Water Extraction >> Carpet Cleaning After A Flood

Wet bottom sediment was extracted overnight within a Soxhlet apparatus. Two aliquots of the sample extract were quantitatively injected into a polystyrene-divinylbenzene gel permeation column (GPC) andeluted with dichloromethane to remove sulfur and Carpet Cleaning After A Flood partially isolate the target analytes. 

Eluent from the first aliquot wasanalyzed for PAHs and alkyl-PAHs by capillary-column gaschromatography (GC) with detection by full-scan mass spectrometry (MS) or by selected ion monitoring MS. Nineteenparent PAHs, 10 specific alkyl-PAHs, and Carpet Cleaning After A Flood the homologousseries of alkyl-PAHs for 2- to 5-ringed PAH were determined.

Total PAH refers to the summation used by MacDonald andothers (2000) for the probable effect concentration (PEC),an SQG, and Carpet Cleaning After A Flood hereinafter is designated as ΣPAHSQG. 

Eluentfrom the second GPC aliquot was split into two fractions bycombined alumina/silica adsorption chromatography followed by Florisil adsorption chromatography for further cleanupof the second fraction. Both fractions Carpet Cleaning After A Flood were analyzed by dualcapillary-column GC with electron capture detection for the determination of the organochlorine pesticides and PCBs.

PCBs were quantified as individual Aroclor (1016/1242, 1254,or 1260) equivalents and as 27 specific congeners.Quality assurance for organic-compound analyses by these methods was provided by analyzing an environmental duplicate sample split at the laboratory, Carpet Cleaning After A Flood laboratory reagent blanks.

Spiked reagent samples with each set of 12 environmental samples, and by monitoring recovery of surrogatecompounds in all samples. Although the methods were thesame for street mud, suspended sediment, and Carpet Cleaning After A Flood bottom sediment, sample mass was much smaller for suspended-sediment samples, thus affecting laboratory reporting levels and precision and limiting the number of duplicates analyzed.

Van Metre and others (2004) reported that the median relativepercent difference (RPD) using these methods for sedimentcore samples for chlorinated hydrocarbons was 11.8 percentfor 41 lab duplicate samples and Carpet Cleaning After A Flood for PAHs was 11.9 percentfor 40 lab duplicate samples.

Urban Waste Indicator CompoundsThe UWI analytical method measures a diverse suiteof organic compounds that reflects urban non-point sourcesand wastewater inputs to surface waters (Kolpin and others,2002); Carpet Cleaning After A Flood methods for analysis of UWI compounds in sedimentwere developed only recently (Burkhardt, ReVello, and others,2005; Burkhardt, Zaugg, and others, 2006). 

The compoundsmeasured by the UWI method fall into four groups: PAHs andrelated compounds, fecal and sewage indicator compounds,industrial chemicals, and pesticides and other householdchemicals. Wet bottom sediment was extracted twice, Carpet Cleaning After A Flood usingisopropanol/water mixtures on a commercially available accelerated solvent extraction (ASE) system. 

These extracts werethen diluted and method compounds were extracted from thebuffer solution using solid-phase extraction (SPE) cartridges.A mixture of dichloromethane/diethyl ether was used to elutethe method compounds from the SPE cartridge and Carpet Cleaning After A Flood passed through a 1-gram Florisil SPE column. These SPE extractswere reduced in volume and fortified with internal injection standards. 

The sample extracts were analyzed for 61 compounds by capillary-column GC with detection by full-scan MS.The UWI compounds were reported as individual compounds except for the nonylphenols and Carpet Cleaning After A Flood octylphenols,which were reported as estimated concentrations because thereference standards are from technical mixtures. 

The ASE is amore vigorous extraction technique than the dichloromethane Soxhlet extraction used for the chlorinated hydrocarbons andPAHs. As a result, Carpet Cleaning After A Flood analytical results from the two methods arenot comparable. 

Quality assurance was provided by analyzing an environmental duplicate sample split at the laboratory,laboratory reagent blanks, and spiked reagent samples, and bymonitoring recovery of surrogate compounds in all samples.Burkhardt, ReVello, and Carpet Cleaning After A Flood others (2005) reported that themedian precision using this method for PAHs on a standardreference material was 102 ±11.1 percent. 

Median recovery forspiked sand samples included with environmental samples forall UWI compounds was 76 percent for this study. Althoughthe methods were the same for the street-mud, Carpet Cleaning After A Flood suspended sediment, and bottom-sediment samples, small sample massfor suspended-sediment samples affected laboratory reporting levels and precision and limited the number of duplicatesanalyzed. 

Five environmental duplicate samples analyzed forUWI compounds for this study had a median RPD of 22 percent for the 19 analyte pairings detected. An acceptable rangeof RPDs for this Carpet Cleaning After A Flood method has not been established because thisis a recently developed analytical method.

Current-Use PesticidesSediment samples were extracted with 25-percent acetonein dichloromethane in an ASE system at 100 °C under pressurized conditions (10,342 kilopascals). Resultant extracts weredried with sodium sulfate, reduced in volume, and Carpet Cleaning After A Flood exchangedto ethyl acetate using Kuderna-Danish distillation and nitrogengas evaporation. 

The extract was introduced to a graphitizedcarbon SPE column and Carpet Cleaning After A Flood eluted with a 50-percent dichloromethane in ethyl acetate solution. The eluent was reduced andthe analytes were further isolated from elemental sulfur byGPC using ethyl acetate mobile phase. 

The GPC fraction wasreduced and a procedural internal standard solution of perdeuterated PAHs was added to the extract before final solventreduction and Carpet Cleaning After A Flood exchange to toluene. 

Sixty-three analytes in theextract were determined by GC/MS operated in the selectedion monitoring mode using procedures described in Zaugg andothers (1995), Sandstrom and Carpet Cleaning After A Flood others (2001), and Madsen andothers (2003); 62 of the analytes were determined by thosefiltered-water methods.

Quality assurance for current-use pesticide analyses by these methods was provided by analyzing an environmental duplicate sample split at the laboratory, Carpet Cleaning After A Flood laboratory reagentblanks, and spiked reagent samples with each set of 3 to 20 environmental samples, and by monitoring recovery of surrogate compounds in all samples. 

Thirty of the 63 method analytes exhibited acceptable performance (between 60 and 120percent median recovery and Carpet Cleaning After A Flood no more than 25 percent relative standard deviation) in 21 reagent spikes. Concentrations ofthe 33 other analytes, if detected, are reported as estimatedbecause of greater bias or variability or recognized GC thermalinstability (Foreman and others, 2005). 

Median recovery was81 percent for all analytes in the five reagent spikes analyzedwith environmental samples for this study. Four environmental duplicate samples analyzed for current-use pesticides for this Carpet Cleaning After A Flood study had a median RPD of 9 percent for the six analyte pairings detected.

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