EPA: 632: Carbamate and urea pesticides in municipal and industrial wastewater by HPLC with UV detection

Summary
Analytes
Revision
Data and Sites

Official Method Name

Method 632: The Determination of Carbamate and Urea Pesticides in Municipal and Industrial Wastewater

Current Revision

Original method, 1992

Media

WATER

Instrumentation

High Performance Liquid Chromatography with Ultraviolet Detection

Method Subcategory

Organic

Method Source

EPA

Citation

Method 632: The Determination of Carbamate and Urea Pesticides in Municipal and Industrial Wastewater

Brief Method Summary

A measured volume of sample, approximately 1 L, is extracted with methylene chloride using a separatory funnel. The methylene chloride extract is dried and concentrated to a volume of 10 mL or less. HPLC chromatographic conditions are described which permit the separation and measurement of the compounds in the extract by HPLC with a UV detector.

Scope and Application

This method covers the determination of carbamate and urea pesticides in municipal and industrial wastewater.

Applicable Concentration Range

Interferences

(A) Glassware contamination: Clean all glassware as soon as possible after use by thoroughly rinsing with the last solvent used in it. Follow by washing with hot water and detergent and thorough rinsing with tap and reagent water. Drain dry, and heat in an oven or muffle furnace at 400°C for 15 to 30 minutes. Do not heat volumetric ware. Thorough rinsing with acetone and pesticide-quality hexane may be substituted for the heating. After drying and cooling, seal and store glassware in a clean environment to prevent any accumulation of dust or other contaminants. Store inverted or capped with aluminum foil. (B) Reagent and solvent contamination: Use high-purity reagents and solvents. Purification of solvents by distillation in all-glass systems may be required. (C) Coextracted contaminants from the sample: The cleanup procedure in Section 11 can be used to overcome many of these interferences but specific samples may require additional cleanup approaches.

Quality Control Requirements

Matrx spikes, matrix duplicates, laboratory reagent blank, field duplicates, standard reference materials analysis,

Sample Handling

Grab samples: glass bottles, not prerinsed. Automated sampling: free as possible from plastic. Iced or refrigerated at 4°C until extraction.

Maximum Holding Time

Extraction within 7 days of collection; analysis within 40 days after extraction.

Relative Cost

Sample Preparation Methods

Extraction with methylene chloride with optional Florisil cleanup procedure.

