EPA-OGWDW/TSC: 515.4: Chlorinated Acids by GCECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Chlorinated Acids in Drinking Water by Liquid-Liquid Microextraction, Derivitization, and Fast Gas Chromatography with Electron Capture Detection

Current Revision

Revision 1.0, April 2000

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 40-mL sample is adjusted to alkaline pH and is allowed to sit for one hour to hydrolyze derivatives. The sample is then washed with hexane:MTBE to clean the sample. The aqueous phase is acidified and extracted with MTBE. Chlorinated acids in the MTBE are converted to methyl esters using diazomethane. The concentrations of the derivatized chlorinated acids (now esters) in the extract are measured using a fast capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD).

Note: Method 515.4 calls for a solvent wash step after hydrolysis and prior to acidification and derivatization. Dacthal, the parent di-ester, does not hydrolyze, and is extracted in the wash step, leaving the mono- and di-acid metabolites to be measured.

Scope and Application

This method determines chlorinated acids in drinking waters.

Applicable Concentration Range

0.5-20 ug/L for a 40 mL sample was tested.

Interferences

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

(B) Sodium sulfate: Sodium sulfate often contains contaminants. Analyze blanks with sodium sulfate to determine if the sodium sulfate is contaminated.

(C) Co-extracted interferences: Compounds that are co-extracted with analytes may interfere. Some matrices tested contained an interference with Dalapon which was resolved by using as low initial temperature program.

(D) Phthalate ester interference: Avoid the use of plastics and use pure reagents to avoid contamination by these ubiquitous compounds.

Quality Control Requirements

Initial Demonstration of Capability (IDC), determination of MDL, subsequent analysis in each analysis batch of a Laboratory Reagent Blank (LRB), Continuing Calibration Check Standards (CCC), 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 amber glass containers with PTFE-lined screw caps and capacities of at least 40 mL. Dechlorinate sample with sodium sulfite (approximately 2 mg/40 mL of sample) prior to collection. After collection, seal the bottle and agitate by hand for 15 seconds. All samples should be iced during shipment and must not exceed 10^oC during the first 48 hours after collection. Samples stored in lab must be held at or below 6^oC, but not frozen, and protected from light until extraction. Extracts must be stored at or below 0^oC and protected form light in glass vials with PTFE-lined caps.

