EPA Method 515.4

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EPA Method 515.4:
Chlorinated Acids by GCECD. Official Name: Determination of Chlorinated Acids in Drinking Water by Liquid-Liquid Microextraction, Derivitization, and Fast Gas Chromatography with Electron Capture Detection

A 40-mL sample is adjusted to alkaline pH and is allowed to sit for one hour to hydrolyze derivatives. The sample is then washed with hexane:MTBE to clean the sample. The aqueous phase is acidified and extracted with MTBE. Chlorinated acids in the MTBE are converted to methyl esters using diazomethane. The concentrations of the derivatized chlorinated acids (now esters) in the extract are measured using a fast capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD).Note: Method 515.4 calls for a solvent wash step after hydrolysis and prior to acidification and derivatization. Dacthal, the parent di-ester, does not hydrolyze, and is extracted in the wash step, leaving the mono- and di-acid metabolites to be measured.

This method determines chlorinated acids in drinking waters.

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

(A) Glassware contamination: Solvent rinse and bake glassware to minimize contamination.(B) Sodium sulfate: Sodium sulfate often contains contaminants. Analyze blanks with sodium sulfate to determine if the sodium sulfate is contaminated.(C) Co-extracted interferences: Compounds that are co-extracted with analytes may interfere. Some matrices tested contained an interference with Dalapon which was resolved by using as low initial temperature program.(D) Phthalate ester interference: Avoid the use of plastics and use pure reagents to avoid contamination by these ubiquitous compounds.

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

Maximum Holding Time:
Extract samples with 14 days of collection.Analyze samples within 21 days of extraction.



0.5-20 ug/L for a 40 mL sample was tested.

Precision and accuracy values were calculated using data obtained from seven replicate analyses of fortified reagent water, using the conditions specified in Table 5 of the method. Additional data are available in the method.

MDLs were determined using the standard deviation of 9 replicate analyses of an analyte-fortified reagent water (over a 3-day span) multiplied by the t-value for 8 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, April 2000

Test Description:
Chlirinated Acids in

Instrument used for this test: