Jean M. Morrison

Laboratory data from testing parameters of EPA Method 3060A on Soils Contaminated with Chromium or Processing Residue

It has been shown that EPA Method 3060A does not adequately extract Cr(VI) from solids containing chromium ore processing residue (COPR). We systematically tested modifications to prescribed parameters of EPA 3060A towards improving extraction efficiency of Cr(VI) from NIST SRM 2701, a standard COPR-contaminated soil from New Jersey (NJ). The alkaline extraction fluid leached Al, Si, and B from the prescribed borosilicate glass vessels which interfered with Cr(VI) extraction from COPR. The use of polytetrafluoroethylene (PTFE) vessels increased the extraction efficiency. Intensive grinding of NIST 2701 resulted in the extraction of 730±30 mg kg-1 Cr(VI), which is substantially greater than the certified Cr(VI) value of 551±35 mg kg-1 but still less than the Cr(VI) value of ~3000 mg kg-1 previously determined by X-ray absorption near edge structure (XANES) spectroscopy. Increasing the extraction fluid to sample ratio also increased the efficiency of Cr(VI) extraction. Ratios similar to the 20 mL g-1 prescribed by 3060A resulted in low and highly variable extraction efficiencies. Ratios of 900 mL g-1 or greater resulted in relatively consistent extraction, yielding as much as ~950 mg kg-1 Cr(VI) from intensively ground NIST 2701 after 2.25 hours of extraction. Increasing the extraction time to 48 hours resulted in up to 1274 mg kg-1.

Modifications to EPA Method 3060A to Improve Extraction of Cr(VI) from Chromium Ore Processing Residue-Contaminated Soils

It has been shown that EPA Method 3060A does not adequately extract Cr(VI) from chromium ore processing residue (COPR). We modified various parameters of EPA 3060A toward understanding the transformation of COPR minerals in the alkaline extraction and improving extraction of Cr(VI) from NIST SRM 2701, a standard COPR-contaminated soil. Aluminum and Si were the major elements dissolved from NIST 2701, and their concentrations in solution were correlated with Cr(VI). The extraction fluid leached additional Al and Si from the method-prescribed borosilicate glass vessels which appeared to suppress the release of Cr(VI). Use of polytetrafluoroethylene vessels and intensive grinding of NIST 2701 increased the amount of Cr(VI) extracted. These modifications, combined with an increased extraction fluid to sample ratio of ≥900 mL g-1 and 48-h extraction time resulted in a maximum release of 1274 ± 7 mg kg-1 Cr(VI). This is greater than the NIST 2701 certified value of 551 ± 35 mg kg-1 but less than 3050 mg kg-1 Cr(VI) previously estimated by X-ray absorption near edge structure spectroscopy. Some of the increased Cr(VI) may have resulted from oxidation of Cr(III) released from brownmillerite which rapidly transformed during the extractions. Layered-double hydroxides remained stable during extractions and represent a potential residence for unextracted Cr(VI).