EPA Method 3060A

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EPA Method 3060A:
ALKALINE DIGESTION FOR HEXAVALENT CHROMIUM

Summary:
This method uses an alkaline digestion to solubilize both water-insoluble (with the exception of partial solubility of barium chromate in some soil matrices, see Reference 10.9) and water soluble Cr(VI) compounds in solid waste samples. The pH of the digestate must be carefully adjusted during the digestion procedure. Failure to meet the pH specifications will necessitate redigestion of the samples.

Scope:
Method 3060 is an alkaline digestion procedure for extracting hexavalent chromium [Cr(VI)] from soluble, adsorbed, and precipitated forms of chromium compounds in soils, sludges, sediments, and similar waste materials. To quantify total Cr(VI) in a solid matrix, three criteria must be satisfied: (1) the extracting solution must solubilize all forms of Cr(VI), (2) the conditions of the extraction must not induce reduction of native Cr(VI) to Cr(III), and (3) the method must not cause oxidation of native Cr(III) contained in the sample to Cr(VI). Method 3060 meets these criteria for a wide spectrum of solid matrices. Under the alkaline conditions of the extraction, minimal reduction of Cr(VI) or oxidation of native Cr(III) occurs. The addition of Mg2+ in a phosphate buffer to the alkaline solution has been shown to suppress oxidation, if observed. The accuracy of the extraction procedure is assessed using spike recovery data for soluble and insoluble forms of Cr(VI) (e.g., K Cr O and PbCrO ), coupled with measurement of ancillary soil properties, indicative of the 2 2 7 4 potential for the soil to maintain a Cr(VI) spike during digestion, such as oxidation reduction potential (ORP), pH, organic matter content, ferrous iron, and sulfides. Recovery of an insoluble Cr(VI) spike can be used to assess the first two criteria, and method-induced oxidation is usually not observed except in soils high in Mn and amended with soluble Cr(III) salts or freshly precipitated Cr(OH) .

Report Number:
SW-846 Ch 3.2