |
0.0 |
Unknown A |
0.0 |
1.3 |
3.8 |
M18 |
10.3 |
3.7 |
2.0 |
M4 & M24/Na |
6.2 |
0.8 |
2.3 |
M23 & M9 |
2.2 |
1.1 |
0.7 |
Baseline |
21.4 |
21.8 |
6.1 |
Remainder |
40.6 |
27.1 |
19.7 |
Unanalysed fraction |
0 |
0.4 |
0 |
Loss on concentration |
0 |
0 |
0 |
Vessel-glasswash |
0.0 |
0 |
0 |
14CO2 from analysis day |
0 |
0 |
0.1 |
14CO2 (Cumulative) |
0 |
0 |
0.1 |
Unextracted |
3.5 |
38.4 |
65.3 |
Total recovery |
84.2 |
94.6 |
100.1 |
Base line: radioactivity remaining at or close to the origin of the TLC plate
Remainder consists of streaking (non-discrete activity) or minor unknowns as below:
Analysis time |
Surface water amd sediment extract |
|
Minimum number of unknowns |
No single Component |
|
7 DAT |
6 |
4.5 |
14 DAT |
6 |
3.8 |
47 DAT |
5 |
3.1 |
Table 10. T1/2 Values for the Surface Water Alone and Combined Sediment and Water Phases Using the SFO Model
Sediment |
Emperor Lake |
Bury Pond |
||
Compartment |
Surface Water |
Total System |
Surface Water |
Total System |
T1/2 (hours) |
59.4 |
59.4 |
20.1 |
20.1 |
DT90 (hours) |
197.3 |
197.4 |
66.7 |
66.7 |
R2 |
0.9982 |
0.9982 |
0.9744 |
0.9744 |
Table 6. Radiochemical Purity Results
Time Point/Event |
Radiochemical Purity (%) |
|||
Pre-dose |
Post-dose |
|||
HPLC |
TLC |
HPLC |
TLC |
|
Swiss Lake Treatment Solution |
97.4 |
98.1 |
96.0 |
99.0 |
Calwich Abbey Treatment Solution |
97.9 |
99.8 |
98.1 |
98.1 |
Table 7. Distribution and Recovery of Radioactivity: Swiss Lake (Aerobic Incubation)
Fraction |
Rep. |
% AR in Sample at Timepoint (DAT) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
15 |
29 |
48 |
61 |
102 |
||
Surface Water |
A |
79.2 |
84.2 |
74.9 |
79.4 |
86.7 |
72.5 |
64.9 |
28.1 |
33.2 |
18.0 |
29.4 |
B |
86.7 |
82.7 |
86.2 |
74.6 |
86.2 |
50.5 |
66.7 |
50.6 |
35.9 |
38.5 |
24.8 |
|
Mean |
83.0 |
83.5 |
80.6 |
77.0 |
86.5 |
61.5 |
65.8 |
39.4 |
34.6 |
28.3 |
27.1 |
|
Sediment Extract 1(a) |
A |
13.0 |
8.6 |
12.0 |
8.8 |
3.7 |
8.9 |
10.7 |
24.4 |
23.4 |
26.6 |
26.0 |
B |
5.8 |
10.3 |
10.2 |
13.9 |
5.6 |
16.6 |
9.3 |
18.5 |
20.5 |
21.2 |
24.7 |
|
Mean |
9.4 |
9.5 |
11.1 |
11.4 |
4.7 |
12.8 |
10.0 |
21.5 |
22.0 |
23.9 |
25.4 |
|
Sediment Extract 2(b) |
A |
1.1 |
1.2 |
2.1 |
1.7 |
0.9 |
2.9 |
3.8 |
10.0 |
9.0 |
14.1 |
9.6 |
B |
0.8 |
1.3 |
1.6 |
1.9 |
1.0 |
6.5 |
3.5 |
6.3 |
7.8 |
8.0 |
12.2 |
|
Mean |
1.0 |
1.3 |
1.9 |
1.8 |
1.0 |
4.7 |
3.7 |
8.2 |
8.4 |
11.1 |
10.9 |
|
Total Extractable |
Mean |
93.4 |
94.3 |
93.6 |
90.2 |
92.2 |
79.0 |
79.5 |
69.3 |
65.0 |
63.3 |
63.4 |
Non-Extractables(c) |
A |
1.7 |
2.2 |
5.3 |
4.1 |
1.6 |
10.0 |
11.0 |
22.0 |
24.5 |
30.0 |
29.2 |
B |
2.0 |
1.9 |
2.2 |
4.0 |
1.5 |
15.6 |
10.7 |
18.0 |
21.9 |
23.4 |
30.0 |
|
Mean |
1.9 |
2.1 |
3.8 |
4.1 |
1.6 |
12.8 |
10.9 |
20.0 |
23.2 |
26.7 |
29.6 |
|
14CO2 |
A |
NA |
<LOQ |
<0.1 |
<LOQ |
<LOQ |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.2 |
B |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
0.1 |
<0.1 |
<0.1 |
0.1 |
0.3 |
|
Mean |
- |
- |
- |
- |
- |
- |
0.1 |
- |
- |
0.1 |
0.3 |
|
TOTAL |
A |
95.0 |
96.2 |
94.3 |
94.0 |
92.9 |
94.3 |
90.4 |
84.9 |
90.1 |
88.7 |
94.4 |
B |
95.3 |
96.2 |
100.2 |
94.4 |
94.3 |
89.2 |
90.3 |
93.4 |
86.1 |
91.2 |
92.0 |
|
Mean |
95.2 |
96.2 |
97.3 |
94.2 |
93.6 |
91.8 |
90.4 |
89.2 |
88.1 |
90.0 |
93.2 |
|
Mean ± SD |
|
92.6 ± 3.5 |
||||||||||
(a) Acetonitrile:0.3M HCl (8:2, v/v) x 2 extractions
(b) Acetonitrile:1.5M HCl (8:2, v/v) x 2 extractions
(c) Further investigated at 102 DAT using reflux and organic matter fractionation
NA: Not applicable
<LOQ: Below Limit of Quantification
Table 8. Distribution and Recovery of Radioactivity: Calwich Abbey (Aerobic Incubation)
Fraction |
Rep. |
% AR in Sample at Timepoint (DAT) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
||
Surface Water |
A |
86.6 |
92.0 |
89.1 |
85.4 |
84.3 |
69.5 |
62.0 |
39.8 |
33.4 |
19.7 |
10.2 |
B |
87.1 |
94.8 |
86.1 |
83.6 |
84.5 |
70.8 |
54.8 |
41.2 |
24.6 |
25.1 |
13.8 |
|
Mean |
86.9 |
93.4 |
87.6 |
84.5 |
84.4 |
70.2 |
58.4 |
40.5 |
29.0 |
22.4 |
12.0 |
|
Sediment Extract 1(a) |
A |
10.1 |
4.4 |
5.5 |
11.1 |
12.8 |
16.6 |
19.4 |
23.5 |
22.3 |
19.9 |
15.3 |
B |
10.6 |
2.4 |
6.9 |
9.2 |
9.0 |
16.4 |
22.8 |
19.9 |
22.7 |
18.8 |
14.3 |
|
Mean |
10.4 |
3.4 |
6.2 |
10.2 |
10.9 |
16.5 |
21.1 |
21.7 |
22.5 |
19.4 |
14.8 |
|
Sediment Extract 2(b) |
A |
0.8 |
0.3 |
0.4 |
0.9 |
1.2 |
1.5 |
1.9 |
2.5 |
2.6 |
3.9 |
4.1 |
B |
0.8 |
0.2 |
0.4 |
0.8 |
0.8 |
1.4 |
2.2 |
2.4 |
3.6 |
3.4 |
3.7 |
|
Mean |
0.8 |
0.3 |
0.4 |
0.9 |
1.0 |
1.5 |
2.1 |
2.5 |
3.1 |
3.7 |
3.9 |
|
Total Extractable |
Mean |
98.1 |
97.1 |
94.2 |
95.6 |
95.6 |
88.3 |
81.6 |
64.7 |
54.6 |
45.5 |
30.7 |
Non-Extractables(c) |
A |
1.0 |
1.1 |
1.1 |
2.3 |
3.8 |
8.4 |
13.3 |
30.2 |
37.7 |
45.8 |
64.6 |
B |
2.3 |
0.5 |
2.6 |
2.8 |
3.5 |
8.8 |
17.7 |
32.0 |
43.5 |
49.4 |
65.7 |
|
Mean |
1.7 |
0.8 |
1.9 |
2.6 |
3.7 |
8.6 |
15.5 |
31.1 |
40.6 |
47.6 |
65.2 |
|
14CO2 |
A |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Mean |
- |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
TOTAL |
A |
98.5 |
97.8 |
96.1 |
99.7 |
102.1 |
96.0 |
96.6 |
96.0 |
96.0 |
89.3 |
94.2 |
B |
100.8 |
97.9 |
96.0 |
96.4 |
97.8 |
97.4 |
97.5 |
95.5 |
94.4 |
96.7 |
97.5 |
|
Mean |
99.7 |
97.9 |
96.1 |
98.1 |
100.0 |
96.7 |
97.1 |
95.8 |
95.2 |
93.0 |
95.9 |
|
Mean ± SD |
|
96.8 ± 2.5 |
||||||||||
(a) Acetonitrile:0.3M HCl (8:2, v/v) x 2 extractions
(b) Acetonitrile:1.5M HCl (8:2, v/v) x 2 extractions
(c) Further investigated at 102 DAT using reflux and organic matter fractionation
NA: Not applicable
<LOQ: Below Limit of Quantification
Table 9. Summary of Characterisation / Identification of Radioactive Residues in Aerobic Swiss Lake Water-Sediment System
(a) Radioactive residue in the total system:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 (b) |
15 |
29 |
48 |
61 |
102 |
||
A |
89.2 |
90 |
82.1 |
79.5 |
77 |
55.3 |
22 |
0.8 |
ND |
ND |
ND |
|
Substance |
B |
90 |
89.9 |
90.2 |
82.4 |
82.2 |
10.3 |
40.3 |
3.1 |
ND |
ND |
ND |
Mean |
89.6 |
90 |
85.9 |
81 |
79.6 |
55.3 |
31.2 |
2 |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.7 |
1.9 |
1.6 |
1.8 |
1.5 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.9 |
0.8 |
ND |
1 |
|
Mean |
- |
- |
- |
- |
- |
- |
0.4 |
1.4 |
1.2 |
0.6 |
1.3 |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
1.1 |
2.5 |
2.7 |
1.5 |
1.3 |
2 |
B |
ND |
ND |
ND |
ND |
ND |
1.5 |
1.9 |
2.9 |
2 |
2.7 |
ND |
|
Mean |
- |
- |
- |
- |
- |
1.1 |
2.2 |
2.8 |
1.8 |
2 |
1 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
1.4 |
1.7 |
0.6 |
2.3 |
0.6 |
1.5 |
B |
ND |
ND |
ND |
ND |
ND |
3.9 |
3.3 |
1.9 |
1.3 |
1.8 |
ND |
|
Mean |
- |
- |
- |
- |
- |
1.4 |
2.5 |
1.3 |
1.8 |
1.2 |
0.8 |
|
M18 |
A |
ND |
ND |
ND |
ND |
0.4 |
8.7 |
19.6 |
26.1 |
25.3 |
16.7 |
16.5 |
B |
ND |
ND |
ND |
ND |
ND |
11.7 |
9.4 |
26.3 |
23.8 |
21.4 |
11 |
|
Mean |
- |
- |
- |
- |
0.2 |
8.7 |
14.5 |
26.2 |
24.6 |
19.1 |
13.8 |
|
M19 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.7 |
0.9 |
ND |
1.4 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
3.9 |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
ND |
0.4 |
0.5 |
- |
0.7 |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
0.8 |
9.9 |
3.6 |
5.4 |
9.9 |
5.1 |
2.7 |
B |
ND |
ND |
ND |
ND |
ND |
22.4 |
7.6 |
17.3 |
7.2 |
6.5 |
6.5 |
|
Mean |
- |
- |
- |
- |
0.4 |
9.9 |
5.6 |
11.4 |
8.6 |
5.8 |
4.6 |
|
Unknown 38 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
4.8 |
6.8 |
3.4 |
ND |
1.7 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
1.6 |
6.5 |
6.3 |
ND |
1.8 |
|
Mean |
- |
- |
- |
- |
- |
- |
3.2 |
6.7 |
4.9 |
- |
1.8 |
|
Unknown 40 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.8 |
2.8 |
11.2 |
6 |
23.2 |
B |
ND |
ND |
ND |
ND |
ND |
1.6 |
0.7 |
3.8 |
5.5 |
14.6 |
26.6 |
|
Mean |
- |
- |
- |
- |
- |
ND |
0.8 |
3.3 |
8.4 |
10.3 |
24.9 |
|
Unknown 44 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
0.9 |
ND |
11.2 |
3.6 |
4.3 |
5.5 |
B |
ND |
ND |
ND |
ND |
ND |
0.7 |
ND |
2.8 |
2.2 |
5.8 |
6.8 |
|
Mean |
- |
- |
- |
- |
- |
0.9 |
- |
7 |
2.9 |
5.1 |
6.2 |
|
Minor Unknowns (c) |
A |
0.6 |
0.3 |
0.2 |
0.5 |
ND |
9.7 |
8.7 |
4.1 |
5.6 |
20.6 |
10.5 |
B |
0.6 |
0.3 |
ND |
0.4 |
ND |
11.4 |
6.3 |
14 |
4 |
15 |
7.2 |
|
Mean |
0.6 |
0.3 |
0.1 |
0.5 |
- |
10.6 |
7.5 |
9.1 |
4.8 |
17.8 |
8.9 |
|
Unassigned Regions (d) |
A |
1.8 |
1.7 |
4.3 |
3.9 |
NA |
0.7 |
0.3 |
NA |
NA |
NA |
NA |
B |
1.4 |
1.9 |
4.9 |
3.5 |
NA |
0.8 |
0.7 |
NA |
NA |
NA |
NA |
|
Mean |
1.6 |
1.8 |
4.6 |
3.7 |
- |
0.8 |
0.5 |
- |
- |
- |
- |
|
Origin Bound |
A |
0.6 |
0.8 |
2.4 |
4.4 |
NA |
2 |
2.9 |
NA |
NA |
NA |
NA |
(e) |
B |
0.5 |
0.9 |
1.3 |
2.2 |
NA |
4.9 |
2.4 |
NA |
NA |
NA |
NA |
Mean |
0.6 |
0.9 |
1.9 |
3.3 |
- |
3.5 |
2.7 |
- |
- |
- |
- |
|
Carbon Dioxide |
A |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
0.2 |
B |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
0.1 |
<0.1 |
<0.1 |
0.1 |
0.3 |
|
Mean |
- |
- |
- |
- |
- |
- |
0.1 |
- |
- |
0.1 |
0.3 |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints.All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6 h samples.
