Microwave-Assisted Vapor-Phase Nitric Acid Digestion of Small Biological Samples for Inductively Coupled Plasma Spectrometry

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Abstract:

The applicability of microwave-assisted, vapor-phase nitric acid digestion of small biological samples in closed-vessel microwave systems is examined for the inductively coupled plasma atomic emission spectroscopy (ICP-AES) determination of 10 elements (Al, As, Ca, Cu, Cd, Fe, Mn, Mo, Pb, and Zn). A 1.8 mL quartz sample container geometry was optimized for the successful decomposition of 50 to 90 mg of powdered biological samples. Microwave energy was efficiently coupled by addition of 250 mu L of distilled deionized water to the sample. A single microwave-assisted, vapor-phase acid sample digestion was accomplished within 30 min (including cooling time) at ~ 1200 psi pressure and 450 W microwave power in a commercial pressurized microwave decomposition (PMD) system. Multiple microwave-assisted, vapor-phase acid digestions were achieved at moderately high pressure (400 to 480 psi) and 230 C with a second closed-vessel microwave apparatus. The results for 10 elements in biological standard reference materials agree well with the certified values.
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