EPA-OGWDW/TSC: 551.1: Chlorinated Compounds in Water Using GC-ECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Chlorinated Disinfection Byproducts, Chlorinated Solvents, and Halogenated Pesticides/Herbicides in Drinking Water by Liquid/Liquid Extraction and Gas Chromatography with Electron Capture Detection

Current Revision

Revision 1.0, 1995

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-OGWDW/TSC

Citation

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

Brief Method Summary

A 50-mL sample is extracted with 3-mL of MTBE or 5-mL of pentane. The concentrations of compounds in the extract are measured using a fused silica capillary column gas chromatography (GC) system equipped a linearized electron capture detector (ECD).

Scope and Application

This method determines certain chlorinated or halogenated compounds (disinfection byproducts, pesticides, herbicides, and solvents) in finished drinking water, drinking water during intermediate stages of treatment, and raw source water.

Applicable Concentration Range

Ranges differ for each analyte.

Interferences

(A) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse.

(B) Solvent contamination: Use high purity solvents, and test solvents to prevent contamination: Contamination of MTBE and pentane with chlorinated solvents (common occurrence) can be reduced by double distillation.

(C) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced using confirmation analysis.

(D) Endrin degradation: The splitless injector may cause endrin degradation. Endrin can break down by reacting with the active sites on the port sleeve.

(E) Phthalate interference: An unknown interference (probably phthalates) appears in retention windows of metribuzin, alachlor, cyanazine, and heptachlor. Seal containers and avoid sample contact with plastics.

Quality Control 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.

Sample Handling

Two sets of 60-mL vials must be prepared for sampling: one set for all target analytes except chloral hydrate with 100 mg/L of ammonium chloride as a dechlorinating agent and one set for the analysis of chloral hydrate using 100 mg/L of sodium sulfite as the dechlorinating agent. Ammonium chloride must also be used as the dechlorinating agent if samples are to be analyzed for haloacetonitriles, 1,1-dichloro-2-propanone, 1,1,1-trichloro-2-propanone, and chloropicrin.

All samples should be collected in duplicate. Overfill all bottles, making sure to leave no bubbles or headspace. Store samples at 4^oC until analysis.