(b) Day 7 Replicate B is a clear outlier and has been removed from any further calculations. The mean value for all Day 7 results does not contain the result from Replicate B.
(c) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(d) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(e) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(f) Minor shift in retention time observed throughout chromatography
<LOQ: Below Limit of Quantification
ND: Not Detected
NA: Not Applicable
(b) Radioactive residue in the water phase:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 (b) |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
78.6 |
83.3 |
72.6 |
73.8 |
75 |
54.3 |
21.1 |
ND |
ND |
ND |
ND |
B |
86.1 |
81.4 |
82.3 |
71.6 |
78.2 |
9 |
39.3 |
2.9 |
ND |
ND |
ND |
|
Mean |
82.4 |
82.4 |
77.5 |
72.7 |
76.6 |
54.3 |
30.2 |
1.5 |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.7 |
1.9 |
0.4 |
0.4 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.8 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
0.4 |
1 |
0.6 |
0.2 |
- |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
0.5 |
2.5 |
2.7 |
1.5 |
1.3 |
2 |
B |
ND |
ND |
ND |
ND |
ND |
1.5 |
1.9 |
2.9 |
2 |
2.7 |
ND |
|
Mean |
- |
- |
- |
- |
- |
0.5 |
2.2 |
2.8 |
1.8 |
2 |
1 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
1.4 |
1.7 |
0.6 |
1.1 |
0.6 |
1.5 |
B |
ND |
ND |
ND |
ND |
ND |
2.7 |
3.3 |
1.9 |
1.3 |
1.8 |
ND |
|
Mean |
- |
- |
- |
- |
- |
1.4 |
2.5 |
1.3 |
1.2 |
1.2 |
0.8 |
|
M18 |
A |
ND |
ND |
ND |
ND |
ND |
8.7 |
17.4 |
9.6 |
13.8 |
2.3 |
7.3 |
B |
ND |
ND |
ND |
ND |
ND |
8.3 |
9.4 |
21.7 |
16.4 |
16.1 |
2.5 |
|
Mean |
- |
- |
- |
- |
- |
8.7 |
13.4 |
15.7 |
15.1 |
9.2 |
4.9 |
|
M19 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.9 |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
3.9 |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
ND |
- |
0.5 |
- |
- |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
ND |
8.6 |
2.3 |
2.6 |
2.9 |
2 |
0.9 |
B |
ND |
ND |
ND |
ND |
ND |
17.1 |
7.6 |
7.6 |
2.9 |
3.7 |
3.9 |
|
Mean |
- |
- |
- |
- |
- |
8.6 |
5 |
5.1 |
2.9 |
2.9 |
2.4 |
|
Unknown 38 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
4.8 |
6.8 |
3.4 |
ND |
1.7 |
B |
ND |
ND |
ND |
ND |
ND |
1.6 |
1.6 |
6.5 |
6.3 |
ND |
1.5 |
|
Mean |
- |
- |
- |
- |
- |
ND |
3.2 |
6.7 |
4.9 |
- |
1.6 |
|
Unknown 40 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.8 |
0.5 |
4.1 |
1.8 |
8.1 |
B |
ND |
ND |
ND |
ND |
ND |
1.6 |
0.7 |
1.7 |
1 |
4.9 |
6 |
|
Mean |
- |
- |
- |
- |
- |
ND |
0.8 |
1.1 |
2.6 |
3.4 |
7.1 |
|
Unknown 44 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.7 |
3.8 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.7 |
3.4 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
2.7 |
3.6 |
|
Minor Unknowns (c) |
A |
ND |
ND |
ND |
ND |
ND |
6.5 |
4.9 |
2.5 |
4.8 |
7.3 |
4.1 |
B |
ND |
ND |
ND |
ND |
ND |
2.1 |
2.8 |
5.6 |
4 |
5.7 |
6.7 |
|
Mean |
- |
- |
- |
- |
- |
6.5 |
3.9 |
4.1 |
4.4 |
6.5 |
5.4 |
|
Unassigned Regions (d) |
A |
0.6 |
0.5 |
1.5 |
2.1 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
0.6 |
0.8 |
3 |
1.6 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.6 |
0.7 |
2.3 |
1.9 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (e) |
A |
ND |
0.4 |
0.8 |
3.6 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
0.5 |
0.9 |
1.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
- |
0.5 |
0.9 |
2.5 |
- |
- |
- |
- |
- |
- |
- |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6 h samples.
(b) Day 7 Replicate B is a clear outlier and has been removed from any further calculations. The mean value for all Day 7 results does not contain the result from Replicate B.
(c) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(d) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(e) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(f) Minor shift in retention time observed throughout chromatography
ND: Not Detected
NA: Not Applicable
(c) Radioactive residue in the sediment phase (Extract 1):
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 (b) |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
10.6 |
6.7 |
9 |
5.7 |
2 |
1 |
0.9 |
0.8 |
ND |
ND |
ND |
B |
3.9 |
8.5 |
7.9 |
10.8 |
4 |
1.3 |
1 |
0.2 |
ND |
ND |
ND |
|
Mean |
7.3 |
7.6 |
8.5 |
8.3 |
3 |
1 |
1 |
0.5 |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.2 |
1.4 |
1.5 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.9 |
ND |
ND |
1 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
0.5 |
0.6 |
0.7 |
1.3 |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
0.6 |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
0.6 |
- |
- |
- |
- |
- |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
1.2 |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
ND |
- |
- |
- |
- |
- |
|
M18 |
A |
ND |
ND |
ND |
ND |
0.4 |
ND |
2.2 |
16.5 |
8.3 |
12.1 |
4.6 |
B |
ND |
ND |
ND |
ND |
ND |
3.4 |
ND |
6.7 |
7.4 |
5.3 |
4.3 |
|
Mean |
- |
- |
- |
- |
0.2 |
ND |
1.1 |
11.6 |
7.9 |
8.7 |
4.5 |
|
M19 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
0.7 |
ND |
ND |
0.8 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
0.4 |
- |
- |
0.4 |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
0.8 |
1.3 |
1.3 |
2.8 |
3.2 |
3.1 |
1.8 |
B |
ND |
ND |
ND |
ND |
ND |
5.3 |
ND |
4.6 |
4.3 |
1.9 |
2.6 |
|
Mean |
- |
- |
- |
- |
0.4 |
1.3 |
0.7 |
3.7 |
3.8 |
2.5 |
2.2 |
|
Unknown 38 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.3 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
0.2 |
|
Unknown 40 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.3 |
7.1 |
4.2 |
15.1 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.1 |
4.5 |
9.7 |
12.6 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
2.2 |
5.8 |
7 |
13.9 |
|
Unknown 44 min (f) |
A |
ND |
ND |
ND |
ND |
ND |
0.9 |
ND |
2.8 |
3.6 |
2.6 |
1.7 |
B |
ND |
ND |
ND |
ND |
ND |
0.7 |
ND |
1.5 |
2.2 |
2.1 |
3.4 |
|
Mean |
- |
- |
- |
- |
- |
0.9 |
- |
2.2 |
2.9 |
2.4 |
2.6 |
|
Minor Unknowns (c) |
A |
0.6 |
0.3 |
ND |
0.5 |
ND |
2.9 |
3.2 |
ND |
ND |
2.5 |
1.4 |
B |
0.6 |
0.3 |
ND |
0.4 |
ND |
8.5 |
3.1 |
3.7 |
ND |
2.1 |
0.5 |
|
Mean |
0.6 |
0.3 |
- |
0.5 |
- |
2.9 |
3.2 |
1.9 |
- |
2.3 |
1 |
|
Unassigned Regions (d) |
A |
1.2 |
1.2 |
2.4 |
1.8 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
0.8 |
1.1 |
1.9 |
1.9 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
1 |
1.2 |
2.2 |
1.9 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (e) |
A |
0.6 |
0.4 |
0.6 |
0.8 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
0.5 |
0.4 |
0.4 |
0.8 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.6 |
0.4 |
0.5 |
0.8 |
- |
- |
- |
- |
- |
- |
- |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) Day 7 Replicate B is a clear outlier and has been removed from any further calculations. The mean value for all Day 7 results does not contain the result from Replicate B.
(c) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(d) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(e) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(f) Minor shift in retention time observed throughout chromatography
ND: Not Detected
NA: Not Applicable
(d) Radioactive residue in the sediment phase (Extract 2):
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 (b) |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
NA |
NA |
0.5 |
NA |
NA |
ND |
ND |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
0.3 |
- |
- |
- |
- |
- |
- |
- |
- |
|
M8 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M17 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M13 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
1.2 |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
0.6 |
- |
- |
|
M18 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
3.2 |
2.3 |
4.6 |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
4.2 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
1.6 |
1.2 |
4.4 |
|
M19 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
0.6 |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
0.3 |
- |
|
M4 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
3.8 |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
5.1 |
ND |
0.9 |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
2.6 |
1.9 |
0.5 |
- |
|
Unknown 38 min (f) |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Unknown 40 min (f) |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
8 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
4 |
|
Unknown 44 min (f) |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
8.4 |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
1.3 |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
4.9 |
- |
- |
- |
|
Minor Unknowns (c) |
A |
NA |
NA |
0.2 |
NA |
NA |
0.3 |
0.6 |
1.6 |
0.8 |
11.1 |
5 |
B |
NA |
NA |
NA |
NA |
NA |
0.8 |
0.4 |
4.7 |
7.8 |
7.2 |
ND |
|
Mean |
- |
- |
0.1 |
- |
- |
0.6 |
0.5 |
3.2 |
4.3 |
9.2 |
2.5 |
|
Unassigned Regions (d) |
A |
NA |
NA |
0.4 |
NA |
NA |
0.7 |
0.3 |
NA |
NA |
NA |
NA |
B |
NA |
NA |
NA |
NA |
NA |
0.8 |
0.7 |
NA |
NA |
NA |
NA |
|
Mean |
- |
- |
0.2 |
- |
- |
0.8 |
0.5 |
- |
- |
- |
- |
|
Origin Bound (e) |
A |
NA |
NA |
1 |
NA |
NA |
2 |
2.9 |
NA |
NA |
NA |
NA |
B |
NA |
NA |
NA |
NA |
NA |
4.9 |
2.4 |
NA |
NA |
NA |
NA |
|
Mean |
- |
- |
0.5 |
- |
- |
3.5 |
2.7 |
- |
- |
- |
- |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0 - 6h samples.
(b) Day 7 Replicate B is a clear outlier and has been removed from any further calculations. The mean value for all Day 7 results does not contain the result from Replicate B.
