Prepared as part of the
Comprehensive Everglades Restoration Plan
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Purpose and Scope
Description of the South District Wastewater Treatment Plant
Methods of Investigation
Sampling and Processing Methods
Laboratory Analytical Methods
Organic Wastewater Compounds
Enzyme-Linked Immunosorbent Assays
Solid-Phase Extraction—Liquid Chromatography/Mass Spectrometry
Evaluation of Emerging Contaminants of Concern in Influent and Effluent
Dry-Season Low-Inflow Constituents
Wet-Season Average-Inflow Constituents
pConstituents Detected during High-Rate Disinfection/Chlorine Dioxide and Ultraviolet Pilot Tests
October 5th Sampling Event
October 20th Sampling Event
Concentration and Distribution of Constituents Detected in Composite Samples
Constituents Detected in Influent
Constituents Detected in Effluent
Comparison of Analytical Results from Composite and Discrete Samples
Analytical Results of Field Blanks, Equipment Blanks, and Duplicate Samples
Matrix Spike Recoveries
The Comprehensive Everglades Restoration Plan has identified highly treated wastewater as a possible water source for the restoration of natural water flows and hydroperiods in selected coastal areas, including the Biscayne Bay coastal wetlands. One potential source of reclaimed wastewater for the Biscayne Bay coastal wetlands is the effluent from the South District Wastewater Treatment Plant in southern Miami-Dade County. The U.S. Geological Survey, in cooperation with the Comprehensive Everglades Restoration Plan Wastewater Reuse Technology Pilot Project Delivery Team, initiated a study to assess the presence of emerging contaminants of concern in the South District Wastewater Treatment Plant influent and effluent using current wastewater-treatment methods.
As part of the study, 24-hour composite and discrete samples were collected at six locations (influent at plants 1 and 2, effluent pump, reuse train, chlorine dioxide unit, and ultraviolet pilot unit) at the plant during: (1) a dry-season, low-flow event on March 2-3, 2004, with an average inflow rate of 83.7 million gallons per day; (2) a wet-season, average-flow event on July 20-21, 2004, with an average inflow rate of 89.7 million gallons per day; and (3) high-rate disinfection tests on October 5 and 20, 2004, with average flow rates of 84.1 and 119.6 million gallons per day, respectively. During these four sampling events, 26, 27, 29, and 35 constituents were detected, respectively. The following transformations in concentration were determined in the waste stream: -100 to 180 percent at the effluent pump and -100 to 85 percent at the reuse train on March 2-3, 2004, and -100 to 1,609 percent at the effluent pump and -100 to 832 percent at the reuse train on July 20-21, 2004; -100 to -37 percent at the effluent pump, -100 to -62 percent at the reuse train, -100 to -56 percent at the chlorine dioxide unit, and -100 to -40 percent at the ultraviolet pilot unit on October 5, 2004; and -100 to -4 percent at the effluent pump, -100 to 17 percent at the reuse train, -100 to -40 percent at the chlorine dioxide unit, and -100 to -14 percent at the ultraviolet pilot unit on October 20, 2004.
Samples were tested for detection of household and industrial (organic) wastewater compounds, pharmaceutical compounds, antibiotic compounds, and hormones in influent. Two "known" endocrine disrupting compounds—17 beta-estradiol (E2) and diethoxynonylphenol— and four "suspected" endocrine-disrupting compounds—1,4-dichlorobenzene, benzophenone, tris(2-chloroethyl) phosphate, and tris(dichloroisopropyl) phosphate—were detected during these sampling events. Phenanthrene and indole showed the greatest concentration ranges and highest concentrations for the organic wastewater compounds. Acetaminophen showed the greatest concentration range and highest concentration, and warfarin showed the smallest concentration range for the pharmaceutical compounds. Sulfamethoxazole (a sulfonamide) showed the greatest concentration range and highest concentration, and sulfathiozole (also a sulfonamide) showed the smallest concentration range for the antibiotic compounds. Two hormones, 17 beta-estradiol (E2) and estrone (E1), were detected in influent.
