Method 552.2

Determination of Haloacetic Acids and Dalapon in Drinking Water by Liquid-Liquid Extraction, Derivatization and Gas Chromatography with Electron Capture Detection


This is a gas chromatographic (GC) method applicable to the determination of halogenated acetic acids (HAA's) in drinking water, ground water, raw source water and water at any intermediate treatment stage.  In addition, the chlorinated herbicide, Dalapon, can be determined using this method.

A 40mL sample is adjusted to pH < 0.5 and extracted with 4mL of methyl-tert-butyl-ether (MTBE).  The haloacetic acids are partitioned into the organic phase and converted to their methyl ester by addition of acidic methanol followed by slight heating.  The acidic extract is neutralized by a backextraction with a saturated solution of sodium bicarbonate.  The sample is analyzed by GC/ECD (electron capture detector).

 

 


(EPA: Office of Water)

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Method Data

Hold Times, Preservatives, Preps, Collection, Analytical & Documentation
Holding Time:   14 days from sample collection to analysis if sample have been preserved. 7 days from extraction to analysis if samples kept at 4°C and 14 days if kept at <-10°C.
Preservatives:   Add crystalline or granular ammonium chloride (NH4Cl), 5mg per 50mL container, to bottle prior to collection. Store samples at 4°C and keep away from light.
Required Preps:   50mL Amber glass bottle with Teflon-lined lid
Collection Method:   Grab sampling
Analytical Methodology:   GC/ECD
Documentation:   552.2

Analyte List*

Analyte Formula CAS Number Detection Limit
Dibromoacetic acid (DBAA)
C2H2Br2O2
631-64-1
0.2
 μg/L
Tribromoacetic acid (TBAA)
C2HBr3O2
75-96-7
1.5
 μg/L
Dalapon
C3H4Cl2O2
75-99-0
0.4
 μg/L
Trichloroethanoic acid (TCAA)
C2HCl3O2
76-03-9
0.2
 μg/L
Monobromoacetic acid (MBAA)
C2H3BrO2
79-08-3
0.2
 μg/L
Monochloracetic Acid (MCAA)
C2H3ClO2
79-11-8
0.6
 μg/L
Dichloroacetic acid (DCAA)
C2H2Cl2O2
79-43-6
0.24
 μg/L
Bromochloroacetic acid (BCAA)
BrClCHCOOH
5589-96-3
0.25
 μg/L
Bromodichloroacetic acid (BDCAA)
BrCl2CO2H
7113-314-7
0.4
 μg/L
Chlorodibromoacetic acid (CDBAA)
C2HBr2ClO2
5278-95-5
0.75
 μg/L

* The analytes and detection limits listed for each method represent the typical detection limits and analytes reported for that particular method. Keep in mind that analyte lists may vary from laboratory to laboratory. Detection limits may also vary from lab to lab and are dependent upon the sample size, matrix, and any interferences that may be present in the sample.