Maximum Holding Time

14 days; extracts within 14 days.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 41 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
1,1,1-Trichloro-2-propanone(918-00-3) 1,1,1-Trichloro-2-propanone 1,1,1-Trichloro-propanone 2-Propanone, 1,1,1-trichloro-	0.010 ug/L	106% Rec (SL)	0.81 % RSD (SL)	5.00 ug/L
1,1,1-Trichloroethane(71-55-6) 1,1,1-Trichloroethane Baltana Chlorothene Ethane, 1,1,1-trichloro- Methyl chloroform TCEA	0.005 ug/L	130% Rec (SL)	12.35 % RSD (SL)	0.01 ug/L
1,1,2-Trichloroethane(79-00-5) 1,1,2-Trichloroethane Ethane, 1,1,2-trichloro- Vinyltrichloride	0.010 ug/L	89% Rec (SL)	3.27 % RSD (SL)	0.14 ug/L
1,1-Dichloroacetone(513-88-2) 1,1-Dichloro-2-propanone 1,1-Dichloroacetone 1,1-Dichloropropanone 2-Propanone, 1,1-dichloro- Dichloromethyl methyl ketone	0.002 ug/L	110% Rec (SL)	6.22 % RSD (SL)	0.01 ug/L
1,2,3-Trichloropropane(96-18-4) 1,2,3-Trichloropropane Allyl trichloride Glycerol trichlorohydrin Propane, 1,2,3-trichloro-	0.008 ug/L	88% Rec (SL)	1.95 % RSD (SL)	0.16 ug/L
1,2-Dibromoethane(106-93-4) 1,2-Dibromoethane Bromofume Dowfume EDB Ethane, 1,2-dibromo- Ethylene bromide Ethylene dibromide Glycol dibromide	0.008 ug/L	200% Rec (SL)	12.54 % RSD (SL)	0.01 ug/L
Alachlor(15972-60-8) 2-Chloro-N-(2,6-diethylphenyl)-N-(methoxymethy Acetanilide,2-chloro-2',6'-diethyl-n-(methoxymethyl)- Alachlor Alanex Lasso Metachlor Methachlor	0.025 ug/L	117% Rec (SL)	2.13 % RSD (SL)	0.33 ug/L
Atrazine(1912-24-9) 1,3,5-Triazine-2,4-diamine, 6-chloro-N-ethyl-N'-(1- ... 2-Chloro-4-(ethylamino)-6-(isopropylamino)-S-triazine 2-Chloro-4-(ethylamino)-6-(isopropylamino)-s-t 2-Chloro-4-ethylamino-6-isopropylamine-sym-triazine AAtrex Atratol 8P Atrazine Atrazine (ANSI) Bicep	0.082 ug/L	121% Rec (SL)	3.56 % RSD (SL)	0.63 ug/L
Bromacil(314-40-9) 5-Bromo-3-sec-butyl-6-methyluracil Borea Bromacil Bromacil (ANSI) Bromax Hyvar Uragon Urox "B" Urox 'B'	0.030 ug/L	105% Rec (SL)	10.05 % RSD (SL)	0.09 ug/L
Bromochloroacetonitrile(83463-62-1) Acetonitrile, bromochloro- Bromochloroacetonitrile Bromochloromethyl cyanide	0.002 ug/L	110% Rec (SL)	5.42 % RSD (SL)	0.01 ug/L
Bromodichloromethane(75-27-4) Bromodichloromethane Dichlorobromomethane Dichloromonobromomethane Methane, bromodichloro- Monobromodichloromethane	0.003 ug/L	120% Rec (SL)	7.50 % RSD (SL)	0.01 ug/L
Bromoform(75-25-2) Bromoform Methane, tribromo- Methenyl tribromide Tribromomethane	0.004 ug/L	180% Rec (SL)	8.12 % RSD (SL)	0.01 ug/L
Carbon tetrachloride(56-23-5) Benzinoform Carbon tetrachloride Methane tetrachloride Methane, tetrachloro- Perchloromethane Tetrachloromethane	0.002 ug/L	110% Rec (SL)	6.32 % RSD (SL)	0.01 ug/L
Chloral hydrate(302-17-0) 1,1,-Ethanediol, 2,2,2-trichloro- 1,1,1-Trichloro-2,2-ethanediol 1,1-Ethanediol, 2,2,2-trichloro- Chloral hydrate Chloralhydrate Trichloroacetaldehyde hydrate	0.005 ug/L	116% Rec (SL)	5.61 % RSD (SL)	0.03 ug/L
Chloroform(67-66-3) Chloroform Methane, trichloro- Trichloroform Trichloromethane	0.050 ug/L	102% Rec (SL)	1.30 % RSD (SL)	5.00 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	0.316 ug/L	134% Rec (SL)	13.93 % RSD (SL)	0.57 ug/L
