EPA Method 556.1

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EPA Method 556.1:
Determination of Carbonyl Compounds in Drinking Water by Fast Gas Chromatography

Summary:
A 20-mL sample is adjusted to a slightly acidic pH, and the compounds of interest are derivatized by reacting them with PFBHA reagent for 2 hours with heat. The oxime derivatives are extracted from the sample using hexane. The extract is processed through an acid wash step. The concentrations of oxime derivatives (converted from compounds of interest) are measured using a fast gas chromatography (FGC) system equipped with an electron capture detector (ECD).

Scope:
This method determines certain carbonyl compounds in finished drinking water and raw source water.

Citation:
Methods for the Determination of Organic and Inorganic Compounds in Drinking Water, Volume 1 (EPA/815-R-00-014)

Interferences:
(A) Reagent water contamination: To reduce aldehyde contamination, expose water to UV light or distill with permanganate.(B) Equipment contamination: Use non-Latex gloves, minimize exposure of reagent and sample to air (formaldehyde source), and use polypropylene (not phenolic resin) caps.(C) Reagent contamination: Solvents may contain carbonyl compounds.(D) Glassware contamination: Solvent rinse and bake glassware to minimize contamination.(E) Co-extracted interferences: Compounds that are co-extracted with analytes may interfere.(F) Chlorinated waters: An compound eluting just prior to the acetaldehyde (E) isomer is found in many chlorinated and chloraminated waters. Quantify using acetaldehyde if this occurs.

QC Requirements:
Initial demonstration of laboratory capability (which includes calculation of the MDL), analysis of laboratory reagent blanks, laboratory fortified blanks, field reagent blanks, laboratory fortified sample matrices, and other QC samples.

Maximum Holding Time:
7 days; 14 days after extraction.

Media:
WATER

Subcategory:
Organic

Concentration:
5-40 ug/L.

Precision:
Precision and accuracy values were calculated using data from eight replicate analyses of fortified reagent water in a single laboratory. The reagent water used contained measurable background concentrations of formaldehyde, heptanal, nonanal, and propanal. Additional data are available in the method.

Detection:
MDLs represent performance on the primary column. Secondary columns used in validation of the method allowed for much lower MDLs for some analytes. MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water (over a 3-day span) multiplied by the t-value for 6 degrees of freedom at the 99% confidence level (3.14). Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B and Section 9.2.4 of the method.

Revision Number:
Revision 1.0, September 1999