(c) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(d) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(e) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(f) Minor shift in retention time observed throughout chromatography
ND: Not Detected
NA: Not Applicable
Table 10. Summary of Characterisation / Identification of Radioactive Residues in Aerobic Calwich Abbey-Sediment System
(a) Radioactive residue in the total system:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 (b) |
15 |
29 |
48 |
61 |
102 |
||
Substance (a) |
A |
88.9 |
92.8 |
88.5 |
77.4 |
66.6 |
17.9 |
7.2 |
ND |
ND |
ND |
ND |
B |
90.3 |
94.8 |
84.8 |
79.3 |
68.1 |
33.3 |
ND |
ND |
ND |
ND |
ND |
|
Mean |
89.6 |
93.8 |
86.7 |
78.4 |
67.4 |
25.6 |
3.6 |
- |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
6.5 |
10.4 |
1.9 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
4.1 |
2.4 |
0.6 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
3.3 |
7.3 |
2.2 |
0.3 |
|
M17 |
A |
ND |
ND |
ND |
ND |
0.8 |
7.1 |
10.3 |
ND |
6.7 |
3.9 |
ND |
B |
ND |
ND |
ND |
ND |
3.4 |
ND |
13.1 |
5.3 |
5.8 |
8.6 |
1.4 |
|
Mean |
- |
- |
- |
- |
2.1 |
3.6 |
11.7 |
2.7 |
6.3 |
6.3 |
0.7 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.9 |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
1.5 |
- |
- |
- |
- |
|
M18 |
A |
ND |
ND |
ND |
ND |
8.3 |
6.7 |
31.3 |
17.2 |
9.7 |
12.7 |
4.8 |
B |
ND |
ND |
ND |
ND |
3.5 |
11.7 |
41.2 |
9 |
13.4 |
11.7 |
5 |
|
Mean |
- |
- |
- |
- |
5.9 |
9.2 |
36.3 |
13.1 |
11.6 |
12.2 |
4.9 |
|
M19 |
A |
ND |
ND |
ND |
ND |
7.1 |
6.7 |
7.4 |
8.7 |
1.7 |
1.6 |
ND |
B |
ND |
ND |
ND |
ND |
2.6 |
6.2 |
8.6 |
10.3 |
3 |
1.7 |
0.5 |
|
Mean |
- |
- |
- |
- |
4.9 |
6.5 |
8 |
9.5 |
2.4 |
1.7 |
0.3 |
|
M4 |
A |
ND |
ND |
ND |
ND |
45.2 |
47.7 |
11.2 |
11.3 |
13.8 |
8.4 |
7.7 |
B |
ND |
ND |
ND |
ND |
7.7 |
45.2 |
8.8 |
10.2 |
3.6 |
6.3 |
4.3 |
|
Mean |
- |
- |
- |
- |
26.5 |
46.5 |
10 |
10.8 |
8.7 |
7.4 |
6 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
1.2 |
1.9 |
5.4 |
4.7 |
ND |
2.7 |
0.8 |
B |
ND |
ND |
ND |
ND |
ND |
1.6 |
4.1 |
7.8 |
2.1 |
5.6 |
1.2 |
|
Mean |
- |
- |
- |
- |
0.6 |
1.8 |
4.8 |
6.3 |
1.1 |
4.2 |
1 |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.4 |
4.8 |
5.2 |
3.6 |
B |
ND |
ND |
ND |
ND |
ND |
0.9 |
ND |
ND |
2.9 |
4.3 |
6.8 |
|
Mean |
- |
- |
- |
- |
- |
0.5 |
- |
0.7 |
3.9 |
4.8 |
5.2 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.7 |
4.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.6 |
1.3 |
1.8 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
0.8 |
1.5 |
3.2 |
|
Minor Unknowns (b) |
A |
4.6 |
1.4 |
2 |
9.3 |
4.8 |
9.2 |
3.1 |
13.5 |
8.5 |
1.6 |
3.8 |
B |
4.8 |
0.7 |
2.4 |
4.8 |
ND |
6.6 |
1.9 |
18.4 |
10.7 |
2 |
6.5 |
|
Mean |
4.7 |
1.1 |
2.2 |
7.1 |
2.4 |
7.9 |
2.5 |
16 |
9.6 |
1.8 |
5.2 |
|
Unassigned Regions (c) |
A |
2.5 |
1 |
1.9 |
3.5 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
2.5 |
0.7 |
2.6 |
2.5 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
2.5 |
0.9 |
2.3 |
3 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.6 |
1.3 |
2.2 |
6.1 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
0.3 |
1.1 |
3.1 |
6.2 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.5 |
1.2 |
2.7 |
6.2 |
- |
- |
- |
- |
- |
- |
- |
|
Carbon Dioxide |
A |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
B |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
Mean |
- |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) Minor shift in retention time observed throughout chromatography
ND: Not Detected
NA: Not Applicable
(b) Radioactive residue in the water phase:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
||
Substance (a) |
A |
84.4 |
90.3 |
85.9 |
73.5 |
66.6 |
15.9 |
7.2 |
ND |
ND |
ND |
ND |
B |
85.3 |
93.4 |
81.4 |
73.9 |
68.1 |
31.2 |
ND |
ND |
ND |
ND |
ND |
|
Mean |
84.9 |
91.9 |
83.7 |
73.7 |
67.4 |
23.6 |
3.6 |
- |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
7.7 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.1 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
5.4 |
- |
- |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.9 |
ND |
2.3 |
2.1 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
2.6 |
1.1 |
2.4 |
5 |
1.4 |
|
Mean |
- |
- |
- |
- |
- |
- |
2.8 |
0.6 |
2.4 |
3.6 |
0.7 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.9 |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
1.5 |
- |
- |
- |
- |
|
M18 |
A |
ND |
ND |
ND |
ND |
1.2 |
2.7 |
29.8 |
12.4 |
6.5 |
7.9 |
0.5 |
B |
ND |
ND |
ND |
ND |
1.1 |
2.9 |
38.5 |
6.1 |
6.6 |
8.1 |
2.1 |
|
Mean |
- |
- |
- |
- |
1.2 |
2.8 |
34.2 |
9.3 |
6.6 |
8 |
1.3 |
|
M19 |
A |
ND |
ND |
ND |
ND |
3.6 |
2.6 |
ND |
5.5 |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
0.6 |
3.3 |
ND |
8.7 |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
2.1 |
3 |
- |
7.1 |
- |
- |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
43.9 |
46.2 |
9.7 |
5.9 |
6 |
3.5 |
2.8 |
B |
ND |
ND |
ND |
ND |
6.5 |
42.7 |
7.8 |
8.1 |
3.6 |
2.9 |
1.6 |
|
Mean |
- |
- |
- |
- |
25.2 |
44.5 |
8.8 |
7 |
4.8 |
3.2 |
2.2 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
1.2 |
1.9 |
5.4 |
4.6 |
ND |
2.7 |
0.8 |
B |
ND |
ND |
ND |
ND |
ND |
1.6 |
4.1 |
7.8 |
ND |
5.6 |
1.2 |
|
Mean |
- |
- |
- |
- |
0.6 |
1.8 |
4.8 |
6.2 |
- |
4.2 |
1 |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.3 |
2.7 |
0.9 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.9 |
2.2 |
3.3 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
2.6 |
2.5 |
2.1 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.6 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
0.8 |
- |
1 |
|
Minor Unknowns (b) |
A |
ND |
ND |
0.4 |
3.4 |
4.8 |
9.2 |
1.6 |
10.4 |
8.5 |
0.9 |
3.1 |
B |
ND |
ND |
0.6 |
2.8 |
ND |
5.2 |
1.9 |
9.4 |
4.3 |
1.3 |
4.1 |
|
Mean |
- |
- |
0.5 |
3.1 |
2.4 |
7.2 |
1.8 |
9.9 |
6.4 |
1.1 |
3.6 |
|
Unassigned Regions (c) |
A |
1.8 |
0.7 |
0.9 |
3.1 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
1.5 |
0.5 |
1.3 |
1.1 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
1.7 |
0.6 |
1.1 |
2.1 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.4 |
1 |
1.9 |
5.3 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
0.3 |
0.9 |
2.8 |
5.8 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.4 |
1 |
2.4 |
5.6 |
- |
- |
- |
- |
- |
- |
- |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) Minor shift in retention time observed throughout chromatography
ND: Not Detected
NA: Not Applicable
(c) Radioactive residue in the sediment phase (Extract 1):
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
||
Substance (a) |
A |
4.5 |
2.5 |
2.6 |
3.9 |
ND |
2 |
ND |
ND |
ND |
ND |
ND |
B |
5 |
1.4 |
3.4 |
5.4 |
ND |
2.1 |
ND |
ND |
ND |
ND |
ND |
|
Mean |
4.8 |
2 |
3 |
4.7 |
- |
2.1 |
- |
- |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
6.5 |
2.7 |
1.9 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1 |
2.4 |
0.6 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
3.3 |
1.9 |
2.2 |
0.3 |
|
M17 |
A |
ND |
ND |
ND |
ND |
0.8 |
7.1 |
7.4 |
ND |
4.4 |
1.8 |
ND |
B |
ND |
ND |
ND |
ND |
3.4 |
ND |
10.5 |
4.2 |
3.4 |
3.6 |
ND |
|
Mean |
- |
- |
- |
- |
2.1 |
3.6 |
9 |
2.1 |
3.9 |
2.7 |
- |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M18 |
A |
ND |
ND |
ND |
ND |
7.1 |
4 |
1.5 |
4.8 |
3.2 |
4.8 |
4.3 |
B |
ND |
ND |
ND |
ND |
2.4 |
8.8 |
2.7 |
2.9 |
6.8 |
3.6 |
2.9 |
|
Mean |
- |
- |
- |
- |
4.8 |
6.4 |
2.1 |
3.9 |
5 |
4.2 |
3.6 |
|
M19 |
A |
ND |
ND |
ND |
ND |
3.5 |
4.1 |
7.4 |
3.2 |
1.7 |
1.6 |
ND |
B |
ND |
ND |
ND |
ND |
2 |
2.9 |
8.6 |
1.6 |
3 |
1.7 |
0.5 |
|
Mean |
- |
- |
- |
- |
2.8 |
3.5 |
8 |
2.4 |
2.4 |
1.7 |
0.3 |
|
M4 |
A |
ND |
ND |
ND |
ND |
1.3 |
1.5 |
1.5 |
5.4 |
7.8 |
4.9 |
4.9 |
B |
ND |
ND |
ND |
ND |
1.2 |
2.5 |
1 |
2.1 |
ND |
3.4 |
2.7 |
|
Mean |
- |
- |
- |
- |
1.3 |
2 |
1.3 |
3.8 |
3.9 |
4.2 |
3.8 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.1 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
1.1 |
- |
- |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.4 |
2.5 |
2.5 |
2.7 |
B |
ND |
ND |
ND |
ND |
ND |
0.9 |
ND |
ND |
ND |
2.1 |
3.5 |
|
Mean |
- |
- |
- |
- |
- |
0.5 |
- |
0.7 |
1.3 |
2.3 |
3.1 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.7 |
2.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.3 |
1.8 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
1.5 |
2.2 |
|
Minor Unknowns (b) |
A |
4.6 |
1.4 |
1.6 |
5.9 |
ND |
ND |
1.5 |
2.2 |
ND |
0.7 |
0.7 |
B |
4.8 |
0.7 |
1.8 |
2 |
ND |
1.4 |
ND |
9 |
6.4 |
0.7 |
2.4 |
|
Mean |
4.7 |
1.1 |
1.7 |
4 |
- |
0.7 |
0.8 |
5.6 |
3.2 |
0.7 |
1.6 |
|
Unassigned Regions (c) |
A |
0.7 |
0.3 |
1 |
0.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
1 |
0.2 |
1.3 |
1.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.9 |
0.3 |
1.2 |
0.9 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.2 |
0.3 |
0.3 |
0.8 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
0.2 |
0.3 |
0.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.1 |
0.3 |
0.3 |
0.6 |
- |
- |
- |
- |
- |
- |
- |
|
(a) Substance determined using TLC Method 1 for 0-6 h. Substance determined using TLC Method 2 for all other timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) Minor shift in retention time observed throughout chromatography
ND: Not Detected
NA: Not Applicable
Table 11. Distribution and Recovery of Radioactivity.
