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EPA Method 200.2:Sample preparation procedure for spectrochemical determination of total recoverable elements. Official Name: Sample preparation procedure for spectrochemical determination of total recoverable elements
Summary:Solid and aqueous samples are prepared in a similar manner for analysis. Nitric and hydrochloric acids are dispensed into a beaker containing an accurately weighed or measured, well mixed, homogeneous aqueous or solid sample. Aqueous samples are first reduced in volume by gentle heating. Then, metals and toxic elements are extracted from either solid samples or the undissolved portion of aqueous samples by covering the beaker with a watch glass and refluxing the sample in the dilute acid mixture for 30 minutes. After extraction, the solubilzed analytes are diluted to specified volumes with ASTM Type I water, mixed and either centrifuged or allowed to settle overnight before analysis. Diluted samples are to be analyzed by the appropriate mass and/or atomic spectrometry methods as soon as possible after preparation.
Scope:This method provides sample preparation procedures for the determination of total recoverable analytes in groundwaters, surface waters, drinking waters, wastewaters, and, with the exception of silica, in solid type samples such as sediments, sludges and soils.
Citation:Martin, T.D., Creed, J.T., and Brockhoff, C.A., 1994, Sample preparation procedure for spectrochemcial determination of total recoverable elements: U.S. Environmental Protection Agency Report, Revision 2.8, EMMC Version, 12 p.
Interferences:In sample preparation, contamination is of prime concern. The work area, including bench top and fume hood, should be periodically cleaned in order to eliminate environmental contamination.Chemical interferences are matrix dependent and cannot be documented previous to analysis.Boron and silica from the glassware will grow into the sample solution during and following sample processing. For critical determinations of boron and silica, only quartz and/or PTFE plastic labware should be used. When quartz beakers are not available for extraction of solid samples, to reduce boron contamination, immediately transfer an aliquot of the diluted extract to a plastic centrifuge tube for storage until time of analysis. A series of laboratory reagent blanks can be used to monitor and indicate the contamination effect.
QC Requirements:Each laboratory determining total recoverable elements is required to operate a formal quality control (QC) program. The minimum requirements of a QC program consist of an initial demonstration of laboratory capability, and the analysis of laboratory reagent blanks, fortified blanks and quality control samples as a continuing check on performance. The laboratory is required to maintain performance records that define the quality of data generated.Specific instructions on accomplishing the described aspects of the QC program are discussed in the analytical methods used.
Maximum Holding Time:2 weeks
Media:WATER
Subcategory:Sampling/Preparation
Concentration:Dependent on analytical method used.
Precision:Dependent on analytical method used.
Detection:Dependent on analytical method used.
Revision Number:Rev. 2.8, 1994, EMMC Version