EPA-OGWDW/TSC: 526: SVOCs in Water by GCMS

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Selected Semivolatile Organic Compounds in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

Current Revision

Revision 1.0, June 2000

Media

WATER

Instrumentation

Gas Chromatography with Mass Spectrometry 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 1-L sample is extracted using a solid phase extraction (SPE) cartridge. SVOCs trapped in the cartridge are eluted under vacuum using ethyl acetate and dichloromethane. The extract is dried by passing it though an anhydrous sodium sulfate column, and the dried extract is concentrated. The concentrations of SVOCs in the extract are measured using a capillary column gas chromatography (GC) system equipped with a mass spectrometer (MS) detector.

Scope and Application

This method determines certain semivolatile organic compounds (SVOCs) in raw water and finished drinking water.

Applicable Concentration Range

Not Provided.

Interferences

(A) Glassware contamination: Solvent rinse and bake glassware to minimize contamination.

(B) Co-extracted interferences: Compounds that are co-extracted with analytes may interfere.

(D) Benzophenone: Benzophenone and 1,2-diphenylhydrazine share similar spectra, and their chromatographic peaks must be resolved to accurately quantitate.

(E) Sodium sulfate: Anhydrous sodium sulfate may sometimes have an interference that causes loss of prometon and tailing of phenol peaks. Replace the first meter of column and the deactivated glass inlet liner was required to regain performance after analyzing contaminated samples.

(F) Contamination: Solid Phase Extraction (SPE) devices can introduce contaminants.

(G) Carryover effects: Analytes may carry over to later runs.

(H) Silicone: Silicone may leach from septa, though silicone will usually not interfere.

Quality Control Requirements

Initial Demonstration of Capability (IDC), determination of the MDL, subsequent analysis in each batch of a Laboratory Reagent Blank (LRB), Continuing Calibration Check Standards (CCC), a Laboratory Fortified Blank (LFB), a Laboratory Fortified Sample Matrix (LFM), and either a Laboratory Fortified Sample Matrix Duplicate (LFMD) or a Field Duplicate Sample.

Sample Handling

Grab samples must be collected in accordance with conventional sampling practices using a 1 liter or 1 quart amber or clear glass bottle fitted with PTFE-lined screw-caps. The following preservation reagents are added to each sample bottle prior to shipment to the field: L-Ascorbic Acid - 0.10 g/L, EDTA - 0.35 g/L), Diazolidinyl Urea - 1.0 g/L, Tris(hydroxymethyl)aminomethane - 0.47 g/L (First component of pH 7 buffer mixture), Tris(hydroxymethyl)aminomethane hydrochloride - 7.28 g/L (Second component of pH 7 buffer mixture.
Sampling equipment, including automatic samplers, must be free of plastic tubing, gaskets, and other parts that may leach interfering analytes into the sample. Fill sample bottles, taking care not to flush out the preservation reagents and then cap the bottles and agitate by hand until preservatives are dissolved. Samples must not exceed 10^oC during the first 48 hours after collection. Samples stored in the lab must be held at or below 6^oC until extraction, but should not be frozen. Extracts should be kept at 0^oC or less.

Maximum Holding Time

14 days; 28 days after extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 16 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
1,2-Diphenylhydrazine(122-66-7) 1,2-Diphenylhydrazine Hydrazine, 1,2-diphenyl Hydrazobenzene n,n'-Bianiline	0.028 ug/L	121% Rec (SL)	2.50 % RSD (SL)	0.50 ug/L
2,4,6-Trichlorophenol(88-06-2) 2,4,6-Trichlorophenol Dowicide 2S Phenachlor Phenol, 2,4,6-trichloro-	0.010 ug/L	136% Rec (SL)	2.30 % RSD (SL)	0.50 ug/L
2,4-Dichlorophenol(120-83-2) 1,3-dichloro-4-Hydroxybenzene 2,4-Dichlorophenol DCP Dichlorophenol, 2,4- Phenol, 2,4-dichloro-	0.010 ug/L	114% Rec (SL)	1.90 % RSD (SL)	0.50 ug/L
Acetochlor(34256-82-1) 2'-Ethyl-6'-methyl-N-(ethoxymethyl)-2-chloroacetanilide Acenit Acetal Acetamide, 2-chloro-N-(ethoxymethyl)-N-(2-ethy Acetochlor Acetochlor (ANSI) Chloracetanilide Harness Nevirex	0.015 ug/L	124% Rec (SL)	2.90 % RSD (SL)	0.50 ug/L
Cyanazine(21725-46-2) 2-((4-Chloro-6-(ethylamino)-1,3,5-triazin-2-yl)amino)-2-methylpropanenitrile 2-((4-Chloro-6-(ethylamino)-s-triazin-2-yl)amino)-2-methylpropionitrile Bladex Cyanazine Fortrol Payze	0.025 ug/L	153% Rec (SL)	2.50 % RSD (SL)	0.50 ug/L
Diazinon(333-41-5) Alfa-tox Basudin Diazide, Diazinone, Diazitol, Diazol Diazinon Diazinon (ANSI) Diazitol Dimpylate Dipofene Spectracide	0.015 ug/L	101% Rec (SL)	2.50 % RSD (SL)	0.50 ug/L
Disulfoton(298-04-4) Disulfoton Disulphoton Disyston Disyston S Thiodemeton o,o-Diethyl-s-(2-eththioethyl)phosphorodithioate	0.020 ug/L	105% Rec (SL)	2.40 % RSD (SL)	0.50 ug/L
Fonofos(944-22-9) Difonate Dyfonate Dyphonate Fonofos O-ethyl S-phenyl ethylphosphonodithioate O-ethyl-s-phenyl ethyldithiophosphonate Phosphonodithioic acid, ethyl-, O-ethyl S-phenyl ester Stauffer N-2790	0.020 ug/L	104% Rec (SL)	2.00 % RSD (SL)	0.50 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
Nitrobenzene(98-95-3) Benzene, nitro- EPA Pesticide Chemical Code 056501 Essence of mirbane Essence of myrbane Mirbane oil Mononitrobenzene Nitrobenzene Nitrobenzol Oil of mirbane Oil of myrbane RCRA waste number U169	0.015 ug/L	106% Rec (SL)	3.80 % RSD (SL)	0.50 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Organochlorine pesticides(E-12851) Organochlorine pesticides Pesticides, organochlorine	N/A	N/A	N/A
Organophosphate pesticides(E-12873) Organophosphate pesticides Organophosphorus pesticides Pesticides, organophosphate	N/A	N/A	N/A
Prometon(1610-18-0) 2,4-bis(Isopropylamino)-6-methoxy-S-triazine 2,4-bis(Isopropylamino)-6-methoxy-sym-triazine 2,6-Diisopropylamino-4-methoxytriazine Gesafram 50 Methoxypropazine Pramitol Prometon Prometon (ANSI) Prometon(pramitol) Prometone	0.035 ug/L	138% Rec (SL)	2.30 % RSD (SL)	0.50 ug/L
Terbufos(13071-79-9) Counter Terbufos	0.017 ug/L	111% Rec (SL)	2.70 % RSD (SL)	0.50 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 obtained from seven replicate analyses of fortified reagent water, using the conditions specified in Table 4A of the method. A SDVB extraction disk was used. Additional data using different equipment 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. Consult the method for more information. 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. 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 obtained from seven replicate analyses of fortified reagent water, using the conditions specified in Table 4A of the method. A SDVB extraction disk was used. Additional data using different equipment 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. Consult the method for more information. 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. 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, June 2000

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EPA-OGWDW/TSC: 526: SVOCs in Water by GCMS

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