(a) Swiss Lake (Anaerobic Incubation)
Fraction |
Rep. |
0 |
1 h |
3 h |
6 h |
1 |
7 |
15 |
29 |
48 |
61 |
102 |
Surface Water |
A |
85.5 |
90.5 |
75.0 |
79.4 |
87.7 |
80.4 |
69.4 |
60.7 |
49.5 |
46.7 |
41.6 |
B |
81.4 |
80.7 |
73.6 |
80.7 |
79.6 |
70.6 |
63.0 |
54.2 |
49.5 |
45.8 |
41.1 |
|
Mean |
83.5 |
85.6 |
74.3 |
80.1 |
83.7 |
75.5 |
66.2 |
57.5 |
49.5 |
46.3 |
41.4 |
|
Sediment Extract 1(a) |
A |
7.9 |
4.9 |
10.9 |
11.3 |
2.8 |
5.4 |
9.5 |
15.6 |
17.9 |
19.3 |
20.8 |
B |
9.8 |
10.8 |
16.4 |
13.8 |
6.5 |
9.2 |
11.6 |
17.5 |
17.6 |
18.0 |
20.3 |
|
Mean |
8.9 |
7.9 |
13.7 |
12.6 |
4.7 |
7.3 |
10.6 |
16.6 |
17.8 |
18.7 |
20.6 |
|
Sediment Extract 2(b) |
A |
0.9 |
0.7 |
1.8 |
1.3 |
0.8 |
1.9 |
3.3 |
4.6 |
5.3 |
6.3 |
6.5 |
B |
0.9 |
1.3 |
2.5 |
1.7 |
1.7 |
3.3 |
4.0 |
5.2 |
5.6 |
7.1 |
7.0 |
|
Mean |
0.9 |
1.0 |
2.2 |
1.5 |
1.3 |
2.6 |
3.7 |
4.9 |
5.5 |
6.7 |
6.7 |
|
Total Extractable |
Mean |
93.3 |
94.5 |
90.2 |
94.2 |
89.7 |
85.4 |
80.5 |
79.0 |
72.8 |
71.7 |
68.7 |
Non- (c) Extractables |
A |
1.8 |
1.1 |
3.2 |
1.4 |
1.1 |
4.8 |
8.4 |
12.6 |
15.4 |
22.7 |
24.5 |
B |
2.1 |
2.2 |
4.3 |
2.5 |
3.6 |
10.2 |
12.3 |
18.3 |
19.3 |
20.6 |
24.4 |
|
Mean |
2.0 |
1.7 |
3.8 |
2.0 |
2.4 |
7.5 |
10.4 |
15.5 |
17.4 |
21.7 |
24.5 |
|
14CO2 |
A |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<0.1 |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
B |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
<LOQ |
<0.1 |
<0.1 |
|
Mean |
- |
- |
- |
- |
- |
<0.1 |
<0.1 |
- |
- |
<0.1 |
<0.1 |
|
TOTAL |
A |
96.1 |
97.2 |
90.9 |
93.4 |
92.4 |
92.5 |
90.6 |
93.5 |
88.1 |
95.0 |
93.4 |
B |
94.2 |
95.0 |
96.8 |
98.7 |
91.4 |
93.3 |
90.9 |
95.2 |
92.0 |
91.5 |
92.8 |
|
Mean |
95.2 |
96.1 |
93.9 |
96.1 |
91.9 |
92.9 |
90.8 |
94.4 |
90.1 |
93.3 |
93.1 |
|
Mean ± SD |
93.4 ± 2.5 |
|||||||||||
(a) = Acetonitrile: 0.3M HCl (8:2, v/v) x 2 extractions
(b) = Acetonitrile: 1.5M HCl (8:2, v/v) x 2 extractions
(c) = Further investigated at 102 DAT using reflux and organic matter fractionation
NA = Not applicable
<LOQ = Below Limit of Quantification
(b) Calwich Abbey (Anaerobic Incubation)
Fraction |
Rep. |
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
Surface Water |
A |
94.3 |
89.5 |
93.2 |
86.7 |
83.0 |
79.3 |
59.2 |
51.6 |
43.6 |
40.5 |
37.2 |
B |
85.7 |
89.0 |
87.3 |
84.0 |
85.6 |
80.4 |
70.5 |
45.6 |
44.1 |
41.9 |
37.4 |
|
Mean |
90.0 |
89.3 |
90.3 |
85.4 |
84.3 |
79.9 |
64.9 |
48.6 |
43.9 |
41.2 |
37.3 |
|
Sediment Extract 1(a) |
A |
4.1 |
5.8 |
5.0 |
6.8 |
10.1 |
12.7 |
24.2 |
23.0 |
23.8 |
23.5 |
19.2 |
B |
11.9 |
7.1 |
8.5 |
10.2 |
8.6 |
13.8 |
16.1 |
26.9 |
24.0 |
24.0 |
18.7 |
|
Mean |
8.0 |
6.5 |
6.8 |
8.5 |
9.4 |
13.3 |
20.2 |
25.0 |
23.9 |
23.8 |
19.0 |
|
Sediment Extract 2(b) |
A |
0.4 |
0.4 |
0.7 |
0.6 |
0.9 |
1.1 |
2.3 |
2.4 |
2.8 |
2.7 |
2.8 |
B |
0.9 |
0.5 |
0.4 |
0.9 |
0.8 |
1.2 |
1.7 |
2.9 |
2.8 |
2.7 |
2.7 |
|
Mean |
0.7 |
0.5 |
0.6 |
0.8 |
0.9 |
1.2 |
2.0 |
2.7 |
2.8 |
2.7 |
2.8 |
|
Total Extractable |
Mean |
98.7 |
96.3 |
97.7 |
94.7 |
94.6 |
94.4 |
87.1 |
76.3 |
70.6 |
67.7 |
59.1 |
Non- Extractables(c) |
A |
0.6 |
1.6 |
1.3 |
1.7 |
2.6 |
4.6 |
12.6 |
19.1 |
28.9 |
28.6 |
38.6 |
B |
1.9 |
1.7 |
1.5 |
3.2 |
2.4 |
4.9 |
9.1 |
18.9 |
28.2 |
28.4 |
38.6 |
|
Mean |
1.3 |
1.7 |
1.4 |
2.5 |
2.5 |
4.8 |
10.9 |
19.0 |
28.6 |
28.5 |
38.6 |
|
14CO2 |
A |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
B |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
|
Mean |
- |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
- |
- |
- |
<0.1 |
- |
|
TOTAL |
A |
99.4 |
97.3 |
100.2 |
95.8 |
96.6 |
97.7 |
98.3 |
96.1 |
99.1 |
95.3 |
97.8 |
B |
100.4 |
98.3 |
97.7 |
98.3 |
97.4 |
100.3 |
97.4 |
94.3 |
99.1 |
97.0 |
97.4 |
|
Mean |
99.9 |
97.8 |
99.0 |
97.1 |
97.0 |
99.0 |
97.9 |
95.2 |
99.1 |
96.2 |
97.6 |
|
Mean ± SD |
|
97.8 ± 1.6 |
||||||||||
(a) = Acetonitrile:0.3M HCl (8:2, v/v) x 2 extractions
(b) = Acetonitrile:1.5M HCl (8:2, v/v) x 2 extractions
(c) = Further investigated at 102 DAT using reflux and organic matter fractionation
NA = Not applicable
<LOQ = Below Limit of Quantification
Table 12. Summary of Characterisation / Identification of Radioactive Residues in Anaerobic Swiss Lake Water-Sediment System
(a) Radioactive residue in the total syste
Component |
Rep. |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
90.9 |
92.5 |
77.5 |
84.4 |
73.6 |
36.4 |
16.0 |
1.4 |
ND |
ND |
ND |
B |
96.7 |
87.5 |
83.9 |
83.6 |
50.4 |
21.4 |
5.5 |
0.2 |
ND |
ND |
ND |
|
Mean |
93.8 |
90.0 |
80.7 |
84.0 |
62.0 |
28.9 |
10.8 |
0.8 |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.0 |
1.1 |
3.4 |
3.5 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.6 |
0.8 |
1.8 |
3.3 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
1.3 |
1.0 |
2.6 |
3.4 |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
1.1 |
1.6 |
ND |
2.9 |
ND |
4.3 |
B |
ND |
ND |
ND |
ND |
ND |
2.6 |
1.4 |
4.3 |
2.8 |
2.5 |
ND |
|
Mean |
- |
- |
- |
- |
- |
1.9 |
1.5 |
2.2 |
2.9 |
1.3 |
2.2 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
1.0 |
5.6 |
3.7 |
5.0 |
1.9 |
3.2 |
B |
ND |
ND |
ND |
ND |
ND |
1.4 |
ND |
ND |
3.0 |
2.5 |
2.4 |
|
Mean |
- |
- |
- |
- |
- |
1.2 |
2.8 |
1.9 |
4.0 |
2.2 |
2.8 |
|
M18 |
A |
ND |
ND |
ND |
ND |
ND |
10.6 |
21.2 |
46.4 |
26.4 |
23.5 |
11.4 |
B |
ND |
ND |
ND |
ND |
12.2 |
18.9 |
31.6 |
35.5 |
28.2 |
18.8 |
10.0 |
|
Mean |
- |
- |
- |
- |
6.1 |
14.8 |
26.4 |
40.2 |
27.3 |
21.2 |
10.7 |
|
M19 |
A |
ND |
ND |
ND |
ND |
ND |
7.2 |
5.2 |
ND |
1.6 |
2.8 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
7.8 |
12.1 |
1.5 |
ND |
ND |
3.9 |
|
Mean |
- |
- |
- |
- |
- |
7.5 |
8.7 |
0.8 |
0.8 |
1.4 |
2.0 |
|
M4 |
A |
ND |
ND |
ND |
ND |
0.4 |
3.7 |
6.1 |
11.9 |
6.2 |
6.9 |
4.6 |
B |
ND |
ND |
ND |
ND |
1.4 |
8.8 |
3.8 |
8.3 |
4.7 |
8.5 |
3.0 |
|
Mean |
- |
- |
- |
- |
0.9 |
6.3 |
5.0 |
10.1 |
5.5 |
7.7 |
3.8 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
1.0 |
1.5 |
5.8 |
7.7 |
2.8 |
5.0 |
B |
ND |
ND |
ND |
ND |
ND |
3.5 |
ND |
5.5 |
8.7 |
0.0 |
3.0 |
|
Mean |
- |
- |
- |
- |
- |
2.3 |
0.8 |
5.7 |
8.2 |
1.4 |
4.0 |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.1 |
5.0 |
5.3 |
7.9 |
B |
ND |
ND |
ND |
ND |
ND |
1.0 |
1.4 |
1.4 |
4.5 |
6.2 |
10.1 |
|
Mean |
- |
- |
- |
- |
- |
0.5 |
0.7 |
1.3 |
4.8 |
5.8 |
9.0 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.0 |
ND |
2.8 |
9.5 |
12.9 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.7 |
2.5 |
9.9 |
11.6 |
|
Mean |
- |
- |
- |
- |
- |
- |
1.0 |
0.9 |
2.7 |
9.7 |
12.3 |
|
Minor Unknowns (b) |
A |
ND |
ND |
2.1 |
ND |
ND |
11.6 |
10.7 |
8.2 |
13.8 |
16.3 |
16.2 |
B |
ND |
ND |
0.5 |
2.0 |
ND |
8.3 |
16.8 |
17.0 |
17.4 |
16.8 |
21.4 |
|
Mean |
- |
- |
1.3 |
1.0 |
- |
10.0 |
13.8 |
12.6 |
15.6 |
16.6 |
18.8 |
|
Unassigned Regions (c) |
A |
1.2 |
1.9 |
4.8 |
3.5 |
NA |
NA |
0.1 |
NA |
NA |
NA |
NA |
B |
1.3 |
3.3 |
4.6 |
5.3 |
NA |
0.3 |
0.3 |
NA |
NA |
NA |
NA |
|
Mean |
1.3 |
2.6 |
4.7 |
4.4 |
- |
0.2 |
0.2 |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.6 |
1.0 |
3.3 |
2.5 |
NA |
NA |
2.8 |
NA |
NA |
NA |
NA |
B |
0.3 |
0.8 |
1.3 |
3.2 |
NA |
2.7 |
3.2 |
NA |
NA |
NA |
NA |
|
Mean |
0.5 |
0.9 |
2.3 |
2.9 |
- |
1.4 |
3.0 |
- |
- |
- |
- |
|
Carbon Dioxide |
A |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
B |
NA |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
<LOQ |
<0.1 |
<0.1 |
|
Mean |
- |
- |
- |
- |
- |
- |
<0.1 |
- |
- |
<0.1 |
<0.1 |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
(b) Radioactive residue in the water phase:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
85.0 |
88.4 |
69.4 |
74.9 |
72.0 |
36.4 |
16.0 |
1.4 |
ND |
ND |
ND |
B |
88.8 |
78.7 |
70.8 |
71.9 |
48.2 |
20.9 |
5.5 |
ND |
ND |
ND |
ND |
|
Mean |
86.9 |
83.6 |
70.1 |
73.4 |
60.1 |
28.7 |
10.8 |
0.7 |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.6 |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
0.8 |
- |
- |
- |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
1.1 |
1.6 |
ND |
2.9 |
ND |
4.3 |
B |
ND |
ND |
ND |
ND |
ND |
2.6 |
1.4 |
4.3 |
2.5 |
2.5 |
ND |
|
Mean |
- |
- |
- |
- |
- |
1.9 |
1.5 |
2.2 |
2.7 |
1.3 |
2.2 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
1.0 |
4.4 |
3.7 |
5.0 |
1.9 |
3.2 |
B |
ND |
ND |
ND |
ND |
ND |
1.4 |
ND |
ND |
3.0 |
2.5 |
2.4 |
|
Mean |
- |
- |
- |
- |
- |
1.2 |
2.2 |
1.9 |
4.0 |
2.2 |
2.8 |
|
M18 |
A |
ND |
ND |
ND |
ND |
ND |
9.0 |
21.2 |
42.5 |
23.9 |
20.7 |
9.8 |
B |
ND |
ND |
ND |
ND |
12.2 |
16.1 |
31.6 |
27.9 |
24.7 |
15.2 |
8.7 |
|
Mean |
- |
- |
- |
- |
6.1 |
12.6 |
26.4 |
35.2 |
24.3 |
18.0 |
9.3 |
|
M19 |
A |
ND |
ND |
ND |
ND |
ND |
7.2 |
5.2 |
ND |
1.6 |
2.8 |
ND |
B |
ND |
ND |
ND |
ND |
ND |
7.8 |
12.1 |
1.5 |
ND |
ND |
3.9 |
|
Mean |
- |
- |
- |
- |
- |
7.5 |
8.7 |
0.8 |
0.8 |
1.4 |
2.0 |
|
M4 |
A |
ND |
ND |
ND |
ND |
ND |
2.8 |
6.1 |
5.8 |
4.6 |
4.5 |
2.6 |
B |
ND |
ND |
ND |
ND |
ND |
6.5 |
3.8 |
6.4 |
4.7 |
5.6 |
1.3 |
|
Mean |
- |
- |
- |
- |
- |
4.7 |
5.0 |
6.1 |
4.7 |
5.1 |
2.0 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
1.0 |
1.5 |
8.8 |
6.7 |
2.8 |
5.0 |
B |
ND |
ND |
ND |
ND |
ND |
3.5 |
ND |
5.5 |
8.0 |
ND |
3.0 |
|
Mean |
- |
- |
- |
- |
- |
2.3 |
0.8 |
7.2 |
7.4 |
1.4 |
4.0 |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.8 |
2.6 |
3.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
1.4 |
ND |
2.0 |
2.8 |
5.8 |
|
Mean |
- |
- |
- |
- |
- |
- |
0.7 |
- |
2.4 |
2.7 |
4.7 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
4.5 |
6.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
5.5 |
5.9 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
5.0 |
6.3 |
|
Minor Unknowns (b) |
A |
ND |
ND |
1.8 |
ND |
ND |
9.8 |
6.6 |
ND |
1.9 |
7.0 |
6.6 |
B |
ND |
ND |
0.5 |
2.0 |
ND |
5.0 |
4.7 |
7.0 |
4.6 |
7.9 |
10.3 |
|
Mean |
- |
- |
1.2 |
1.0 |
- |
7.4 |
5.7 |
3.5 |
3.3 |
7.5 |
8.5 |
|
Unassigned Regions (c) |
A |
0.5 |
1.3 |
1.9 |
2.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
1.7 |
1.3 |
4.0 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.3 |
1.5 |
1.6 |
3.2 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
ND |
0.2 |
1.9 |
2.1 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
0.5 |
1.0 |
2.7 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
- |
0.4 |
1.5 |
2.4 |
- |
- |
- |
- |
- |
- |
- |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
(c) Radioactive residue in the sediment phase (Extract 1):
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
5.9 |
4.1 |
8.1 |
9.5 |
1.6 |
ND |
ND |
ND |
ND |
ND |
ND |
B |
7.9 |
8.8 |
12.5 |
11.7 |
2.2 |
0.5 |
ND |
0.2 |
ND |
ND |
ND |
|
Mean |
6.9 |
6.5 |
10.3 |
10.6 |
1.9 |
0.3 |
- |
0.1 |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.0 |
1.1 |
3.4 |
3.5 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.8 |
1.8 |
3.3 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
0.5 |
1.0 |
2.6 |
3.4 |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
1.2 |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
0.6 |
- |
- |
- |
- |
|
M18 |
A |
ND |
ND |
ND |
ND |
ND |
1.6 |
ND |
3.9 |
1.6 |
2.1 |
1.6 |
B |
ND |
ND |
ND |
ND |
ND |
2.8 |
ND |
6.1 |
1.8 |
3.6 |
1.3 |
|
Mean |
- |
- |
- |
- |
- |
2.2 |
- |
5.0 |
1.7 |
2.9 |
1.5 |
|
M19 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
0.4 |
0.9 |
ND |
2.4 |
1.6 |
2.4 |
2.0 |
B |
ND |
ND |
ND |
ND |
1.4 |
2.3 |
ND |
0.8 |
ND |
2.9 |
1.7 |
|
Mean |
- |
- |
- |
- |
0.9 |
1.6 |
- |
1.6 |
0.8 |
2.7 |
1.9 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.0 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
0.7 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
0.9 |
- |
- |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.1 |
1.8 |
2.7 |
4.3 |
B |
ND |
ND |
ND |
ND |
ND |
1.0 |
ND |
1.4 |
2.3 |
3.4 |
4.3 |
|
Mean |
- |
- |
- |
- |
- |
0.5 |
- |
1.3 |
2.1 |
3.1 |
4.3 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.0 |
ND |
2.8 |
5.0 |
6.3 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
1.7 |
2.5 |
4.4 |
5.7 |
|
Mean |
- |
- |
- |
- |
- |
- |
1.0 |
0.9 |
2.7 |
4.7 |
6.0 |
|
Minor Unknowns (b) |
A |
0.5 |
ND |
ND |
0.2 |
ND |
1.8 |
3.7 |
7.3 |
7.9 |
3.7 |
3.1 |
B |
0.3 |
ND |
ND |
0.3 |
ND |
3.0 |
11.6 |
7.4 |
9.5 |
1.8 |
4.1 |
|
Mean |
0.4 |
- |
- |
0.3 |
- |
2.4 |
7.7 |
7.4 |
8.7 |
2.8 |
3.6 |
|
Unassigned Regions (c) |
A |
0.7 |
0.6 |
2.5 |
1.1 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
1.3 |
1.6 |
3.3 |
1.3 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
1.0 |
1.1 |
2.9 |
1.2 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.6 |
0.2 |
0.3 |
0.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
0.3 |
0.5 |
0.6 |
0.5 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.5 |
0.4 |
0.5 |
0.5 |
- |
- |
- |
- |
- |
- |
- |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
(d) Radioactive residue in the sediment phase (Extract 2):
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
15 |
29 |
48 |
61 |
102 |
||
Substance |
A |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
ND |
B |
NA |
NA |
0.6 |
NA |
NA |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
0.3 |
- |
- |
- |
- |
- |
- |
- |
- |
|
M8 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M17 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
0.3 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
0.2 |
- |
- |
|
M13 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M18 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
0.9 |
0.7 |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
1.7 |
|
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
1.3 |
0.4 |
- |
|
M19 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M4 |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Unknown 38 min (e) |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Unknown 40 min (e) |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
0.4 |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
0.2 |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
0.3 |
- |
- |
|
Unknown 44 min (e) |
A |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Minor Unknowns (b) |
A |
NA |
NA |
0.3 |
NA |
NA |
NA |
0.4 |
0.9 |
4.0 |
5.6 |
6.5 |
B |
NA |
NA |
ND |
NA |
NA |
0.3 |
0.5 |
2.6 |
3.3 |
7.1 |
7.0 |
|
Mean |
- |
- |
0.2 |
- |
- |
0.2 |
0.5 |
1.8 |
3.7 |
6.4 |
6.8 |
|
Unassigned Regions (c) |
A |
NA |
NA |
0.4 |
NA |
NA |
NA |
0.1 |
NA |
NA |
NA |
NA |
B |
NA |
NA |
ND |
NA |
NA |
0.3 |
0.3 |
NA |
NA |
NA |
NA |
|
Mean |
- |
- |
0.2 |
- |
- |
0.2 |
0.2 |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
NA |
NA |
1.1 |
NA |
NA |
NA |
2.8 |
NA |
NA |
NA |
NA |
B |
NA |
NA |
ND |
NA |
NA |
2.7 |
3.2 |
NA |
NA |
NA |
NA |
|
Mean |
- |
- |
0.6 |
- |
- |
- |
3.0 |
- |
- |
- |
- |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
Table 13 Summary of Characterisation / Identification of Radioactive Residues in Anaerobic Calwich Abbey Water-Sediment System
(a) Radioactive residue in the total system:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
||
Substance |
A |
94.2 |
90.1 |
92.3 |
79.1 |
68.5 |
31.0 |
1.8 |
ND |
ND |
ND |
ND |
B |
89.5 |
90.9 |
88.3 |
78.7 |
66.8 |
26.7 |
11.0 |
ND |
ND |
ND |
ND |
|
Mean |
91.9 |
90.5 |
90.3 |
78.9 |
67.7 |
28.9 |
6.4 |
- |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.3 |
5.3 |
6.5 |
11.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
4.2 |
8.8 |
10.2 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
1.7 |
4.8 |
7.7 |
10.9 |
|
M17 |
A |
ND |
ND |
ND |
ND |
3.7 |
3.5 |
12.7 |
14.8 |
2.1 |
2.5 |
0.8 |
B |
ND |
ND |
ND |
ND |
3.7 |
7.1 |
6.8 |
13.3 |
2.1 |
2.0 |
1.1 |
|
Mean |
- |
- |
- |
- |
3.7 |
5.3 |
9.8 |
14.1 |
2.1 |
2.3 |
1.0 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
2.0 |
2.5 |
ND |
9.9 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
3.7 |
4.3 |
1.0 |
3.7 |
ND |
3.2 |
|
Mean |
- |
- |
- |
- |
- |
2.9 |
3.4 |
0.5 |
6.8 |
- |
1.6 |
|
M18 |
A |
ND |
ND |
ND |
ND |
6.4 |
25.8 |
36.4 |
40.9 |
15.6 |
21.5 |
4.4 |
B |
ND |
ND |
ND |
ND |
5.7 |
29.3 |
46.3 |
38.6 |
21.9 |
21.4 |
5.4 |
|
Mean |
- |
- |
- |
- |
6.1 |
27.6 |
41.4 |
39.8 |
18.8 |
21.5 |
4.9 |
|
M19 |
A |
ND |
ND |
ND |
ND |
4.1 |
4.6 |
11.7 |
ND |
2.2 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
1.8 |
6.8 |
5.1 |
4.5 |
1.4 |
1.1 |
ND |
|
Mean |
- |
- |
- |
- |
3.0 |
5.7 |
8.4 |
2.3 |
1.8 |
0.6 |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
10.5 |
5.3 |
7.1 |
6.6 |
14.5 |
6.1 |
0.6 |
B |
ND |
ND |
ND |
ND |
6.7 |
6.3 |
8.1 |
6.8 |
10.3 |
4.1 |
2.7 |
|
Mean |
- |
- |
- |
- |
8.6 |
5.7 |
7.6 |
6.7 |
12.4 |
5.1 |
1.7 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
2.5 |
2.4 |
6.5 |
ND |
5.9 |
5.8 |
B |
ND |
ND |
ND |
ND |
1.3 |
2.5 |
5.9 |
3.6 |
ND |
4.1 |
ND |
|
Mean |
- |
- |
- |
- |
0.7 |
2.5 |
4.2 |
5.1 |
- |
5.0 |
2.9 |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
3.5 |
2.0 |
4.5 |
13.9 |
11.1 |
B |
ND |
ND |
ND |
ND |
ND |
1.4 |
ND |
2.6 |
8.7 |
15.8 |
14.0 |
|
Mean |
- |
- |
- |
- |
- |
0.7 |
1.7 |
2.3 |
6.6 |
14.9 |
12.6 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
1.2 |
ND |
ND |
3.9 |
10.1 |
B |
ND |
ND |
ND |
ND |
ND |
0.8 |
1.1 |
ND |
2.1 |
3.5 |
7.9 |
|
Mean |
- |
- |
- |
- |
- |
0.4 |
1.2 |
- |
1.1 |
3.7 |
9.0 |
|
Minor Unknowns (b) |
A |
0.9 |
2.8 |
2.1 |
7.7 |
1.5 |
1.7 |
3.6 |
0.7 |
10.0 |
3.7 |
12.1 |
B |
5.8 |
2.6 |
4.8 |
9.9 |
ND |
7.5 |
1.5 |
2.1 |
11.1 |
5.2 |
11.7 |
|
Mean |
3.4 |
2.7 |
3.5 |
8.8 |
0.8 |
4.6 |
2.6 |
1.4 |
10.6 |
4.5 |
11.9 |
|
Unassigned Regions (c) |
A |
2.9 |
1.4 |
2.3 |
3.0 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
2.4 |
1.6 |
1.3 |
3.3 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
2.7 |
1.5 |
1.8 |
3.2 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.3 |
1.1 |
1.6 |
3.7 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
1.0 |
1.6 |
2.2 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.2 |
1.1 |
1.6 |
3.0 |
- |
- |
- |
- |
- |
- |
- |
|
Carbon Dioxide |
