USGS-NWQL: O-5543-05:  Wastewater compounds in sediment and soil by pressurized solvent extraction, solid-phase extraction, and capillary-column GC/MS

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Official Method Name
 Determination of Wastewater Compounds in Sediment and Soil by Pressurized Solvent Extraction, Solid-Phase Extraction, and Capillary-Column Gas Chromatography/Mass Spectrometry
Current Revision
Original method
Media
 SOILS/SEDIMENT
Instrumentation
 Gas Chromatography with Mass Spectrometry Detection
Method Subcategory
 Organic
Method Source
  USGS-NWQL
Citation
  Burkhardt, M.R., Zaugg, S.D., Smith, S.G., and ReVello, R.C., 2006, Determination of wastewater compounds in sediment and soil by pressurized solvent extraction, solid-phase extraction, and capillary-column gas chromatography/mass spectrometry: U.S. Geological Survey Techniques and Methods, book 5, chap. B2, 40 p.
Brief Method Summary
 Sediment samples are extracted using water/isopropyl alcohol on a pressurized solvent extraction system. Selected compounds in these extracts are isolated using a disposable, polypropylene SPE cartridge, which contains a PSDVB phase. Dry the SPE cartridges for 5 minutes though not exhaustively. Compounds of interest are eluted with a mixture of dichloromethane (DCM) and diethyl ether (DEE) at an 80:20 ratio, respectively. The DCM–DEE is also used to elute sorbed compounds from a Florisil/sodium sulfate SPE cartridge. Extract are evaporated down in a hood by using a gentle stream of nitrogen to a final volume of 1 mL. Compounds of interest in the concentrated extracts are determined using capillary-column gas chromatography/mass spectrometry (GC/MS). The concentrations of 20 out of 61 compounds initially will be reported as estimated with the “E” remark code for one of three reasons: (1) unacceptably low-biased recovery (less than 60 percent) or highly variable method performance (greater than 25 percent relative standard deviation), (2) reference standards prepared from technical mixtures, or (3) potential blank contamination. See Precision Descriptor Notes section for more information.
Scope and Application
 This method is suitable for determining many compounds typically associated with industrial and household wastewater as well as some that are known or suspected endocrine-disrupting compounds in microgram-per-kilogram concentrations in bed-sediment (stream and lake beds), aqueous suspended sediment, and soil samples.
Applicable Concentration Range
 Several thousand micrograms per kilogram without dilution corresponding to a calibration range up to 40 ng/uL as analyzed on the instrument.
Interferences
 Compounds that compete with or displace the compounds of interest from the SPE cartridge materials (PSDVB phase and Florisil) might cause interferences or low method recovery, or both. In addition, compound classes, such as humic and fulvic acids, might influence the extraction efficiency and because of the complex nature of sediment and soil samples, recoveries of compounds of interest might be reduced. Compounds that have gas-chromatographic retention times and characteristic ions with a mass-to-charge ratio identical to or similar to the compounds of interest might interfere, and again because of the complex nature of sediment and soil samples, often there are unknown compounds that might interfere. Phthalates, antioxidants, and preservatives in the SPE cartridge housing often contribute to low-concentration contamination. Samples, collection equipment, or SPE cartridges that are handled improperly also might become contaminated with soaps, caffeine, and fragrances. Precautions are necessary to avoid contamination during sample collection (see section 11.1, Field Sampling) because some method compounds are contained in commonly used commercial consumer products. Sample-collection protocols and cleaning procedures for field equipment (Radtke and others, 1998a, p. 57; 1998b, p. 11–13) need to be followed to reduce interferences.
Quality Control Requirements
 Stock standard solutions at 10,000 ng/uL, Intermediate method compound standard solution at 100 ng/uL, Surrogate spiking solution at 80 ng/uL, Method compound solution at 50 ng/uL, Spiking solution at 20 ng/uL, Polycyclic aromatic hydrocarbon (PAH) procedural internal standard solution at 100 ng/uL, Calibration solutions, field duplicates, matrix spikes, Third-party check solution, set blanks, set spikes, Continuing calibration solutions.
Sample Handling
 Ship all sediment samples on ice to the NWQL in 500- or 1,000-mL wide-mouth glass jars with lids lined with polytetrafluoroethylene (PTFE) via overnight service as soon as possible after collection. The amount of water in the container should be minimized. Allow adequate space for the water present in the sample to expand during freezing. If adequate space is not allowed, the glass container will break and the sample is susceptible to contamination or loss.
Maximum Holding Time
 One year at -20 degrees C.
Relative Cost
 Greater than $400
Sample Preparation Methods
 Accelerated solvent extraction (ASE) extraction
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