EPA Method 506

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EPA Method 506:
Determination of Phthalate and Adipate Esters in Drinking Water by Liquid-Liquid Extraction or Liquid-Solid Extraction and Gas Chromatography with Photoionization Detection - Revision 1.1.

Summary:
Samples are extracted using liquid/liquid extraction (LLE) or liquid/solid extraction (LSE). For LLE, a 1-L sample is extracted with methylene chloride followed by hexane using a glass separatory funnel, and the final extract is dried and reduced to a to a volume of 1-mL. For LSE a measured volume of sample is extracted with a LSE cartridge or disk, and eluted using acetonitrile and methylene chloride (or pure methylene chloride), and the eluent/extract is reduced to a volume of 1-mL. The concentrations of esters in the extracts are measured using a gas chromatography (GC) system equipped with a photoionization detector (PID).

Scope:
This method determines certain phthalate and adipate esters in drinking water.

Citation:
Methods for the Determination of Organic Compounds in Drinking Water - Supplement III (EPA/600/R-95-131)

Interferences:
(A) Phthalate ester interference: Avoid the use of plastics and use pure reagents to avoid contamination by these ubiquitous compounds.(B) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.(C) Reagent contamination: Use high purity reagents.(D) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by cleaning the extract.(E) Variable solvents: Use the same solvent for each analysis.

QC Requirements:
Initial demonstration of laboratory capability, followed by analysis of laboratory reagent blanks (LRB), laboratory fortified blanks (LFB), laboratory fortified sample matrix (LFM), and quality control samples (QCS). A MDL for each analyte must also be determined. Additional quality control practices are recommended.

Maximum Holding Time:
Samples must be extracted within 14 days. Extracts can be held for an additional 14 days prior to analysis.

Media:
WATER

Subcategory:
Organic

Concentration:
Ranges differ for each analyte depending on matrix and instrumentation.

Precision:
Precision and accuracy values determined using single laboratory data from six to seven replicate measurements of fortified reagent water. NOTE: Data represents performance using liquid-liquid extraction. Performance data for liquid-solid extraction also are available.

Detection:
MDLs were determined using the standard deviation of 6 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 5 degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B.

Revision Number:
Revision 1.1, 1995