A |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
<LOQ |
B |
NA |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<LOQ |
<LOQ |
<LOQ |
<0.1 |
<LOQ |
|
Mean |
- |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
<0.1 |
- |
- |
- |
<0.1 |
- |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
(b) Radioactive residue in the water phase:
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
||
Substance |
A |
92.4 |
86.9 |
89.6 |
76.3 |
68.5 |
31.0 |
1.8 |
ND |
ND |
ND |
ND |
B |
84.4 |
86.9 |
84.3 |
74.7 |
66.8 |
26.7 |
11.0 |
ND |
ND |
ND |
ND |
|
Mean |
88.4 |
86.9 |
87.0 |
75.5 |
67.7 |
28.9 |
6.4 |
- |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.3 |
ND |
ND |
6.4 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.0 |
5.2 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
1.7 |
- |
1.0 |
5.8 |
|
M17 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
2.9 |
2.5 |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
1.4 |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
2.2 |
1.3 |
- |
- |
- |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
2.0 |
2.5 |
ND |
9.9 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
3.7 |
4.3 |
1.0 |
3.7 |
ND |
3.2 |
|
Mean |
- |
- |
- |
- |
- |
2.9 |
3.4 |
0.5 |
6.8 |
- |
1.6 |
|
M18 |
A |
ND |
ND |
ND |
ND |
3.7 |
21.9 |
34.0 |
31.3 |
15.6 |
19.8 |
4.4 |
B |
ND |
ND |
ND |
ND |
3.6 |
27.5 |
43.6 |
26.6 |
19.8 |
19.6 |
5.4 |
|
Mean |
- |
- |
- |
- |
3.7 |
24.7 |
38.8 |
29.0 |
17.7 |
19.7 |
4.9 |
|
M19 |
A |
ND |
ND |
ND |
ND |
1.1 |
2.1 |
4.3 |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
3.1 |
ND |
4.5 |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
0.6 |
2.6 |
2.2 |
2.3 |
- |
- |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
9.8 |
4.2 |
6.2 |
5.4 |
11.3 |
2.6 |
ND |
B |
ND |
ND |
ND |
ND |
5.7 |
6.3 |
6.7 |
5.2 |
7.0 |
2.0 |
1.6 |
|
Mean |
- |
- |
- |
- |
7.8 |
5.3 |
6.5 |
5.3 |
9.2 |
2.3 |
0.8 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
2.5 |
2.4 |
6.5 |
ND |
5.9 |
5.8 |
B |
ND |
ND |
ND |
ND |
1.3 |
2.5 |
5.9 |
3.6 |
ND |
4.1 |
ND |
|
Mean |
- |
- |
- |
- |
0.7 |
2.5 |
4.2 |
5.1 |
- |
5.0 |
2.9 |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
3.3 |
2.0 |
4.5 |
11.7 |
10.0 |
B |
ND |
ND |
ND |
ND |
ND |
1.4 |
ND |
2.6 |
5.7 |
13.2 |
13.1 |
|
Mean |
- |
- |
- |
- |
- |
0.7 |
1.7 |
2.3 |
5.1 |
12.5 |
11.6 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
6.0 |
B |
ND |
ND |
ND |
ND |
ND |
0.8 |
ND |
ND |
ND |
ND |
3.1 |
|
Mean |
- |
- |
- |
- |
- |
0.4 |
- |
- |
- |
- |
4.6 |
|
Minor Unknowns (b) |
A |
ND |
0.6 |
1.0 |
4.3 |
1.5 |
ND |
1.1 |
0.7 |
2.3 |
0.5 |
4.6 |
B |
ND |
0.5 |
0.8 |
4.5 |
ND |
6.3 |
1.0 |
2.1 |
8.0 |
1.1 |
5.8 |
|
Mean |
- |
0.6 |
0.9 |
4.4 |
0.8 |
3.2 |
1.1 |
1.4 |
5.2 |
0.8 |
5.2 |
|
Unassigned Regions (c) |
A |
1.6 |
1.3 |
1.2 |
2.7 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
1.3 |
1.0 |
1.0 |
2.8 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
1.5 |
1.2 |
1.1 |
2.8 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
0.3 |
0.7 |
1.4 |
3.4 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
0.6 |
1.3 |
1.9 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
0.2 |
0.7 |
1.4 |
2.7 |
- |
- |
- |
- |
- |
- |
- |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
(c) Radioactive residue in the sediment phase (Extract 1):
Component |
Rep |
Component as % AR at Each Timepoint (DAT) (a) |
||||||||||
0 |
1 h |
3 h |
6 h |
1 |
7 |
14 |
29 |
46 |
60 |
102 |
||
Substance |
A |
1.8 |
3.2 |
2.7 |
2.8 |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
5.1 |
4.0 |
4.0 |
4.0 |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
3.5 |
3.6 |
3.4 |
3.4 |
- |
- |
- |
- |
- |
- |
- |
|
M8 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
5.3 |
6.5 |
5.2 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
4.2 |
6.8 |
5.0 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
4.8 |
6.7 |
5.1 |
|
M17 |
A |
ND |
ND |
ND |
ND |
3.7 |
3.5 |
9.8 |
12.3 |
2.1 |
2.5 |
0.8 |
B |
ND |
ND |
ND |
ND |
3.7 |
7.1 |
5.4 |
13.3 |
2.1 |
2.0 |
1.1 |
|
Mean |
- |
- |
- |
- |
3.7 |
5.3 |
7.6 |
12.8 |
2.1 |
2.3 |
1.0 |
|
M13 |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
M18 |
A |
ND |
ND |
ND |
ND |
2.7 |
3.9 |
2.4 |
9.6 |
ND |
1.7 |
ND |
B |
ND |
ND |
ND |
ND |
2.1 |
1.8 |
2.7 |
12.0 |
2.1 |
1.8 |
ND |
|
Mean |
- |
- |
- |
- |
2.4 |
2.9 |
2.6 |
10.8 |
1.1 |
1.8 |
- |
|
M19 |
A |
ND |
ND |
ND |
ND |
3.0 |
2.5 |
7.4 |
ND |
2.2 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
1.8 |
3.7 |
5.1 |
ND |
1.8 |
1.1 |
ND |
|
Mean |
- |
- |
- |
- |
2.4 |
3.1 |
6.3 |
- |
0.7 |
0.6 |
- |
|
M4 |
A |
ND |
ND |
ND |
ND |
0.7 |
1.1 |
0.9 |
1.2 |
3.2 |
3.5 |
0.6 |
B |
ND |
ND |
ND |
ND |
1.0 |
ND |
1.4 |
1.6 |
3.3 |
2.1 |
1.1 |
|
Mean |
- |
- |
- |
- |
0.9 |
0.6 |
1.2 |
1.4 |
3.3 |
2.8 |
0.9 |
|
Unknown 38 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
- |
|
Unknown 40 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
2.2 |
1.1 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.0 |
2.6 |
0.9 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
- |
1.5 |
2.4 |
1.0 |
|
Unknown 44 min (e) |
A |
ND |
ND |
ND |
ND |
ND |
ND |
1.2 |
ND |
ND |
3.9 |
4.1 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
1.1 |
ND |
2.1 |
3.5 |
4.8 |
|
Mean |
- |
- |
- |
- |
- |
- |
1.2 |
- |
1.1 |
3.7 |
4.5 |
|
Minor Unknowns (b) |
A |
0.9 |
2.2 |
1.1 |
3.4 |
ND |
1.7 |
2.5 |
ND |
7.7 |
3.2 |
7.5 |
B |
5.8 |
2.1 |
4.0 |
5.4 |
ND |
1.2 |
0.5 |
ND |
5.9 |
4.1 |
5.9 |
|
Mean |
3.4 |
2.2 |
2.6 |
4.4 |
- |
1.5 |
1.5 |
- |
6.8 |
3.7 |
6.7 |
|
Unassigned Regions (c) |
A |
1.3 |
0.1 |
1.1 |
0.3 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
1.1 |
0.6 |
0.3 |
0.5 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
1.2 |
0.4 |
0.7 |
0.4 |
- |
- |
- |
- |
- |
- |
- |
|
Origin Bound (d) |
A |
ND |
0.4 |
0.2 |
0.3 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
B |
ND |
0.4 |
0.3 |
0.3 |
NA |
NA |
NA |
NA |
NA |
NA |
NA |
|
Mean |
- |
0.4 |
0.3 |
0.3 |
- |
- |
- |
- |
- |
- |
- |
|
(a) = the test substance determined using TLC Method 1 for 0-6 h. the test substance determined using TLC Method 2 for all other
timepoints. All other components determined using HPLC method 2. No HPLC analysis was carried out on 0-6h samples.
(b) = Sum of individual minor unknown components (Mean %AR did not exceed 5%)
(c) = Unassigned radiocomponents which chromatographed away from the baseline in TLC
(d) = Unassigned radiocomponents which did not chromatograph away from the baseline in TLC
(e) = Minor shift in retention time observed throughout chromatography
<LOQ = Below Limit of Quantification
ND = Not Detected
NA = Not Applicable
Table 14. Reflux Extraction of Selected Samples
Selected samples for Reflux |
Percent of Applied Radioactivity |
||||||
Pre-Reflux |
% AR in Reflux Extract |
% AR in Soil Debris |
Overall Recovery |
||||
Soil Type |
Timepoint (DAT) |
Replicate |
|||||
Swiss Lake Aerobic |
102 |
A |
29.2 |
5.3 |
22.5 |
27.8 |
|
B |
29.6 |
5.5 |
24.3 |
29.8 |
|||
Mean |
29.4 |
5.4 |
23.4 |
28.8 |
|||
Calwich Abbey Aerobic |
102 |
A |
64.6 |
5.6 |
50.8 |
56.4 |
|
B |
65.7 |
5.1 |
52.8 |
57.9 |
|||
Mean |
65.2 |
5.4 |
51.8 |
57.2 |
|||
Swiss Lake Anaerobic |
102 |
A |
24.5 |
4.9 |
17.8 |
22.7 |
|
B |
24.4 |
5.0 |
22.0 |
27.0 |
|||
Mean |
24.5 |
5.0 |
19.9 |
24.9 |
|||
Calwich Abbey Anaerobic |
102 |
A |
38.6 |
3.6 |
32.9 |
36.5 |
|
B |
38.6 |
4.2 |
33.1 |
37.3 |
|||
Mean |
38.6 |
3.9 |
33.0 |
36.9 |
|||
Table 15. Organic Matter Fractionation of Selected Samples
Selected samples for OMF |
Percent of Applied Radioactivity |
|||||||
Pre- OMF |
OMF Fulvic Acid |
OMF Humic Acid |
OMF Humin |
OMF Recovery |
||||
Soil Type |
Timepoint (DAT) |
Replicate |
||||||
Swiss Lake Aerobic |
102 |
A |
29.2 |
5.8 |
8.0 |
19.7 |
33.5 |
|
B |
30.2 |
6.4 |
8.7 |
18.2 |
33.3 |
|||
Mean |
29.4 |
6.1 |
8.4 |
18.9 |
33.4 |
|||
Calwich Abbey Aerobic |
102 |
A |
64.6 |
9.9 |
3.4 |
43.8 |
61.4 |
|
B |
65.7 |
9.8 |
3.5 |
47.1 |
60.4 |
|||
Mean |
65.2 |
9.9 |
3.5 |
45.5 |
60.9 |
|||
Swiss Lake Anaerobic |
102 |
A |
24.5 |
5.4 |
5.8 |
17.3 |
28.5 |
|
B |
24.4 |
5.2 |
6.5 |
14.6 |
26.3 |
|||
Mean |
24.5 |
5.3 |
6.2 |
16.0 |
27.4 |
|||
Calwich Abbey Anaerobic |
102 |
A |
38.6 |
7.8 |
2.2 |
28.8 |
38.8 |
|
B |
38.6 |
7.1 |
2.3 |
26.7 |
36.1 |
|||
Mean |
38.6 |
7.5 |
2.3 |
27.8 |
37.5 |
|||
Table 16. Summary of DegT50 and DegT90 Values
Water-sediment system |
Phase |
SFO |
||||
DegT50 (Days) |
DegT90 (Days) |
χ2 |
R2 |
Prob > t |
||
Aerobic |
||||||
Swiss Lake |
Water Total |
10 9 |
32 30 |
6.2 4.9 |
0.9568 0.9709 |
7.7 x 10-7 9.8 x 10-8 |
Calwich Abbey |
Water Total |
3 3 |
12 12 |
5.8 5.4 |
0.9803 0.9824 |
2.0 x 10-7 9.7 x 10-8 |
Anaerobic |
||||||
Swiss Lake |
Water Total |
5 4 |
15 14 |
8.0 7.6 |
0.9420 0.9535 |
2.1 x 10-5 1.1 x 10-5 |
Calwich Abbey |
Water Total |
4 4 |
13 13 |
5.0 5.4 |
0.9853 0.9854 |
1.0 x 10-8 1.3 x 10-8 |
