EPA 3060A-1996
ALKALINE DIGESTION FOR HEXAVALENT CHROMIUM

Standard No.
EPA 3060A-1996
Release Date
1996
Published By
U.S. Environmental Protection Agency (U.S. EPA)
Status
Scope
1.1 Any reference in this method to "Method 3060" refers to this version of that method, and does not refer to previously published versions (e.g., in the Second Edition of this manual). When published as a new method to SW-846, a method's number does not include a letter suffix. Each time a method is revised and made a part of SW-846 update, it receives a suffix. However, a method reference found within the text of SW-846 methods always refers to the latest version of that method published in SW-846, even if the method number at that location does not include the appropriate letter suffix. 1.2 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(lll), and (3) the method must not cause oxidation of native Cr(lll) 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(lll) 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(Vl) (e.g., K;Cr,0, and PbCrO 4), coupled with measurement of ancillary soil properties, indicative of the 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(lll) salts or freshly precipitated Cr(OH)3. 1.3 The quantification of Cr(VI) in Method 3060 digests should be performed using a suitable technique with appropriate accuracy and precision, for example Method 7196 (colorimetrically by UV-VIS spectrophotometry) or Method 7199 (colorimetrically by ion chromatography (1C)). Analytical techniques such as 1C with inductively coupled plasma - mass spectrometric (ICP-MS) detection, high performance liquid chromatography (HPLC) with ICP-MS detection, capillary electrophoresis (CE) with ICP-MS detection, etc. may be utilized once performance effectiveness has been validated.



Copyright ©2024 All Rights Reserved