EPA Method 552.1


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EPA Method 552.1:
Determination of Haloacetic Acids and Dalapon in Drinking Water by Ion Exchange Liquid-Solid Extraction and Gas Chromatography with an Electron Capture Detector - Revision 1.0.

Summary:
A 100-mL volume of sample is adjusted to a slightly acidic pH and extracted with a preconditioned miniature anion exchange column or a liquid/solid extraction (LSE) disk. The acids and herbicides are eluted from the disk with small aliquots of acidic methanol and esterified directly in this medium after the addition of a small volume of methyl tert-butyl ether (MTBE) as co-solvent. The methyl esters are partitioned into the MTBE phase and identified and measured using a capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD).

Scope:
This method determines haloacetic acids the herbicide Dalapon in drinking water, ground water, raw source water, and water at any intermediate treatment stage.

Citation:
Methods for the Determination of Organic Compounds in Drinking Water - Supplement II (EPA/600/R-92-129)

Interferences:
(A) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.(B) Solvent contamination: Use high purity solvents. Background correct using a reagent blank when background concentrations exceed 0.1 ug/L (observed with bromochloroacetic acid).(C) Ion interferences: Sulfate concentrations above 200 mg/L lower recovery by interfering with the ion exchange process. Dilute sample to mitigate this interference.(D) Neutralization/Adsorption: Acid-rinse glassware and acidify sodium sulfate reagent to prevent loss of organic acids.(E) Organics: Organic acids, phenols, phthalate esters, and chlorinated compounds that can interfere and can be partially removed with a methanol wash of the column.(F) Contamination from sample carryover: Rinsing apparatus with MTBE between analyses can minimize contamination.(G) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by using confirmation analysis.

QC Requirements:
Initial demonstration of laboratory capability, determination of surrogate compound recoveries in each sample and blank, monitoring internal standard peak area or height in each sample and blank, analysis of laboratory reagent blanks (LRBs), laboratory fortified blanks (LFBs), laboratory fortified matrix samples, and QC samples. Additional QC practices are recommended. A MDL for each analyte must also be determined.

Maximum Holding Time:
28 days; extracts within 48 hours.

Media:
WATER

Subcategory:
Organic

Concentration:
Ranges differ depending on matrix and instrumentation used for detection.

Precision:
Precision and accuracy values calculated from the analyses of seven replicate fortified reagent water samples.

Detection:
MDLs were determined using the standard deviation of replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for (# of samples - 1) 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 1.0, August 1992

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