This method has 21 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Aminocarb(2032-59-9) Aminocarb	N/A	N/A	N/A
Barban(101-27-9) 4-Chloro-2-butynyl m-chlorocarbanilate Barban Barban (ANSI) Carbamic acid, (3-chlorophenyl)-, 4-chloro-2-butynyl ... Carbamic acid, m-chloro, 4-chloro-2-butynyl es Carbamic acid, m-chloro, 4-chloro-2-butynyl ester Carbanilic acid, m-chloro-, 4-chloro-2-butynyl ester Carbyne	0.050 ug/L	98% Rec (SL)	4.10 % RSD (SL)	0.30 ug/L
Carbaryl(63-25-2) 1-Naphthyl methylcarbamate 1-Naphthyl-N-methylcarbamate Carbamic acid, methyl-, 1-naphthyl ester Carbaril Carbaryl Carbaryl (ANSI) Carbaryl [1-naphthalenol, methylcarbamate] Sevimol Sevin	0.020 ug/L	101% Rec (SL)	4.10 % RSD (SL)	0.10 ug/L
Carbofuran(1563-66-2) 2,3-Dihydro-2,2-dimethyl-7-benzofuranyl methylcarbamate Carbofuran Carbofuran (ANSI) Dihydro-2,2-dimethyl-7-benzofuranyl methylcarbamate,2,3- Euradan Furadan	3.200 ug/L	88% Rec (SL)	2.70 % RSD (SL)	37.00 ug/L
Chlorpropham(101-21-3) CIPC CIPC, Chloro-IPC Carbamic acid, (3-chlorophenyl)-, 1-methylethy Carbamic acid, (3-chlorophenyl)-, 1-methylethyl ester Chloro-IPC Chlorocarbanilic acid,m-, isopropyl ester Chloropropham, Chlorpropham Chlorpropham Furloe Isopropyl 3-chlorocarbanilate Isopropyl N-(3-chlorophenyl)carbamate Isopropyl-3-chlorocarbanilate Metoxon Preventol n-3-Chlorophenylisopropylcarbamate	0.030 ug/L	95% Rec (SL)	3.90 % RSD (SL)	0.20 ug/L
Diuron(330-54-1) Diuron Urea, N'-(3,4-dichlorophenyl)-N,N-dimethyl- (9CI)	0.009 ug/L	90% Rec (SL)	1.00 % RSD (SL)	10.00 ug/L
Fenuron(101-42-8) Fenuron Urea, N,N-dimethyl-N'-phenyl- (9CI)	N/A	N/A	N/A
Fenuron-TCA(4482-55-7) Fenuron-TCA	N/A	N/A	N/A
Fluometuron(2164-17-2) Fluometuron	11.100 ug/L	94% Rec (SL)	7.00 % RSD (SL)	50.00 ug/L
Linuron(330-55-2) Linuron	0.009 ug/L	95% Rec (SL)	3.40 % RSD (SL)	10.00 ug/L
Methiocarb(2032-65-7) 3,5-Dimethyl-4-(methylthio)phenol methylcarbamate 4-(Methylthio)-3,5-xylyl methylcarbamate Carbamic acid, methyl-, 4-(methylthio)-3,5-xyl Carbamic acid, methyl-, 4-(methylthio)-3,5-xylyl ester Mercaptodimethur Mesurol Methiocarb Phenol, 3,5-dimethyl-4-(methylthio)-, methylca Phenol, 3,5-dimethyl-4-(methylthio)-, methylcarbamate	0.020 ug/L	95% Rec (SL)	2.60 % RSD (SL)	0.20 ug/L
Methomyl(16752-77-5) Acetamidic acid, thio-N-[(methyl-carbamoyl)oxy Acetamidic acid, thio-N-[(methyl-carbamoyl)oxy]-, ... Dupont 1179 Insecticide 1179 Lannate Methomyl S-methyl-n-((methylcarbamoyl)oxy)thioacetimidate	8.900 ug/L	74% Rec (SL)	2.40 % RSD (SL)	100.00 ug/L
Mexacarbate(315-18-4) 4-(Dimethylamino)-3,5-dimethylphenyl methylcarbamate Carbamic acid, methyl-, 4-dimethylamino-3,5-xy Carbamic acid, methyl-, 4-dimethylamino-3,5-xylyl ester Dimethylamino-3,5-xylyl methylcarbamate,4- Mexacarbate Mexacarbate (ANSI) Mexacarbole Phenol, 4-(di-methylamino)-3,5-dimethyl, methy Zectran	0.520 ug/L	96% Rec (SL)	3.50 % RSD (SL)	4.00 ug/L
Monuron(150-68-5) Monuron	0.003 ug/L	97% Rec (SL)	1.70 % RSD (SL)	0.05 ug/L
Monuron-TCA(140-41-0) Monuron-TCA	N/A	N/A	N/A
Neburon(555-37-3) Neburon Urea, N-butyl-N'-(3,4-dichlorophenyl)-N-methyl- (9CI)	0.012 ug/L	96% Rec (SL)	6.60 % RSD (SL)	0.05 ug/L
Oxamyl(23135-22-0) 2-o-Methylcarbamoyl monoxime DPX 1410 Oxamyl Thioxamyl Vydate Vydate L	9.200 ug/L	87% Rec (SL)	8.40 % RSD (SL)	100.00 ug/L
Propham(122-42-9) Carbamic acid, phenyl-, 1-methylethyl ester (9CI) Propham	0.070 ug/L	88% Rec (SL)	5.90 % RSD (SL)	0.30 ug/L
Propoxur(114-26-1) 2-Isopropoxyphenyl-n-methylcarbamate Aprocarb Baygon Blattenex Isocarb N-methyl-2-isopropoxyphenylcarbamate Phenol, 2-(1-methylethoxy)-, methylcarbamate Propoxur Propoxur [phenol, 2-(1-methylethoxy)-, methylcarbamate] Sendran, Suncide Unden o-Isopropoxyphenyl methylcarbamate	0.110 ug/L	95% Rec (SL)	1.70 % RSD (SL)	550.00 ug/L
Siduron(1982-49-6) Siduron	N/A	N/A	N/A
Swep(1918-18-9) Methyl (3,4-dichlorophenyl)carbamate Swep	N/A	N/A	N/A

Precision Descriptor Notes:	The average percent recoveries and standard deviations of the percent recoveries were determined on 4 to 7 replicates at a single laboratory.
Detection Level Note:	The method detection limit (MDL) is defined as the minimum concentration of a substance that can be measured and reported with 99% confidence that the value is above zero. The MDL concentrations were obtained using reagent water or river water.

Revision	PDF/Link
Original method, 1992

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EPA: 632: Carbamate and urea pesticides in municipal and industrial wastewater by HPLC with UV detection

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