EPA Method 3050B

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EPA Method 3050B:

For the digestion of samples, a representative 1-2 gram (wet weight) or 1 gram (dry weight) sample is digested with repeated additions of nitric acid (HNO ) and hydrogen peroxide 3 (H O ). For GFAA or ICP-MS analysis, the resultant digestate is reduced in volume while heating and then diluted to a final volume of 100 mL. For ICP-AES or FLAA analyses, hydrochloric acid (HCl) is added to the initial digestate and the sample is refluxed. In an optional step to increase the solubility of some metals, this digestate is filtered and the filter paper and residues are rinsed, first with hot HCl and then hot reagent water. Filter paper and residue are returned to the digestion flask, refluxed with additional HCl and then filtered again. The digestate is then diluted to a final volume of 100 mL.

This method has been written to provide two separate digestion procedures, one for the preparation of sediments, sludges, and soil samples for analysis by flame atomic absorption spectrometry (FLAA) or inductively coupled plasma atomic emission spectrometry (ICP-AES) and one for the preparation of sediments, sludges, and soil samples for analysis of samples by Graphite Furnace AA (GFAA) or inductively coupled plasma mass spectrometry (ICP-MS). The extracts from these two procedures are not interchangeable and should only be used with the analytical determinations outlined in this section. Samples prepared by this method may be analyzed by ICPAES or GFAA for all the listed metals as long as the detecion limits are adequate for the required end-use of the data. Alternative determinative techniques may be used if they are scientifically valid and the QC criteria of the method, including those dealing with interferences, can be achieved. Other elements and matrices may be analyzed by this method if performance is demonstrated for the analytes of interest, in the matrices of interest, at the concentration levels of interest.

Report Number:
SW-846 Ch 3.2