Samples were also tested for detection of organic wastewater compounds, pharmaceutical compounds, antibiotic compounds, and hormones in effluent. Indole showed the greatest concentration range and highest concentration, and triphenyl phosphate showed the smallest concentration range for the organic wastewater compounds. Dehydronifedipine showed the greatest concentration range and highest concentration, and warfarin had the smallest concentration range for the pharmaceutical compounds. Anhydro-erythromycin (a macrolide degradation product) showed the greatest concentration range, and sulfadiazine (a sulfonamide) and tetracycline showed the lowest concentration ranges for the antibiotic compounds. One hormone, 17 beta-estradiol (E2), was detected in effluent.
A statistical approach using the Wilcoxon signed-ranks test was undertaken to determine if there were statistically significant differences at the 95-percent confidence level between concentrations from composite and discrete samples. Of the 83 constituents detected, only 3.5 percent showed any statistically significant differences at the 95-percent confidence level.
Quality-assurance samples were collected for all organic wastewater compounds and included field blanks, equipment blanks, a duplicate sample, and matrix spikes. Analytical results of field and (or) equipment blanks were less than the minimum reporting levels (MRLs) for aceptophenone, N,N-diethyl-meta-toluamide (DEET), and naphthalene. Phenol had a concentration greater than the MRL. One duplicate sample was collected for 63 organic wastewater compounds. The relative percent differences were not determined or estimated for 62 and 11 percent of the compounds, respectively, because of censored data and matrix interference; however, relative percent differences were estimated for 25 percent of the compounds because of data below the MRLs. Of the relative percent differences that were determined, values ranged from 0.0 to 97.
Quality-assurance samples were also collected for pharmaceutical compounds, antibiotic compounds, and hormones. Analytical results of field and (or) equipment blanks for pharmaceutical compounds had concentrations greater than the MRL for 1,7-dimethylxanthene, diphenhydramine, and fluoxetine. Four pharmaceutical compounds had concentrations less than the MRL including acetaminophen, diltiazem, thiabendazole, and trimethoprim. Lincomycin, ofloxacin, and tetracycline were the only antibiotic compounds with concentrations greater than the MRLs for equipment blanks. The hormone 17 beta-estradiol (E2) had concentrations greater than the MRL for field and equipment blanks.
Average matrix spike recoveries were determined for 55 organic wastewater compounds. Average spike recoveries for 22 compounds (40 percent) were outside of the expected spike recovery range, and 16 compounds (29 percent) were considered “estimated” because one or more values were below the MRLs because of matrix interference or multiple detection levels. Recoveries could not be determined for 22 compounds because of a predominance of censored data values and lack of recovery for two samples.
The enzyme-linked immunosorbent assay (ELISA) analyses for hormones were confirmed by liquid chromatography/mass spectrometry (LC/MS) results. For 17-beta estradiol (E2), the average concentration of spiked samples and the spiked minus unspiked samples was about twice as high for the ELISA tests as for the LC/MS results. For the estrone (E1) and ethenyl estradiol (EE2) analyses, the average concentrations for the spiked samples and spiked minus unspiked samples were similar.
Surrogate performance was analyzed for selected compounds. Results indicated that decafluorobiphenyl, caffeine C-13, bisphenol A-d3, and fluoranthene d-10 were all within expected surrogate recovery ranges, indicating acceptable laboratory extraction and processing procedures.
Lietz, A.C., and Meyer, M.T., 2006, Evaluation of emerging contaminants of concern at the South District Wastewater Treatment Plant based on seasonal events, Miami-Dade County, Florida, 2004: U.S. Geological Survey Scientific Investigations Report 2006-5240, 38 p.
For additional information, contact:
U.S. Geological Survey
3110 SW 9th Avenue
Ft. Lauderdale, FL 33315
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Last modified: Thursday, 01-Dec-2016 19:28:51 EST