EPA Method 552.3REV1.0

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EPA Method 552.3REV1.0:
Haloacetic Acids and Dalapon in Drinking Water by Microextraction, Derivitization, and GC-ECD. Official Name: Determination of Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid Microextraction, Derivitization, and Gas Chromatography With Electron Capture Detection

A 40 mL sample is adjusted to pH of 0.5 or less and extracted with 4 mL of either methyl tert-butyl ether (MTBE) or tert-amyl methyl ether (TAME) containing an internal standard (1,2,3-trichloropropane is recommended). Haloacetic acids that have been partitioned into the organic phase are converted to their methyl esters by addition of acidic methanol followed by heating for 2 hours. The solvent phase containing the methylated haloacetic acids is then separated from the acidic methanol by adding a concentrated aqueous solution of sodium sulfate. The extract is then neutralized with saturated solution of sodium bicarbonate and an aliquot of the solvent layer is analyzed by GC/ECD.

This method determines haloacetic acids and dalapon in drinking water by GC-ECD.

EPA Web site for Analytical Methods for Drinking Water

(A) Contamination (general): Interferences may be caused by contaminants in solvents, reagents (including sodium sulfate), glassware, and other sample processing apparatus that lead to discrete artifacts or elevated baselines. The ester of bromochloroacetic acid coelutes with a low-level interferent on both the primary and confirmation GC columns (it may be dimethyl sulfide from the sodium sulfate). Some lots of TAME contain interferants including one that coelutes with the ester of monochloroacetic acid. To minimize potential interferences, glassware must be thoroughly cleaned and blanks should be analyzed to test for contamination.(B) Matrix interferences: Matrix interferences may be caused by contaminants that are extracted from the sample and will vary from source to source.(C) Phthalate esters: Phthalate esters can pose serious interferences with the electron capture detector (ECD) so plastics should be avoided in the laboratory. In addition, exhaustive purification of glassware and reagents may be required.

QC Requirements:
Initial demonstration of accuracy (which must be + or - 30% of fortified value), precision (RSD must be

Maximum Holding Time:
14 days (sample); 21 days (MTBE extract); 28 days (TAME extract)



0.5 - 30 ug/L

Precision and accuracy were determined using 8 replicate analyses of fortified reagent water, and TAME for microextraction (see Table 6 of the Method). Additional data for TAME and MTBE are presented in the method.

Detection Limits (DLs) were determined from 7 determinations of replicate laboratory fortified blanks (LFB) containing analyte concentrations estimated to be near the Detection Limit. Extraction (using TAME) and analyses took place over a 3 day period. The procedure used, detailed in Section 9 of the method, is similar to that found in 40 CFR 136, Appendix B, but with the addition of a multi-day testing requirement. Additional data for MTBE are provided in the method.

Revision Number:
Revision 1.0, July 2003