EPA Method 526

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EPA Method 526:
Determination of Selected Semi-Volatile Organic Compounds in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry.

Summary:
A 1-L sample is extracted using a solid phase extraction (SPE) cartridge. SVOCs trapped in the cartridge are eluted under vacuum using ethyl acetate and dichloromethane. The extract is dried by passing it though an anhydrous sodium sulfate column, and the dried extract is concentrated. The concentrations of SVOCs in the extract are measured using a capillary column gas chromatography (GC) system equipped with a mass spectrometer (MS) detector.

Scope:
This method determines certain semivolatile organic compounds (SVOCs) in raw water and finished drinking water.

Citation:
Methods for the Determination of Organic and Inorganic Compounds in Drinking Water, Volume 1 (EPA/815-R-00-014)

Interferences:
(A) Glassware contamination: Solvent rinse and bake glassware to minimize contamination.(B) Co-extracted interferences: Compounds that are co-extracted with analytes may interfere.(C) Reagents: Buffers and preservatives used may contain organic contaminants.(D) Benzophenone: Benzophenone and 1,2-diphenylhydrazine share similar spectra, and their chromatographic peaks must be resolved to accurately quantitate.(E) Sodium sulfate: Anhydrous sodium sulfate may sometimes have an interference that causes loss of prometon and tailing of phenol peaks. Replace the first meter of column and the deactivated glass inlet liner was required to regain performance after analyzing contaminated samples.(F) Contamination: Solid Phase Extraction (SPE) devices can introduce contaminants. (G) Carryover effects: Analytes may carry over to later runs.(H) Silicone: Silicone may leach from septa, though silicone will usually not interfere.

QC Requirements:
Initial Demonstration of Capability (IDC), determination of the MDL, subsequent analysis in each batch of a Laboratory Reagent Blank (LRB), Continuing Calibration Check Standards (CCC), a Laboratory Fortified Blank (LFB), a Laboratory Fortified Sample Matrix (LFM), and either a Laboratory Fortified Sample Matrix Duplicate (LFMD) or a Field Duplicate Sample.

Maximum Holding Time:
14 days; 28 days after extraction.

Media:
WATER

Subcategory:
Organic

Concentration:
Not Provided.

Precision:
Precision and accuracy values were calculated using data obtained from seven replicate analyses of fortified reagent water, using the conditions specified in Table 4A of the method. A SDVB extraction disk was used. Additional data using different equipment are available in the method.

Detection:
MDLs represent performance on the primary column. Secondary columns used in validation of the method allowed for much lower MDLs for some analytes. Consult the method for more information. MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water (over a 3-day span) multiplied by the t-value for 6 degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B and Section 9.2.4 of the method.

Revision Number:
Revision 1.0, June 2000