EPA Method 555


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EPA Method 555:
Determination of Chlorinated Acids in Water by High Performance Liquid Chromatography with a Photodiode Array Ultraviolet Detector - Revision 1.0.

Summary:
A 100-mL water sample is adjusted to a basic pH with sodium hydroxide, shaken, and allowed to set for 1 hr to hydrolyze chlorinated esters. The sample is acidified with H3PO4, filtered, and the chlorinated acids are extracted from a 20-mL aliquot. The aliquot is pumped through a high performance liquid chromatography (HPLC) cartridge (containing C-18-silica), trapping the chlorinated acids. The concentrator cartridge is valved in-line with the C-18 analytical column following extraction. The acids are separated by HPLC and detected using an ultraviolet (UV) absorption spectrometer.

Scope:
This method determines certain chlorinated acids in ground water and finished drinking water.

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) Reagent contamination: Use high purity reagents. NOTE: When purifying solvents by distillation stabilizers and preservatives are removed, making them potentially more dangerous and decreasing shelf-life.(C) Neutralization/Adsorption: Acid-rinse glassware and acidify sodium sulfate reagent to prevent loss of organic acids.(D) 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, analysis of laboratory reagent blanks (LRBs), laboratory fortified samples (LFS), laboratory fortified blanks (LFBs), field reagent blanks (FRBs), and QC samples. A MDL for each analyte must also be determined.

Maximum Holding Time:
14 days.

Media:
WATER

Subcategory:
Organic

Precision:
Precision and accuracy values were calculated using six to seven replicate analyses of fortified reagent water samples (20 mL sample volumes were used). Additional data are available in the method.

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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