Methods US EPA

SW-846 On-line, Method 3500B, Organic Extraction and Sample Preparation , 3000 Series Methods, US EPA Office of Sohd Waste, www.epa.gov/epaoswer/hazwaste/test/3xxx.htm, 1996. 

US EPA chromatography method US EPA methods Determination of trace elements in marine waters by online Sr +, Ba + Cd +, Co +, Cu +, Brines, seawater, marine... 

Polycyclic aromatic hydrocarbons (PAHs) are nonpolar analytes regulated by the EPA. One standard method, US EPA SW-846 Method 8310, dictates that an acetonitrile/water gradient on a Cig column be used. However, PAH solubility decreases rapidly as the ring number increases fiom naphthalene (two fused rings) to benzo[g,/i,/]perylene (six fused rings). Such solubility limitations are not a problem when alkane solvents are used. 

The P T technique is recommended as an extraction technique for VOCs in several standard methods (Table 23.3). The US EPA has proposed different standard protocols for the analysis of volatiles in water using P T. These methods can be used for most of VOCs that have boiling points below 200°C and are insoluble or slightly soluble in water. The type of sample matrix being analyzed determines the implemented configuration of the extraction technique. The 500 series EPA methods are addressed to potable waters, whereas the 600 series refer to analysis of wastewaters. The analytical methods for determining hazardous waste are known as the 8000 series methods (US EPA SW-846). 

The described isotope dilution method for the quantification of polychlorinated dioxins, furans and dioxin-hke polychlorinated biphenyls (dl-PCBs) follows the EPA 1613 Rev.B method (US EPA, 1994,1998a/b). The MID scheme on the accurate target masses typically uses isotope ratio qualifiers besides the specific retention time for all native dioxin/furan congeners, as well as for their specific labelled internal standards, one quantification mass and one ratio mass. The analytical setup for the high resolution GC-MS is given with the MID descriptor, as... 

Reprinted from Executive Summary of Chemical Warfare Agents and their Hydrolysis Products from the US EPA Standardized Analytical Methods and GC-MS Analytical Method for the Analysis of Chemical Warfare Agent Degradation Products listed in the EPA Standardized Analytical Methods US EPA, Theodore A. Haigh... 

Reference methods for criteria (19) and hazardous (20) poUutants estabHshed by the US EPA include sulfur dioxide [7446-09-5] by the West-Gaeke method carbon monoxide [630-08-0] by nondispersive infrared analysis ozone [10028-15-6] and nitrogen dioxide [10102-44-0] by chemiluminescence (qv) and hydrocarbons by gas chromatography coupled with flame-ionization detection. Gas chromatography coupled with a suitable detector can also be used to measure ambient concentrations of vinyl chloride monomer [75-01-4], halogenated hydrocarbons and aromatics, and polyacrylonitrile [25014-41-9] (21-22) (see Chromatography Trace and residue analysis). 

Method 1613 of US Environmental Protection Agency (US EPA) was used for the PCDD detection in the objects of environment (water, soil etc.). PCDD detection was done with the help of Polaris Q gas chromatograph/ mass spectrometer on mass-spectrum of electronic impact in the MS-MS mode. Division of isomer PCDD was carried out on a capillary column from the sintered quartz DB-5 MS (60 m x 0,25 mm, thickness of tape 0,25 p.m). The same device was used for detection of fungicides formulations active ingredients in soil. 

A method for determining the LOD and LOQ for water samples was proposed by the US EPA. This method has also been discussed by Roy-Keith Smith in his book titled Handbook of Environmental Analysis .The method has also been proposed by the US EPA in their guidelines for Assigning Values to Non-detected/Non-quantitied Pesticide Residues in Human Health Pood Exposure Assessments . ... 

MQL. This method has been described previously by the US EPA and by Smith ... 

Once the determinative or confirmatory method has been developed to take full advantage of the chemical properties of the analyte molecule, a study is necessary to prove that the method is valid. Criteria for method validation are outlined in guidelines from the US FDA, US EPA, and EU. A summary of the differences in regulatory requirements for method validation is provided in Table 3. The parameters addressed by all of the regulatory guidelines include accuracy, precision, sensitivity, specificity, and practicability. 

Table 3 Comparison of US FDA, US EPA, and EU Committee for Veterinary Medicinal Products (CVMP) method validation requirements...