DBCP(96-12-8) 1,2-Dibromo-3-chloropropane Chloro-1,2-dibromopropane,3- DBCP Dibromochloropropane Fumagon, Fumazone Nemabrom, Nemafume, Nemagon, Nematocide Nemagon Nematocide Propane, 1,2-dibromo-3-chloro-	0.009 ug/L	200% Rec (SL)	15.50 % RSD (SL)	0.01 ug/L
Dibromoacetonitrile(3252-43-5) Acetonitrile, dibromo- Dibromoacetonitrile Dibromocyanomethane	0.006 ug/L	160% Rec (SL)	12.78 % RSD (SL)	0.01 ug/L
Dibromochloromethane(124-48-1) Chlorodibromomethane Dibromochloromethane Methane, dibromochloro-	0.001 ug/L	110% Rec (SL)	4.55 % RSD (SL)	0.01 ug/L
Dichloroacetonitrile(3018-12-0) Acetonitrile, dichloro- Dichloroacetonitrile	0.001 ug/L	90% Rec (SL)	4.28 % RSD (SL)	0.01 ug/L
Endrin(72-20-8) 2,7:3,6-Dimethanonaphth[2,3-b]oxirene, 3,4,5,6,9,9- ... 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-oct 3,4,5,6,9,9-Hexachloro-1a,2,2a,3,6,6a,7,7a-octahydro ... Compound 269 Endrin Hexachloroepoxyoctahydro-endo,endo-dimethanonaphthalene Hexadrin Mendrin Nendrin	0.002 ug/L	144% Rec (SL)	2.57 % RSD (SL)	0.02 ug/L
Endrin aldehyde(7421-93-4) 1,2,4-Methenocyclopenta[c,d]pentalene-5- ... Endrin aldehyde	0.002 ug/L	105% Rec (SL)	2.25 % RSD (SL)	0.02 ug/L
Endrin ketone(53494-70-5) 2,5,7-Metheno-3H-cyclopenta[a]pentalen-3-one, 3b,4,5 ... Endrin ketone Keto-endrin	0.002 ug/L	100% Rec (SL)	5.14 % RSD (SL)	0.02 ug/L
Heptachlor(76-44-8) 1,4,5,6,7,8,8-Heptachlorotetrahydro-4,7-methanoindene Drinox Heptachlor Heptachlor [1,4,5,6,7,8,8-heptachloro-3a,4,7,7a- ... Heptachlor/Heptachlor epoxide (SARA 110) Heptachlorodicyclopentadiene Heptagran Heptamul Velsicol-104	0.081 ug/L	112% Rec (SL)	2.84 % RSD (SL)	0.31 ug/L
Heptachlor epoxide(1024-57-3) Heptachlor epoxide Velsicol 53-CS-17 Vesicol 53-CS-17	0.002 ug/L	114% Rec (SL)	1.64 % RSD (SL)	0.04 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
Hexachlorobenzene(118-74-1) Anticarie Benzene, hexachloro- Bunt-cure HCB Hexachlorobenzene Perchlorobenzene	0.001 ug/L	100% Rec (SL)	5.44 % RSD (SL)	0.01 ug/L
Hexachlorocyclopentadiene(77-47-4) 1,3-Cyclopentadiene, 1,2,3,4,5,5-hexachloro- HCCPD HCP Hexachloro-1,3-cyclopentadiene Hexachlorocyclo-1,3-pentadiene Hexachlorocyclopentadiene Perchlorocyclopentadiene	0.018 ug/L	100% Rec (SL)	31.81 % RSD (SL)	0.02 ug/L
Lindane(58-89-9) Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha Cyclohexane, 1,2,3,4,5,6-hexachloro-, (1-alpha, 2- ... HCH-gamma Hexachlorocyclohexane (gamma) Lindane Lindane ( gamma isomer of benzene hexachloride ) (99 ... gamma-BHC gamma-Benzenehexachloride gamma-HCH gamma-Hcch gamma-Hexachlorocyclohexane	0.004 ug/L	167% Rec (SL)	9.90 % RSD (SL)	0.01 ug/L
Methoxychlor(72-43-5) 1,1'-(2,2,2-Trichloroethylidene)bis[4-methoxybenzene] 1,1,1-Trichloro-2,2-bis(4-methoxyphenyl)ethane Benzene, 1,1'-(2,2,2-trichloroethylidene)bis[4-methoxy- Dimethoxy DDT Ethane, 1,1,1-trichloro-2,2-bis(p-methoxypheny Ethane, 1,1,1-trichloro-2,2-bis(p-methoxyphenyl)- Marlate Methoxcide Methoxychlor Metox p,p'-Methoxychlor p,p'DMDT	0.008 ug/L	90% Rec (SL)	4.85 % RSD (SL)	0.06 ug/L
Metolachlor(51218-45-2) 2-Chloro-N-(2-ethyl-6-methylphenyl)-N-(2-methoxy-4- ... 2-Chloro-N-(6-ethyl-o-tolyl)-N-(2-methoxy-1- ... 2-chloro-6'-ethyl-N-(2-methoxy-1-methylethyl)-o- ... Acetamide, 2-chloro-N-(2-ethyl-6-methylphenyl)-N-(2- ... Codal Cycle Dual Metelilachlor Metolachlor Metolachlor (ANSI)	0.024 ug/L	116% Rec (SL)	3.20 % RSD (SL)	0.22 ug/L
