EPA-OGWDW/TSC: 556.1: Carbonyls by Fast GC/ECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Carbonyl Compounds in Drinking Water by Fast Gas Chromatography

Current Revision

Revision 1.0, September 1999

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-OGWDW/TSC

Citation

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

Brief Method 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 and Application

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

Applicable Concentration Range

5-40 ug/L.

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.

(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.

Quality Control 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.

Sample Handling

Grab samples must be collected in accordance with conventional sampling practices using amber glass containers with PTFE-lined screw caps or caps with PTFE-faced silicon septa and capacities of at least 30 mL. Dechlorinate with 15 mg of ammonium chloride or ammonium sulfate. To inhibit bacteriological decay of analytes, add 15 mg of copper sulfate pentahydrate prior to sample collection. After collection, seal the bottle and agitate by hand for 1 minute. Samples must be iced or refrigerated at 4^oC +/- 2^oC away from light until extraction. Extracts must be stored at 4^oC +/- 2^oC away from light in glass vials with PTFE-faced silicon-lined caps.

Maximum Holding Time

7 days; 14 days after extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 15 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Acetaldehyde(75-07-0) Acetaldehyde	0.180 ug/L	89% Rec (SL)	2.50 % RSD (SL)	5.00 ug/L
Benzaldehyde(100-52-7) Benzaldehyde	0.190 ug/L	90% Rec (SL)	4.10 % RSD (SL)	5.00 ug/L
Butanal(123-72-8) Butanal Butyraldehyde	0.090 ug/L	111% Rec (SL)	2.40 % RSD (SL)	5.00 ug/L
Cyclohexanone(108-94-1) Cyclohexanone	0.190 ug/L	124% Rec (SL)	3.20 % RSD (SL)	5.00 ug/L
Decanal(112-31-2) Decanal	0.460 ug/L	109% Rec (SL)	5.10 % RSD (SL)	5.00 ug/L
Formaldehyde(50-00-0) Formaldehyde	0.090 ug/L	114% Rec (SL)	1.90 % RSD (SL)	5.00 ug/L
Glyoxal(107-22-2) Ethanedial Glyoxal	0.390 ug/L	92% Rec (SL)	6.30 % RSD (SL)	5.00 ug/L
Heptanal(111-71-7) Heptanal	0.400 ug/L	102% Rec (SL)	5.00 % RSD (SL)	5.00 ug/L
Hexanal(66-25-1) Hexaldehyde Hexanal	0.100 ug/L	111% Rec (SL)	4.00 % RSD (SL)	5.00 ug/L
Methyl glyoxal(78-98-8) 2-Oxopropanal Methyl glyoxal Pyruvic aldehyde	0.260 ug/L	90% Rec (SL)	5.70 % RSD (SL)	5.00 ug/L
Nonanal(124-19-6) Nonanal	0.620 ug/L	100% Rec (SL)	4.60 % RSD (SL)	5.00 ug/L
Octanal(124-13-0) Octanal	0.220 ug/L	104% Rec (SL)	5.40 % RSD (SL)	5.00 ug/L
Pentanal(110-62-3) Pentanal Valeraldehyde	0.090 ug/L	111% Rec (SL)	2.90 % RSD (SL)	5.00 ug/L
Propanal(123-38-6) Propanal Propionaldehyde	0.110 ug/L	103% Rec (SL)	2.00 % RSD (SL)	5.00 ug/L
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A

Precision Descriptor Notes:	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 Level Note:	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.

Precision Descriptor Notes:

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 Level Note:

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	PDF/Link
Revision 1.0, September 1999

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EPA-OGWDW/TSC: 556.1: Carbonyls by Fast GC/ECD

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