The reader should consult US EPA for a complete description of the method requirements. 

Full acceptance of HPLC/MS methods by the US EPA OPP as enforcement methods occurred between 1998 and 2001. For example, in 1998, the EPA OPP accepted HPLC/MS (without MS/MS) methods as primary enforcement methods, and high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) only was suitable for confirmatory methods. However, in 2001, HPLC/MS/MS methods also became acceptable for primary enforcement. Table 4 summarizes the types of methods that were validated by the EPA OPP method validation program, for both food tolerance enforcement methods and environmental chemistry methods. 

In addition to HPLC/fluorescence, there are references to the use of both APCI and/or ESI with HPLC/MS for the determination of A/-methyl carbamate insecticides in a variety of matrices." Ongoing studies at the US EPA for the determination of /V-methyl carbamate insecticides in nine fmits and vegetables at the 1.0 ngg level are described below. The fruits and vegetables investigated were cranberries, peaches, blueberries, kiwi, carrots, tomatoes, potatoes, lettuce, and grapefmit juice. The purpose of including an account of this work is to illustrate why HPLC/MS/MS is the method of choice for residue work at the 1.0 ng g level, especially for difficult matrices. 

Other ways to minimize matrix effects include improving the sample cleanup, diluting the sample, using labeled internal standards, using standard addition, or using matrix-matched standards. The last approach, however, is not permitted for enforcement methods at present by the US EPA or the US Pood and Drug Administration... 

ASE is recognised as an official extraction method in US EPA SW-846 Method 3545 and has shown to be equivalent to standard EPA extraction technology in terms of recovery and precision. 

V. Lopez-Avila, Sonication and Soxhlet Extraction in Environmental Analysis Methods Comparison. EPA Report 600/X-93/010, US Environmental Protection Agency Environmental Monitoring Systems Laboratory, Las Vegas, NV (February 1993). 

A valuable source of up-to-date information is the proceedings of the biennial QSAR conferences. The QSAR 2002 conference proceedings have been edited by Breton et al. (2003). A set of critical reviews has been edited by Walker (2003). Of particular note is the collection of estimation methods developed by the Syracuse Research Corporation with US EPA support and available on the internet at www.syrres.com under estimation methods. ... 

Schumacher, B.A. 2002. Methods for the determination of total organic carbon in soils and sediments. US EPA Report, NCEA-C-1282, EMASC-001. 

US EPA (2000) Methods for measuring the toxicity and bioaccumulation of sediment-associated contaminants with freshwater invertebrates, 2nd edn. EPA 600/R-99/064. US EPA, Washington DC... 

A number of EIA theorists believe in incorporating formal RA methods into EIA as a way to cope with uncertainties, especially in impact prediction where a formal framework for ecological risk assessment (EcoRA) is already developed. It includes three generic phases problem formulation, analysis, and risk characterization followed by risk management. The analysis phase includes an exposure assessment and an ecological effects assessment (see, e.g., US EPA (1998)). 

US-EPA (1996) Office of Solid Waste and Emergency Response. Test methods for evaluating solid waste (SW-846)... 

The sustainable management of sediments, in addition to water, soil and sludge environmental matrices, in relation to surfactant regulations, is also an important and relevant issue. The US EPA has recently shown concern regarding the levels of surfactants in sediments and has thus released a Draft Contaminated Sediment Science Plan. In this draft, recommendations for the development of analytical methods and evaluations of the toxicity and risk assessment of Emerging endocrine disrupters like APEOs and their metabolites in sediment samples are outlined. 

Since the first description of the BMD approach in health risk assessment of chemicals, the method has been modified and extended by many others. Central in this work was a workshop organized by the International Life Science Institute (ILSl) and reported in Barnes et al. (1995) and a workshop organized by the US-EPA Risk Assessment Eomm resulting in a US-EPA report (US-EPA 1995). No consensus was reached at these workshops on which variation and extension of the BMD approach is most appropriate for the use in human health risk assessment. 

The adopted test guideline methods for repeated dose toxicity testing include a number of parameters relevant for the evaluation of a substance s immunotoxic potential. Furthermore, a specific test guideline for immunotoxicity has also been adopted by the US-EPA. These test methods are addressed in Section 4.7.3.1 and Tables 4.11 and 4.12. 

---