USEPA Methods

Brandt [200] has extracted tri(nonylphenyl) phosphite (TNPP) from a styrene-butadiene polymer using iso-octane. Brown [211] has reported US extraction of acrylic acid monomer from polyacrylates. Ultrasonication was also shown to be a fast and efficient extraction method for organophosphate ester flame retardants and plasticisers [212]. Greenpeace [213] has recently reported the concentration of phthalate esters in 72 toys (mostly made in China) using shaking and sonication extraction methods. Extraction and analytical procedures were carefully quality controlled. QC procedures and acceptance criteria were based on USEPA method 606 for the analysis of phthalates in water samples [214]. Extraction efficiency was tested by spiking blank matrix and by standard addition to phthalate-containing samples. For removal of fatty acids from the surface of EVA pellets a lmin ultrasonic bath treatment in isopropanol is sufficient [215]. It has been noticed that the experimental ultrasonic extraction conditions are often ill defined and do not allow independent verification. 

USEPA, Method 606 - Phthalate Ester. Federal Register 409 (209), 73-80 (1984). 

Eichelberger JW, Bellar TA, Donnelly JP, et al. 1990. Determination of volatile organics in drinking water with USEPA method 524.2 and the ion trap detector. J Chromatogr Sci 28 460-467. 

Precipitation titrations are typified by the titration of chloride with silver or vice versa. In this case, interferences with the precipitation reaction may occur because of components in the soil, and the soil itself may interfere with detection of the end point. Thus, complexation reactions are rarely applied directly to soil however, they can be applied to soil extracts. Common environmental titration methods described in the United States Environmental Protection Agency (USEPA) methods are summarized in Table 10.1 [1,2],... 

Cool and filter the sample (Whatman No. 41 filter paper or equivalent) into a 100-mL volumetric flask and dilute to 100 mL with water. This sample can be analyzed by AAS or ICP (adapted from USEPA Method 3050B see Reference 11). 

There is one case in environmental work where the methyl and methylene absorptions are useful and used. This is in the United States Environmental Protection Agency (USEPA) method for the determination of total recoverable petroleum hydrocarbons (TRPHs) in a soil or other extract. Here, a supercritical carbon dioxide extraction of a hydrocarbon-contaminated soil is made (EPA Method 3560). The extracted hydrocarbons are dissolved in... 

Determination of Organic Compounds in Drinking Water by Liquid- Solid Extraction and Capillary Column/Mass Spectrometry, USEPA Method 525.2, Rev. 2, USEPA, Cincinnati, OH, 1995. 

The results of these interlaboratory studies are reported in USEPA Method Validation Studies 14 through 24 (14). The data were reduced to four statistical relationships related to the overall study 1, multilaboratory mean recovery for each sample 2, accuracy expressed as relative error or bias 3, multilaboratory standard deviation of the spike recovery for each sample and 4, multilaboratory relative standard deviation. In addition, single-analyst standard deviation and relative standard deviation were calculated. 

Smith, G.A. and E.T. Heggs. 2001. Optimization of method parameters for the evaluation of USEPA method 524.2 using a Tekmar-Dohrmann 3100 purge and trap with GC/MS. ACS National Meeting Book of Abstracts 41 25-30. 

USEPA, Methods for Assessing Consumer Exposure to Chemical Substances, Volume 7, Report No. 560/5-85/007, Exposure Assessment Branch, Office of Pollution Prevention and Toxics, US Environmental Protection Agency, Washington, DC, USA, 1987. 

FDA approved 1998 for die following materials to be used in contact with food adhesive preservatives, 21CFR175.105 a rubber accelerator (up to 1.5% of weight of rubber), 21CFR177.2600 in the synthesis of slimicides for use in paper/paper-board, 21CFR176.300 an adjuvant in die manufacture of foamed plastics, 21CFR178.3010. Listed in 40CFR136.1 and USEPA Method 640 The Determination of Mercaptobenzothiazole in Municipal and Industrial Wastewaters. 

USEPA Method 1614 Brominated diphenyl ethers in water, soil, sediment, and tissue by HRGC/HRMS and USEPA Method 1614 Brominated diphenyl ethers in water, soil, sediment, and tissue by HRGC/HRMS. 

Table 1.2.5 USEPA methods content (USEPA, 1996a)...

While an attempt has been made to place some context on each extraction technique, it should also be noted that most of the techniques described have been validated by the United States Environmental Protection Agency (USEPA) in terms of standard methods. The current USEPA methods for the extraction of pollutants from solid matrices are shown in Table 7.3. It should be noted that the supercritical fluid extraction technique has three specific methods for a range of compounds of environmental importance, whereas other techniques have more general, non-specific methods. 

Table 7.3 Current USEPA methods for the extraction of organic pollutants from solid environmental samples... 

USEPA method Extraction technique Application Further comments... 

USEPA, Method 8310, Polynuclear aromatic hydrocarbons (high liquid chromatographic method), Method 8100, Polynuclear aromatic hydrocarbons, 1986. 

Table 3. Results of samples of Figs. 1 and 2 (according to USEPA method)...

Target analyte Target analytes are compounds that are required analytes in USEPA analytical methods. BTEX and PAHs are examples of petroleum related compounds that are target analytes in USEPA methods. 

Notes Values listed as fresh/weathered and aged exposure treatments. All values (mg kg-1, dry soil mass) are based on acetonitrile extractable concentrations in soil (USEPA Method 8330). NT = not tested. a Greatest concentrations tested. 

United States Environmental Protection Agency (USEPA), Method 8330 Nitroaromatics and Nitramines by High Performance Liquid Chromatography (HPLC), U.S. Environmental Protection Agency, Washington, DC, 2003, http //www.epa.gov/SW-846/pdfs/8330. pdf (accessed August 2008). 

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