EPA Method 200.13


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EPA Method 200.13:
Trace Elements by GFAA (w/ Preconcentration). Official Name: Determination of Trace Elements in Marine Waters by Offline Chelation Preconcentration with Graphite Furnace Atomic Absorption

Summary:
A sample is refluxed with nitric acid to solubilize elements. The solubilized sample is buffered using an on-line system, and is then preconcentrated using a chelating column with an iminodiacetate functionalized chelating resin. Anions and Group I and II metals are eluted from the column with ammonium acetate. The elements of interest are then eluted into a dilute nitric acid matrix. The concentrations of elements in the matrix are measured using a graphite furnace atomic absorption (GFAA) system.

Scope:
This method determines total recoverable elements in marine waters, including estuarine water, sea water, and brines.

Citation:
Methods for Determination of Chemical Substances in Marine and Estuarine Matrices - 2nd Edition (EPA/600/R-97/072)

Interferences:
(A) Blackbody radiation: Emission of blackbody radiation from the oven can interfere with absorbance measurements.(B) Elemental interferences: Spectral overlap of elemental absorptions can occur, but are relatively uncommon. Appropriate furnace temperature programs and high purity lamps can reduce interferences.(C) Matrix interferences: Some matrix components can inhibit the formation of free atoms.(D) Memory interferences: Analyte can carry over in the furnace and in the chelating columns between runs. Use low concentration samples to ensure that analytes do not carry over.(E) Loss of analyte: Low recoveries may be encountered if the sample contains chelating agents (humic/fulvic) or colloids that compete with the chelation column. Acid solubilization of the sample minimizes this interference.

QC Requirements:
Initial demonstration of laboratory capability and the periodic analysis of laboratory reagent blanks, fortified blanks, and other laboratory solutions as a continuing check on performance.

Maximum Holding Time:
6 months.

Media:
WATER

Subcategory:
Inorganic

Concentration:
Not Provided

Precision:
Precision and accuracy values were calculated using data from four replicate analyses of fortified certified seawater (NASS-3).

Detection:
MDL procedure is equivalent to the procedure at 40 CFR part 136, Appendix B. MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level (3.14). Detailed instructions for how MDLs are determined are found in Section 9.2.4 of the Method.

Revision Number:
Revision 1.0, September 1997

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