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
Table 6. Radiochemical Purity Results
Time Point/Event |
Radiochemical Purity (%) |
|||
Low Rate |
High Rate |
|||
HPLC |
TLC |
HPLC |
TLC |
|
Treatment Solution |
99.3 |
99.4 |
97.7 |
95.1 |
Table 7. Distribution and Recovery of Radioactivity: Surface Water Expressed as % Applied Radioactivity
a. Test samples - low concentration (10 µg/L)
Fraction |
Rep. |
Incubation Time (DAT) |
|||||||
0 |
1 h |
3 h |
12 h |
2 |
5 |
29 |
60 |
||
Surface water |
A |
96.1 |
89.4 |
98.2 |
95.5 |
92.8 |
90.4 |
92.1 |
87.1 |
B |
97.7 |
98.7 |
94.9 |
97.1 |
90.3 |
89.1 |
90.1 |
83.7 |
|
Mean |
96.9 |
94.1 |
96.6 |
96.3 |
91.6 |
89.8 |
91.1 |
85.4 |
|
Apparatus Wash |
A |
1.1 |
1.0 |
1.1 |
0.9 |
1.7 |
2.2 |
4.4 |
2.9 |
B |
1.2 |
1.0 |
1.1 |
0.9 |
1.8 |
1.8 |
5.2 |
3.7 |
|
Mean |
1.2 |
1.0 |
1.1 |
0.9 |
1.8 |
2.0 |
4.8 |
3.3 |
|
14CO2 |
A |
NA |
< LOD |
< LOD |
< LOD |
< LOD |
< LOD |
0.6 |
16.0 |
B |
NA |
< LOD |
< LOD |
< LOD |
2.7 |
1.8 |
0.5 |
5.5 |
|
Mean |
- |
- |
- |
- |
1.4 |
0.9 |
0.6 |
10.8 |
|
TOTAL |
A |
97.2 |
90.4 |
99.3 |
96.4 |
94.5 |
92.6 |
97.1 |
106.0 |
B |
98.9 |
99.7 |
96.0 |
98.0 |
94.8 |
92.7 |
95.8 |
92.9 |
|
Mean |
98.1 |
95.1 |
97.7 |
97.2 |
94.7 |
92.7 |
96.5 |
99.5 |
|
Mean ± SD |
96.4 ± 2.2 |
||||||||
b.Test samples - high concentration (50 µg/L)
Fraction |
Rep. |
Incubation Time (DAT) |
|||||||
0 |
1 h |
3 h |
12 h |
2 |
5 |
30 |
60 |
||
Surface water |
A |
98.3 |
96.6 |
94.5 |
99.7 |
95.2 |
86.4 |
75.3 |
79.6 |
B |
96.4 |
95.8 |
93.6 |
102.4 |
89.6 |
91.1 |
77.4 |
79.3 |
|
Mean |
97.4 |
96.2 |
94.1 |
101.2 |
92.4 |
88.8 |
76.4 |
79.5 |
|
Apparatus Wash |
A |
1.5 |
0.8 |
12.5 |
0.7 |
0.9 |
2.9 |
11.2 |
6.1 |
B |
1.2 |
0.8 |
0.8 |
0.8 |
2.4 |
3.5 |
8.4 |
6.9 |
|
Mean |
1.4 |
0.8 |
6.7 |
0.8 |
1.7 |
3.2 |
9.8 |
6.5 |
|
14CO2 |
A |
NA |
0.2 |
0.1 |
0.4 |
0.4 |
0.7 |
0.1 |
0.4 |
B |
NA |
0.3 |
< LOD |
< LOD |
0.4 |
0.6 |
1.2 |
2.0 |
|
Mean |
- |
0.2 |
0.1 |
0.2 |
0.4 |
0.7 |
0.8 |
1.2 |
|
TOTAL |
A |
99.8 |
97.6 |
107.1 |
100.8 |
96.5 |
90.0 |
86.6 |
86.1 |
B |
97.6 |
96.9 |
94.4 |
103.2 |
92.4 |
95.2 |
87.0 |
88.2 |
|
Mean |
98.7 |
97.3 |
100.8 |
102.0 |
94.5 |
92.6 |
86.8 |
87.2 |
|
Mean ± SD |
95.0 ± 5.8 |
||||||||
c. Sterilised samples analysed with low concentration (10 µg/L)
Fraction |
Rep. |
Incubation Time (DAT) |
65 |
||
Surface water |
A |
91.5 |
B |
90.5 |
|
Mean |
91.0 |
|
Apparatus Wash |
A |
1.2 |
B |
1.8 |
|
Mean |
1.5 |
|
14CO2 |
A |
0.5 |
B |
< LOD |
|
Mean |
0.3 |
|
TOTAL |
A |
93.2 |
B |
92.3 |
|
Mean ± SD |
92.8 ± 0.7 |
|
d. Sterilised samples analysed with high concentration (50 µg/L)
Fraction |
Rep. |
Incubation Time (DAT) |
59 |
||
Surface water |
A |
89.2 |
B |
75.5 |
|
Mean |
89.2 |
|
Apparatus Wash |
A |
4.5 |
B |
1.2 |
|
Mean |
4.5 |
|
14CO2 |
A |
0.4 |
B |
< LOD |
|
Mean |
0.4 |
|
TOTAL |
A |
94.1 |
B |
76.7(a) |
|
Mean ± SD |
94.1 |
|
(a) = Postulated to be a result of treatment error; excluded from calculations
e. Reference samples - [14C]-Sodium benzoate (10 µg/L) - Low Rate Experiment
Fraction |
Rep. |
Incubation time (days) |
65 |
||
Surface water |
A |
3.9 |
B |
3.2 |
|
Mean |
3.6 |
|
Apparatus Wash |
A |
< LOD |
B |
< LOD |
|
Mean |
- |
|
14CO2 |
A |
90.0 |
B |
79.0 |
|
Mean |
84.5 |
|
TOTAL |
A |
93.9 |
B |
82.2(a) |
|
Mean ± SD |
88.1 ± 8.3 |
|
(a) = Low mass balance. Postulated incomplete capture of CO2
f. Reference samples - [14C]-Sodium benzoate (10 µg/L) – High Rate Experiment
Fraction |
Rep. |
Incubation time (days) |
59 |
||
Surface water |
A |
10.0 |
B |
9.5 |
|
Mean |
9.8 |
|
Apparatus Wash |
A |
3.5 |
B |
3.0 |
|
Mean |
3.3 |
|
14CO2 |
A |
39.1 |
B |
12.5 |
|
Mean |
25.8 |
|
TOTAL |
A |
52.6 |
B |
25.0 |
|
Mean ± SD |
38.8 ± 19.5(a) |
|
(a) = Low mass balance. Postulated incomplete capture of CO2
g. Solvent Control samples - [14C]-Sodium benzoate (10 µg/L) - Low Rate Experiment
Fraction |
Rep. |
Incubation time (days) |
65 |
||
Surface water |
A |
6.7 |
B |
4.0 |
|
Mean |
5.4 |
|
Apparatus Wash |
A |
0.0 |
B |
0.1 |
|
Mean |
0.1 |
|
14CO2 |
A |
103.3 |
B |
58.9 |
|
Mean |
81.1 |
|
TOTAL |
A |
110.0 |
B |
63.0(a) |
|
Mean ± SD |
86.5 ± 33.2 |
|
(a) = postulated incomplete capture of CO2 in replicate B
h. Solvent Control samples - [14C]-Sodium benzoate (10 µg/L) – High Rate Experiment
Fraction |
Rep. |
Incubation time (days) |
59 |
||
Surface water |
B |
11.3 |
Apparatus Wash |
3.2 |
|
14CO2 |
101.8 |
|
TOTAL |
116.3 |
|
Mean ± SD |
116.3(a) |
|
(a) = Only 1 replicate. Replicate A discounted due to a failure of the trapping equipment. Trapping solutions show no 14CO2 was trapped.
DAT = Days After Treatment
LOD = Limit of Detection
NA = Not Applicable
Table 8. Summary of Characterisation / Identification of Radioactive Residues in Low Concentration Samples Expressed as % Applied Radioactivity
a. surface Water - low rate
Fraction |
Rep. |
Incubation time (DAT) |
|||||||
0 |
1 h |
3 h |
12 h |
2 |
5 |
29 |
60 |
||
Test substance |
A |
66.2 |
60.7 |
67.7 |
26.4 |
5.5 |
ND |
ND |
ND |
B |
68.5 |
67.4 |
65.5 |
27.0 |
3.9 |
ND |
ND |
ND |
|
Mean |
67.4 |
64.1 |
66.6 |
26.7 |
4.7 |
- |
- |
- |
|
M13 |
A |
ND |
ND |
ND |
ND |
2.2 |
2.2 |
6.2 |
6.3 |
B |
ND |
ND |
ND |
ND |
0.6 |
3.2 |
5.6 |
6.3 |
|
Mean |
- |
- |
- |
- |
1.4 |
2.7 |
5.9 |
6.3 |
|
M4 |
A |
26.2 |
26.8 |
30.5 |
63.9 |
77.5 |
75.1 |
81.4 |
73.2 |
B |
24.5 |
28.8 |
29.4 |
61.5 |
77.6 |
76.8 |
78.3 |
70.5 |
|
Mean |
25.4 |
27.8 |
30.0 |
62.7 |
77.6 |
76.0 |
79.9 |
71.9 |
|
Origin |
A |
3.7 |
1.9 |
ND |
5.2 |
7.5 |
13.1(a) |
4.6 |
6.8 |
B |
4.7 |
2.5 |
ND |
8.6 |
8.2 |
9.1(a) |
6.3 |
6.9 |
|
Mean |
4.2 |
2.2 |
- |
6.9 |
7.9 |
11.1 |
5.5 |
6.9 |
|
Apparatus Wash |
A |
1.1 |
1.0 |
1.1 |
0.9 |
1.7 |
2.2 |
4.4 |
2.9 |
B |
1.2 |
1.0 |
1.1 |
0.9 |
1.8 |
1.8 |
5.2(b) |
3.7 |
|
Mean |
1.2 |
1.0 |
1.1 |
0.9 |
1.8 |
2.0 |
4.8 |
3.3 |
|
14CO2 |
A |
NA |
<LOD |
<LOD |
<LOD |
<LOD |
<LOD |
0.6 |
16.2 |
B |
NA |
<LOD |
<LOD |
<LOD |
2.7 |
1.8 |
0.5 |
5.5 |
|
Mean |
- |
- |
- |
- |
1.4 |
0.9 |
0.6 |
10.8 |
|
(a) = Representative origin sample analysed. Confirmed as M4 (8.7-12.0% AR) and 2 minor components (< 0.6% AR) following HPLC analysis
(b) = no further analysis carried out on this sample as mean < 5% AR
DAT = Days After Treatment
LOD = Limit of Detection
NA = Not Applicable
ND = Not Detected
Table 9. Summary of Characterisation / Identification of Radioactive Residues in High Concentration Samples Expressed as % Applied Radioactivity
(a) Surface Water, high rate
Fraction |
Rep |
Incubation Time (DAT) |
|||||||
0 |
1 h |
3 h |
12 h |
2 |
5 |
30 |
60 |
||
Test substance (a) |
A |
93.2 |
89.6 |
90.9 |
91.0 |
85.9 |
47.1 |
1.5 |
ND |
B |
89.8 |
90.8 |
87.8 |
91.2 |
81.8 |
52.6 |
1.8 |
ND |
|
Mean |
91.5 |
90.2 |
89.4 |
91.1 |
83.9 |
49.9 |
1.7 |
- |
|
M18 (a) |
A |
ND |
ND |
ND |
ND |
ND |
3.7 |
19.4 |
31.3 |
B |
ND |
ND |
ND |
ND |
ND |
4.0 |
21.4 |
32.9 |
|
Mean |
- |
- |
- |
- |
- |
3.9 |
20.4 |
32.1 |
|
M13 |
A |
ND |
ND |
ND |
ND |
1.4 |
5.4 |
6.9 |
15.1 |
B |
ND |
ND |
ND |
ND |
1.1 |
4.5 |
8.1 |
12.6 |
|
Mean |
- |
- |
- |
- |
1.3 |
5.0 |
7.5 |
13.9 |
|
M4 |
A |
6.1 |
6.9 |
6.3 |
7.3 |
4.1 |
11.9 |
7.7 |
5.9 |
B |
5.3 |
7.0 |
8.7 |
7.9 |
4.4 |
12.5 |
7.6 |
7.3 |
|
Mean |
5.7 |
7.0 |
7.5 |
7.6 |
4.3 |
12.2 |
7.7 |
6.6 |
|
Peak at ca 21.1 min |
A |
ND |
ND |
ND |
ND |
1.9 |
6.4 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
4.7 |
ND |
3.0 |
|
Mean |
- |
- |
- |
- |
1.0 |
5.6 |
- |
1.5 |
|
Peak at ca 23.1 min |
A |
ND |
ND |
ND |
ND |
ND |
4.7 |
4.5 |
2.5 |
B |
ND |
ND |
ND |
ND |
ND |
6.7 |
3.2 |
2.5 |
|
Mean |
- |
- |
- |
- |
- |
5.7 |
3.9 |
2.5 |
|
Peak at ca 25.6 min |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
6.4 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
5.0 |
|
Peak at ca 31.1 min |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.9 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
5.8 |
ND |
|
Mean |
- |
- |
- |
- |
- |
- |
2.9 |
2.0 |
|
Sum of Minor Unknowns(b) |
A |
NA |
NA |
NA |
NA |
1.1 |
16.5 |
23.7 |
13.8 |
B |
NA |
NA |
NA |
NA |
NA |
27.7 |
25.7 |
14.1 |
|
Mean |
- |
- |
- |
- |
0.6 |
22.1 |
24.7 |
14.0 |
|
(a) = the test substance and M18 determined using TLC Solvent System 1. All other components determined using HPLC Method 1
(b) = No individual component greater than 4.4% AR
DAT = Days After Treatment
LOD = Limit of Detection
NA = Not Applicable
ND = Not Detected
(b) Apparatus Wash, high rate
Fraction |
Rep |
Incubation Time (DAT) |
|||||||
0 |
1 h |
3 h |
12 h |
2 |
5 |
30 |
60 |
||
Test substance |
A |
NA |
NA |
9.9 |
NA |
NA |
NA |
1.3 |
1.5 |
B |
NA |
NA |
NA |
NA |
NA |
NA |
2.2 |
1.7 |
|
Mean |
- |
- |
5.0 |
- |
- |
- |
1.8 |
1.6 |
|
M13 |
A |
NA |
NA |
2.1 |
NA |
NA |
NA |
ND |
ND |
B |
NA |
NA |
NA |
NA |
NA |
NA |
ND |
ND |
|
Mean |
- |
- |
1.1 |
- |
- |
- |
- |
- |
|
M4 |
A |
NA |
NA |
ND |
NA |
NA |
NA |
1.5 |
0.7 |
B |
NA |
NA |
NA |
NA |
NA |
NA |
1.6 |
0.4 |
|
Mean |
- |
- |
- |
- |
- |
- |
1.6 |
0.6 |
|
