EPA-NERL: 555:  Chlorinated Acids in Water Using HPLC/UV

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Determination of Chlorinated Acids in Water By High Performance Liquid Chromatography, with a Photodiode Array Ultraviolet Detector
Current Revision
Revision 1.0, August 1992
High Performance Liquid Chromatography with Ultraviolet Detection
Method Subcategory
Method Source
  Methods for the Determination of Organic Compounds in Drinking Water - Supplement II (EPA/600/R-92-129)
Brief Method 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 and Application
This method determines certain chlorinated acids in ground water and finished drinking water.
Applicable Concentration Range

(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.

Quality Control 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.

Sample Handling

Grab samples must be collected in glass containers in accordance with conventional sampling practices; however, the bottle must not be prerinsed with sample before collection. Add hydrochloric acid (1:1) to the sample to produce a pH of 2. Dechlorinate the sample with the addition of 4-5 mg of sodium sulfite for each 100 mL of water. Store samples at 4oC away from light until analysis.

Maximum Holding Time

14 days.

Relative Cost
$201 to $400
Sample Preparation Methods