Metribuzin(21087-64-9) 4-Amino-6-(1,1-dimethylethyl)-3-(methylthio)-1 Bay 94337 Lexone Metribuzin Sencoral Sencorer	0.037 ug/L	161% Rec (SL)	12.45 % RSD (SL)	0.06 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
Simazine(122-34-9) 1,3,5-Triazine-2,4-diamine, 6-chloro-N,N'-diethyl- 2,4-bis(Ethylamino)-6-chloro-s-triazine 2-Chloro-4,6-bis(ethylamino)-1,3,5-triazine 2-Chloro-4,6-bis(ethylamino)-S-triazine 6-Chloro-N,N'-diethyl-1,3,5-triazine-2,4-diami 6-Chloro-N,N'-diethyl-1,3,5-triazine-2,4-diamine Aquazine Princep Radocon S-Triazine,2-chloro-4,6-bis(ethylamino)- Simadex, Simanex, Simazine (ANSI) Simazine	0.142 ug/L	127% Rec (SL)	5.95 % RSD (SL)	0.63 ug/L
TTHM(N-55743) TTHM Total Trihalomethanes	N/A	N/A	N/A
Tetrachloroethene(127-18-4) 1,1,2,2-Tetrachloroethene 1,1,2,2-Tetrachloroethylene Ethene, tetrachloro- Ethylenetetrachloride Perchloroethylene Perclene Tetrachloroethene Tetrachloroethylene	0.002 ug/L	120% Rec (SL)	5.04 % RSD (SL)	0.01 ug/L
Trichloroacetonitrile(545-06-2) Acetonitrile, trichloro- Trichloroacetonitrile Trichloromethyl cyanide Trichloromethylnitrile Tritox	0.002 ug/L	100% Rec (SL)	5.31 % RSD (SL)	0.01 ug/L
Trichloroethene(79-01-6) 1,1,2-Trichloroethene 1,1,2-Trichloroethylene Ethene, trichloro Ethinyl trichloride Ethylene trichloride Ethylene, trichloro- TCE Tri-clene Trichloroethene Trichloroethylene	0.002 ug/L	80% Rec (SL)	8.68 % RSD (SL)	0.01 ug/L
Trifluralin(1582-09-8) Commence Dinitro-n,n-dipropyl-4-(trimethylfluoro)benzenamine,2,6- Treflan Trifluoralin, Trifluraline Trifluralin Triflurex p-Toluidine, alpha, alpha, alpha-trifluoro-2,6	0.003 ug/L	118% Rec (SL)	3.89 % RSD (SL)	0.02 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 determined using single laboratory data from eight replicate analyses of reagent water fortified with the analytes of interest. NOTES: (1) Total trihalomethanes (TTHMs) is a regulatory parameter representing the sum of multiple trihalomethanes. See the data for specific trihalomethanes for performance information. (2) The samples were preserved with NH4Cl. Additional data is available in the method for samples preserved with Na2SO3, and for different matrix types and analyte concentrations.
Detection Level Note:	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.

Precision Descriptor Notes:

Precision and accuracy values were determined using single laboratory data from eight replicate analyses of reagent water fortified with the analytes of interest. NOTES: (1) Total trihalomethanes (TTHMs) is a regulatory parameter representing the sum of multiple trihalomethanes. See the data for specific trihalomethanes for performance information. (2) The samples were preserved with NH4Cl. Additional data is available in the method for samples preserved with Na2SO3, and for different matrix types and analyte concentrations.

Detection Level Note:

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.

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Revision 1.0, 1995

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EPA-OGWDW/TSC: 551.1: Chlorinated Compounds in Water Using GC-ECD

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