Peak at ca 31.1 min |
A |
NA |
NA |
0.4 |
NA |
NA |
NA |
0.5 |
0.9 |
B |
NA |
NA |
NA |
NA |
NA |
NA |
0.3 |
ND |
|
Mean |
- |
- |
0.2 |
- |
- |
- |
0.4 |
0.5 |
|
Sum of Minor Unknowns(a) |
A |
NA |
NA |
ND |
NA |
NA |
NA |
8.0 |
3.0 |
B |
NA |
NA |
NA |
NA |
NA |
NA |
4.3 |
4.6 |
|
Mean |
- |
- |
- |
- |
- |
- |
6.2 |
3.8 |
|
Apparatus Wash Not Analysed |
A |
1.5 |
0.8 |
NA |
0.7 |
0.9 |
2.9 |
NA |
NA |
B |
1.2 |
0.8 |
0.8 |
0.8 |
2.4 |
3.5 |
NA |
NA |
|
Mean |
1.4 |
0.8 |
0.4 |
0.8 |
1.7 |
3.2 |
- |
- |
|
(a) = No individual component greater than 1.8% AR
DAT = Days After Treatment
LOD = Limit of Detection
NA = Not Applicable
ND = Not Detected
(c). Total System (sum of surface water and apparatus wash), high rate
Fraction |
Rep |
Incubation Time (DAT) |
|||||||
0 |
1 h |
3 h |
12 h |
2 |
5 |
30 |
60 |
||
Test substance (a) |
A |
93.2 |
89.6 |
100.8 |
91.0 |
85.9 |
47.1 |
2.8 |
1.5 |
B |
89.8 |
90.8 |
87.8 |
91.2 |
81.8 |
52.6 |
4.0 |
1.7 |
|
Mean |
91.5 |
90.2 |
94.3 |
91.1 |
83.9 |
49.9 |
3.4 |
1.6 |
|
M18 (a) |
A |
ND |
ND |
ND |
ND |
ND |
3.7 |
19.4 |
31.3 |
B |
ND |
ND |
ND |
ND |
ND |
4.0 |
21.4 |
32.9 |
|
Mean |
- |
- |
- |
- |
- |
3.9 |
20.4 |
32.1 |
|
M13 |
A |
ND |
ND |
2.1 |
ND |
1.4 |
5.4 |
6.9 |
15.1 |
B |
ND |
ND |
ND |
ND |
1.1 |
4.5 |
8.1 |
12.6 |
|
Mean |
- |
- |
1.1 |
- |
1.3 |
5.0 |
7.5 |
13.9 |
|
M4 |
A |
6.1 |
6.9 |
6.3 |
7.3 |
4.1 |
11.9 |
9.2 |
6.6 |
B |
5.3 |
7.0 |
8.7 |
7.9 |
4.4 |
12.5 |
9.2 |
7.7 |
|
Mean |
5.7 |
7.0 |
7.5 |
7.6 |
4.3 |
12.2 |
9.2 |
7.2 |
|
Peak at ca 21.1 min |
A |
ND |
ND |
ND |
ND |
1.9 |
6.4 |
ND |
ND |
B |
ND |
ND |
ND |
ND |
ND |
4.7 |
ND |
3.0 |
|
Mean |
- |
- |
- |
- |
1.0 |
5.6 |
- |
1.5 |
|
Peak at ca 23.1 min |
A |
ND |
ND |
ND |
ND |
ND |
4.7 |
4.5 |
2.5 |
B |
ND |
ND |
ND |
ND |
ND |
6.7 |
3.2 |
2.5 |
|
Mean |
- |
- |
- |
- |
- |
5.7 |
3.9 |
2.5 |
|
Peak at ca 25.6 min |
A |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
3.6 |
B |
ND |
ND |
ND |
ND |
ND |
ND |
ND |
6.4 |
|
Mean |
- |
- |
- |
- |
- |
- |
- |
5.0 |
|
Peak at ca 31.1 min |
A |
ND |
ND |
0.4 |
ND |
ND |
ND |
0.5 |
4.8 |
B |
ND |
ND |
NA |
ND |
ND |
ND |
6.1 |
ND |
|
Mean |
- |
- |
0.2 |
- |
- |
- |
3.3 |
2.4 |
|
Sum of Minor Unknowns(a) |
A |
NA |
NA |
NA |
NA |
1.1 |
16.5 |
31.7 |
16.8 |
B |
NA |
NA |
NA |
NA |
NA |
27.7 |
30.0 |
18.7 |
|
Mean |
- |
- |
- |
- |
0.6 |
22.1 |
30.9 |
17.8 |
|
Apparatus Wash Not Analysed |
A |
1.5 |
0.8 |
NA |
0.7 |
0.9 |
2.9 |
NA |
NA |
B |
1.2 |
0.8 |
0.8 |
0.8 |
2.4 |
3.5 |
NA |
NA |
|
Mean |
1.4 |
0.8 |
0.4 |
0.8 |
1.7 |
3.2 |
- |
- |
|
14CO2 |
A |
NA |
0.2 |
0.1 |
0.4 |
0.4 |
0.7 |
0.1 |
0.4 |
B |
NA |
0.3 |
<LOD |
<LOD |
0.4 |
0.6 |
1.2 |
2.0 |
|
Mean |
- |
0.3 |
0.1 |
0.2 |
0.4 |
0.7 |
0.7 |
1.2 |
|
(a) =The test substance and M18 determined using TLC Solvent System 1. All other components determined using HPLC Method 1
(b) = No individual component greater than 4.4% AR
DAT = Days After Treatment
LOD = Limit of Detection
NA = Not Applicable
ND = Not Detected
Table 10. Summary of Characterisation / Identification of Radioactive Residues in Sterilised Samples Expressed as % Applied Radioactivity
(a). Sterilised samples analysed with low concentration [14C]-labelled test substance (10 µg/L)
Component |
Rep |
Incubation time (DAT) |
65 |
||
Test substance |
A |
2.6 |
B |
4.0 |
|
Mean |
3.3 |
|
M4 |
A |
77.1 |
B |
75.7 |
|
Mean |
76.4 |
|
M13 |
A |
ND |
B |
2.2 |
|
Mean |
1.1 |
|
Unidentified products |
A |
0.1 |
B |
4.7 |
|
Mean |
2.4 |
|
Origin |
A |
11.4(a) |
B |
4.0 |
|
Mean |
7.7 |
(a) = Experiments conducted, which demonstrated that this peak was mainly M4
DAT = Days after Treatment
ND = Not Detected
(b). Sterilised samples analysed with high concentration [14C]-labelled test substance (50 µg/L)
Component |
Rep |
Incubation Time (DAT) |
59 |
||
Test substance |
A |
22.4 |
B |
37.2(a) |
|
Mean |
22.4 |
|
M4 |
A |
8.9 |
B |
12.0(a) |
|
Mean |
8.9 |
|
M13 |
A |
3.4 |
B |
21.3(a) |
|
Mean |
3.4 |
|
Peak at ca 30 min |
A |
6.4 |
B |
ND(a) |
|
Mean |
6.4 |
|
Peak at ca 32 min |
A |
11.9 |
B |
ND(a) |
|
Mean |
11.9 |
|
Peak at ca 34 min |
A |
6.4 |
B |
ND(a) |
|
Mean |
6.4 |
|
Sum of Minor Unknowns |
A |
29.9(b) |
B |
ND(a) |
|
Mean |
29.9 |
DAT = Days after Treatment
ND = Not Detected
NA = Not Applicable
(a) = Sample with low mass balance postulated to be due to a treatment error; excluded from calculations
(b) = No individual component greater than 4.5% AR
Table 11. Summary of DegT50 and DegT90 Values
System |
Test concentration (µg/L) |
SFO |
|||||
DegT50 (days) |
DegT90 (days) |
k |
Chi2 |
R2 |
Prob > t |
||
Surface water |
10 |
0.4 |
1.4 |
0.516 |
10.7 |
0.9835 |
6.12 x 10-4 |
Surface water |
50 |
6 |
21 |
0.4657 |
4.8 |
0.9897 |
1.65 x 10-4 |
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
Chi2 = 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
Freshwater, DT50 = 6 d, 20 °C, OECD TG 309, Wicksted & Cochrane 2015
Freshwater sediment, DT50 = 9 d, 20 °C, OECD TG 308, aerobic, Wicksted 2015 and BBA Guideline Part IV, 5 -1, Oliver & Hurt 2002
Key value for chemical safety assessment
- Half-life in freshwater:
- 6 d
- at the temperature of:
- 20 °C
Whole System
- Half-life in whole system:
- 9 d
- at the temperature of:
- 20 °C
- Type of system:
- fresh water and sediment
Additional information
Table 1. DT50 values for the test substance in surface water under aerobic test conditions
Test system |
Test conditions |
Mineralisation / Non-extractable residues / Major metabolites (% applied) |
DT50 [d] – Kinetic model |
Author / Year |
Calwich Abbey Lake; 7.1 mg/L OC; pH 7.7; 10µg/L of test substance |
Aerobic incubation for 60 days at 20°C; Darkness; “Pelagic” test |
Mineralisation: 10.8 -1.2% after 60 d Main metabolites: M4 (max. 79.9 – 12.2% after 29 – 5 d), M13 (max. 6.3 – 13.9% after 60 - 60 d), M18 (max. 32.1% after 60d in high concentration system only) |
0.4 -SFO |
Wicksted & Cochrane / 2015 |
Calwich Abbey Lake; 6.54 mg/L OC; pH 8.0; 50µg/L of test substance |
Aerobic incubation for 60 days at 20°C; Darkness; “Pelagic” test; |
Mineralisation: 10.8 -1.2% after 60 d Main metabolites: M4 (max. 79.9 – 12.2% after 29 – 5 d), M13 (max. 6.3 – 13.9% after 60 - 60 d), M18 (max. 32.1% after 60d in high concentration system only) |
6 -SFO |
Wicksted & Cochrane / 2015 |
Table 2. DT50 values for the test substance in water-sediment systems under aerobic test conditions
Test system |
Test conditions |
Mineralisation / Non-extractable residues / Major metabolites (% applied) |
Comp. |
DT50 [d] – |
Author / Year
|
Swiss Lake Sediment: sandy loam, 1.9% OC, pH 5.3 Water: pH 6.97 |
Water:sed ratio 3:1 Aerobic incubation for 100 days at 20°C |
Miner.: max. 0.3% after 100 d Non-extr.: max. 29.6% after 100 d Maj. met.: M18 (max. 26.2% after 29 d), M4 (max. 11.4% after 29 d) |
Water
Total system |
10 – SFO
9 – SFO |
Wicksted / 2015 |
Calwich Abbey Sediment: silt loam, 4.9% OC, pH 7.4 Water: pH 7.75 |
Water:sed ratio 3:1 Aerobic incubation for 100 days at 20°C |
Miner.: max. < 0.1% after 100 d Non-extr.: max. 65.2% after 100 d Maj. met.: M18 (max. 36.3% after 14 d), M17 (max. 11.7% after 14d), M19 (max. 9.5% after 29 d), M4 (max. 46.5% after 7 d) |
Water
Total system |
3 – SFO
3 – SFO |
Wicksted / 2015 |
Emperor Lake Sediment: sandy loam, 3.2% OC, pH 5.6 Water: pH 7.4 |
Water:sed. ratio of 4:1 Aerobic incubation for 103 days at 20°C, 30 µg/L
|
Miner.: max. 0.4% 100 DAT Non-extr.: max. 68.9% 100 DAT Maj. met.: M18 (max. 10.1% in water, 7 DAT) |
Water
Total system |
59.4 h – SFO
59.4 h - SFO |
Oliver & Hurt / 2002
|
Bury pond Sediment: sandy clay loam, 2.4% OC, pH 7.9 Water: pH 7.9 |
Water:sed. ratio of 4:1 Aerobic incubation for 103 days at 20°C, 30 µg/L
|
Miner.: max. 0.6% 100 DAT Non-extr.: max. 67.2% 100 DAT Maj. met.: M18 (max. 8.9% in water, 7 DAT) |
Water
Total system |
20.1 h – SFO
20.1 h - SFO |
Oliver & Hurt / 2002
|
Table 3. DT50 values for the test substance in water-sediment systems under anaerobic test conditions
Test system |
Test conditions |
Mineralisation / Non-extractable residues / Major metabolites (% applied) |
Comp. |
DT50 [h] – |
Author / Year
|
Swiss Lake Sediment: sandy loam, 1.9% OC, pH 5.3 Water: pH 6.97 |
Water:sed ratio 3:1
Anaerobic incubation for 100 days at 20°C |
Miner.: max. < 0.1% after 102 d Non-extr.: max. 24.5% after 102 d Maj. met.: M18 (max. 40.2% after 29d), M19 (max. 8.7 after 15 d), M4 (max. 10.1% after 29 d) |
Water
Total system |
5 – SFO
4 – SFO |
Wicksted / 2015 |
Calwich Abbey Sediment: silt loam, 4.9% OC, pH 7.4 Water: pH 7.75 |
Water:sed ratio 3:1
Anaerobic incubation for 100 days at 20°C |
Miner.: max. < 0.1% after 102 d Non-extr.: max. 38.6% after 102 d Maj. met.: M8 (max. 10.9% after 102 d), M18 (max. 41.4% after 14 d), M17 (max. 14.1% after 29 d), M19 (max. 8.4% after 14 d), M4 (max. 12.4% after 46 d) |
Water
Total system |
5 – SFO
4 – SFO |
Wicksted / 2015 |
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