Maximum Holding Time

Extract samples with 14 days of collection.
Analyze samples within 21 days of extraction.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 21 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
2,4,5-T(93-76-5) 2,4,5-T 2,4,5-T Acid 2,4,5-Trichlorophenoxyacetic acid 2,4,5-trichloro-Acetic acid Acetic acid, (2,4,5-trichlorophenoxy)- Dacamine 4D Weedone	0.024 ug/L	96% Rec (SL)	7.30 % RSD (SL)	0.25 ug/L
2,4-D(94-75-7) 2,4-D 2,4-D Acid 2,4-D [acetic acid, (2,4-dichlorophenoxy)-1] 2,4-Dichlorophenoxyacetic acid, salts and este 2,4-Dichlorophenoxyacetic acid, salts and esters Acetic acid, (2,4-dichlorophenoxy)- Hedonal Trinoxol Weed-b-gone	0.055 ug/L	98% Rec (SL)	5.20 % RSD (SL)	1.00 ug/L
2,4-DB(94-82-6) 2,4-DB 2,4-Dichlorophenoxybutyric acid 4-(2,4-Dichlorophenoxy)butyric acid Butanoic acid, 4-(2,4-dichlorophenoxy)- Butoxone Butyrac Butyric acid, 4-(2,4-dichlorophenoxy)- Embutone Legumex Venceweed	0.246 ug/L	97% Rec (SL)	8.40 % RSD (SL)	1.00 ug/L
3,5-Dichlorobenzoic acid(51-36-5) 3,5-DCBA 3,5-Dichlorobenzoic acid Benzoic acid, 3,5-dichloro-	0.212 ug/L	117% Rec (SL)	16.00 % RSD (SL)	0.50 ug/L
Acifluorfen(50594-66-6) 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2- ... 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitr Acifluorfen Acifluorfen (ANSI) Benzoic acid, 5-[2-chloro-4-(trifluoromethyl)phenoxy ... Blazer Tackle	0.307 ug/L	77% Rec (SL)	5.90 % RSD (SL)	0.50 ug/L
Bentazon(25057-89-0) 3-(1-methylethyl)-1H-2,1,3-benzothiadiazin-4(3 Basagran Bendioxide Bentazon Bentazon (ANSI) Bentazone	0.064 ug/L	100% Rec (SL)	2.10 % RSD (SL)	1.00 ug/L
Chloramben(133-90-4) 3-Amino-2,5-dichlorobenzoic acid Amiben Chloramben Chloramben (ANSI) Chloramben [benzoic acid, 3-amino-2,5-dichloro] Vegiben	0.057 ug/L	90% Rec (SL)	9.00 % RSD (SL)	0.50 ug/L
DCPA Diacid(2136-79-0) Chlorthal DCPA Acid Metabolites DCPA Diacid Dachthal Acid Metabolites	0.113 ug/L	92% Rec (SL)	6.50 % RSD (SL)	0.50 ug/L
DCPA mono-acid degradate(887-54-7) DCPA mono-acid degradate Dacthal mono-acid degradate	N/A	N/A	N/A
Dacthal Acid Metabolites(N-55765) DCPA Acid Metabolites Dacthal Acid Metabolites	N/A	N/A	N/A
Dalapon(75-99-0) .alpha.,.alpha.-Dichloropropionic acid 2,2-Dichloropropanoic acid 2,2-Dichloropropionic Acid Dalapon Dalapon (ANSI) Dalapon, sodium salt Dichloropropionic acid,alpha,alpha- Propanoic acid, 2,2-dichloro- Propionic acid, 2,2-dichloro-	0.054 ug/L	108% Rec (SL)	2.20 % RSD (SL)	1.00 ug/L
Dicamba(1918-00-9) 3,6-Dichloro-2-methoxybenzoic acid 3,6-Dichloro-o-anisic acid Banex Banlen, Banvel Benzoic acid, 3,6-dichloro-2-methoxy- Dianate Dicamba Dicamba ( 3,6-dichloro-o-anisic acid ) Dicamba (3,6-Dichloro-2-methoxybenzoic acid) Mediban Methoxy-3,6-dichlorobenzoic acid,2-	0.032 ug/L	97% Rec (SL)	3.70 % RSD (SL)	0.50 ug/L
Dichlorprop(120-36-5) 2,4-DP 2-(2,4-Dichlorophenoxy)propionic acid 2[2,4-(Dichlorophenoxy)]-propanoic acid Cornox RK Dichloroprop Dichlorprop Hedonal DP Polytox Propanoic acid, 2-(2,4-dichlorophenoxy)- Propionic acid,2-(2,4-dichlorophenoxy)-	0.433 ug/L	95% Rec (SL)	5.70 % RSD (SL)	1.00 ug/L
Dinoseb(88-85-7) 2,4-Dinitro-6-sec-butylphenol 2-sec-Butyl-4,6-dinitrophenol Butaphene Dinitrobutyl phenol Dinoseb Dinoseb (ANSI) Phenol, 2-(1-methylpropyl)-4,6-dinitro- Phenol,2-sec-butyl-4,6-dinitro-	0.166 ug/L	103% Rec (SL)	6.70 % RSD (SL)	1.00 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
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
Pentachlorophenol(87-86-5) PCP Penchlorol Penta Pentachlorophenol Phenol, pentachloro- Santophen I	0.014 ug/L	76% Rec (SL)	7.40 % RSD (SL)	0.10 ug/L
Picloram(1918-02-1) 2-Pyridinecarboxylic acid, 4-amino-3,5,6-trichloro- 4-Amino-3,5,6-trichloro-2-pyridinecarboxylic a 4-Amino-3,5,6-trichloro-2-pyridinecarboxylic acid 4-Amino-3,5,6-trichloropicolinic acid Amdon Borolin Picloram Picolinic acid,4-amino-3,5,6-trichloro- Tordon	0.050 ug/L	92% Rec (SL)	2.60 % RSD (SL)	1.00 ug/L
Quinclorac(84087-01-4) Quinclorac	0.080 ug/L	106% Rec (SL)	9.30 % RSD (SL)	0.10 ug/L
Silvex(93-72-1) 2,4,5-TP 2,4,5-TP Acid 2,4,5-Trichlorophenoxypropionic acid 2-(2,4,5-Trichlorophenoxy)propionic acid Fenoprop Propanoic acid, 2-(2,4,5-trichlorophenoxy)- Propionic acid, 2-(2,4,5-trichlorophenoxy)- Silvex Silvex (ANSI)	0.033 ug/L	84% Rec (SL)	20.00 % RSD (SL)	0.25 ug/L

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 5 of the method. Additional data are available in the method.
Detection Level Note:	MDLs were determined using the standard deviation of 9 replicate analyses of an analyte-fortified reagent water (over a 3-day span) multiplied by the t-value for 8 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, April 2000

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EPA-OGWDW/TSC: 515.4: Chlorinated Acids by GCECD

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