EPA-NERL: 555: Chlorinated Acids in Water Using HPLC/UV

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Chlorinated Acids in Water By High Performance Liquid Chromatography, with a Photodiode Array Ultraviolet Detector

Current Revision

Revision 1.0, August 1992

Media

WATER

Instrumentation

High Performance Liquid Chromatography with Ultraviolet Detection

Method Subcategory

Organic

Method Source

EPA-NERL

Citation

Methods for the Determination of Organic Compounds in Drinking Water - Supplement II (EPA/600/R-92-129)

Brief Method Summary

A 100-mL water sample is adjusted to a basic pH with sodium hydroxide, shaken, and allowed to set for 1 hr to hydrolyze chlorinated esters. The sample is acidified with H₃PO₄, filtered, and the chlorinated acids are extracted from a 20-mL aliquot. The aliquot is pumped through a high performance liquid chromatography (HPLC) cartridge (containing C-18-silica), trapping the chlorinated acids. The concentrator cartridge is valved in-line with the C-18 analytical column following extraction. The acids are separated by HPLC and detected using an ultraviolet (UV) absorption spectrometer.

Scope and Application

This method determines certain chlorinated acids in ground water and finished drinking water.

Applicable Concentration Range

Interferences

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

(B) Reagent contamination: Use high purity reagents. NOTE: When purifying solvents by distillation stabilizers and preservatives are removed, making them potentially more dangerous and decreasing shelf-life.

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

Quality Control Requirements

Initial demonstration of laboratory capability, analysis of laboratory reagent blanks (LRBs), laboratory fortified samples (LFS), laboratory fortified blanks (LFBs), field reagent blanks (FRBs), and QC samples. A MDL for each analyte must also be determined.

Sample Handling

Grab samples must be collected in glass containers in accordance with conventional sampling practices; however, the bottle must not be prerinsed with sample before collection. Add hydrochloric acid (1:1) to the sample to produce a pH of 2. Dechlorinate the sample with the addition of 4-5 mg of sodium sulfite for each 100 mL of water. Store samples at 4^oC away from light until analysis.

Maximum Holding Time

14 days.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 20 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	1.300 ug/L	93% Rec (SL)	4.10 % RSD (SL)	10.00 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	1.300 ug/L	112% Rec (SL)	4.20 % RSD (SL)	10.00 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	1.900 ug/L	92% Rec (SL)	5.90 % RSD (SL)	10.00 ug/L
3,5-Dichlorobenzoic acid(51-36-5) 3,5-DCBA 3,5-Dichlorobenzoic acid Benzoic acid, 3,5-dichloro-	2.100 ug/L	94% Rec (SL)	6.70 % RSD (SL)	10.00 ug/L
4-Nitrophenol(100-02-7) 1-hydroxy-4-Nitrobenzene 4-Hydroxynitrobenzene 4-Nitrophenol Phenol, 4-nitro- p-Hydroxynitrobenzene p-Nitrophenol	1.200 ug/L	95% Rec (SL)	4.00 % RSD (SL)	10.00 ug/L
5-Hydroxydicamba(7600-50-2) 5-Hydroxydicamba Benzoic acid, 2,5-dichloro-3-hydroxy-6-methoxy Benzoic acid, 2,5-dichloro-3-hydroxy-6-methoxy- Dicamba, 5-hydroxy-	2.200 ug/L	132% Rec (SL)	7.00 % RSD (SL)	10.00 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	1.700 ug/L	104% Rec (SL)	1.70 % RSD (SL)	10.00 ug/L
Bentazon(25057-89-0) 3-(1-methylethyl)-1H-2,1,3-benzothiadiazin-4(3 Basagran Bendioxide Bentazon Bentazon (ANSI) Bentazone	4.600 ug/L	126% Rec (SL)	14.60 % RSD (SL)	10.00 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	3.100 ug/L	83% Rec (SL)	10.00 % RSD (SL)	10.00 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-	2.100 ug/L	104% Rec (SL)	6.60 % RSD (SL)	10.00 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)-	1.700 ug/L	108% Rec (SL)	5.40 % RSD (SL)	10.00 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-	1.500 ug/L	97% Rec (SL)	4.80 % RSD (SL)	10.00 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
MCPA(94-74-6) ((4-Chloro-o-tolyl)oxy)acetic acid 2,4-MCPA 2-Methyl-4-chlorophenoxyacetic acid 4-Chloro-o-toloxyacetic acid Acetic acid, (4-chloro-2-methylphenoxy)- Agroxon MCPA Mephanac Mephanac, Metaxon Metaxon Methoxone (4-Chloro-2-methylphenoxy) acetic acid Netazol Rhonox	0.800 ug/L	93% Rec (SL)	2.50 % RSD (SL)	10.00 ug/L
MCPP(93-65-2) 2-(2-Methyl-4-chlorophenoxy)propanoic acid 2-(2-Methyl-4-chlorophenoxy)propionic acid 2-(4-Chloro-2-methylphenoxy) propanoic acid 2-(4-Chloro-2-methylphenoxy)propionic acid Anicon B MCPP Mecoprop Mepro Methoxone Propanoic acid, 2-(4-chloro-2-methylphenoxy)-	1.700 ug/L	95% Rec (SL)	5.50 % RSD (SL)	10.00 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
Pentachlorophenol(87-86-5) PCP Penchlorol Penta Pentachlorophenol Phenol, pentachloro- Santophen I	1.600 ug/L	99% Rec (SL)	5.20 % RSD (SL)	10.00 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	0.500 ug/L	104% Rec (SL)	1.70 % RSD (SL)	10.00 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)	1.800 ug/L	90% Rec (SL)	5.80 % RSD (SL)	10.00 ug/L

Precision Descriptor Notes:	Precision and accuracy values were calculated using six to seven replicate analyses of fortified reagent water samples (20 mL sample volumes were used). Additional data are available in the method.
Detection Level Note:	MDLs were determined using the standard deviation of replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for (# of samples - 1) degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B.

Revision	PDF/Link
Revision 1.0, August 1992

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EPA-NERL: 555: Chlorinated Acids in Water Using HPLC/UV

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