EPA Method 552.2

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EPA Method 552.2:
Determination of Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid Extraction, Derivatization and Gas Chromatography with Electron Capture Detection - Revision 1.0.

A 40-mL sample is adjusted to a highly acidic pH and extracted with methyl tert-butyl ether (MTBE). The haloacetic acids that have been partitioned into the MTBE phase are then converted to their methyl esters by the addition of acidic methanol followed by slight heating. The acidic extract is neutralized by a back extraction with a saturated solution of sodium bicarbonate. The concentrations of acids in the extract are measured using a capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD).

This method determines haloacetic acids in drinking water, ground water, raw source water, and water at any intermediate treatment stage.

Methods for the Determination of Organic Compounds in Drinking Water - Supplement III (EPA/600/R-95-131)

(A) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.(B) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced using confirmation analysis.(C) Memory Interferences: Carryover may occur whenever high and low concentration samples are analyzed in sequence. Rinse the sample syringe and associated equipment with MTBE between samples. Also, unusually concentrated samples should be followed by one or more injections of MTBE to ensure accurate values for the next sample.(D)Bromochloroacetic acid coelutes with an interferant (probably dimethyl sulfide) on the DB-1701 confirmation column. Quantitative confirmation can be performed by manual integration that includes only the peak area of the target ester.(E) Methylation using acidic methanol results in a partial decarboxylation of tribromoacetic acid. Therefore, a substantial peak for bromoform will be observed in the chromatograms. Its elution does not interfere with other analytes.

QC Requirements:
Laboratory performance check standard, initial demonstration of laboratory capability, method detection limit (MDL) determination, analysis of laboratory reagent blanks (LRBs), continuing calibration check standard, laboratory fortified sample matrices, field duplicates, and monitoring surrogate and/or internal standard peak response in each sample and blank. Additional QC practices may be added.

Maximum Holding Time:
14 days; extracts within 7 days if stored at 4oC or 14 days if stored at -10oC or less.



Ranges differ depending on matrix and instrumentation used for detection.

Precision and accuracy values were calculated using data from seven replicate analyses of fortified reagent water. Additional data are available in the method.

MDLs were determined using the standard deviation of 8 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 7 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, 1995

Test Description:
Haloacetic Acids & D

Report Number:

Instrument used for this test: