EPA-OGWDW/TSC: 532: Phenylurea Compounds in Water by HPLCUV

Summary
Analytes
Revision
Data and Sites

Official Method Name

Determination of Phenylurea Compounds in Drinking Water by Solid Phase Extraction and High Performance Liquid Chromatography with UV Detection

Current Revision

Revision 1.0, June 2000

Media

WATER

Instrumentation

High Performance Liquid Chromatography with Ultraviolet 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 500-mL sample is extracted using a solid phase extraction (SPE) cartridge or disk. The pesticides are elute from the SPE cartridge or disk using methanol, and the methanol extract is concentrated. The concentrations of pesticides in the extract are measured using a high performance liquid chromatography (HPLC) system equipped with an ultraviolet/visible (UV/Vis) detector.

Scope and Application

This method determines phenylurea pesticides in drinking water.

Applicable Concentration Range

1.0-30.0 ug/L for all analytes.

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. A peak is observed near fluometuron which can interfere with quantitation.

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 500 mL amber or clear glass bottles fitted with PTFE-lined screw-caps. Prior to shipment to the field, 0.25 g of cupric sulfate and 2.5 g of Trizma crystals must be added to each bottle for each 500 mL of sample collected.
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; 21 days after extraction (Samples exchanged into reagent water/acetonitrile (60/40) for confirmational analysis may be stored 7 days at 0^oC or less; however, the combined extract holding time may not exceed 21 days.)

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 9 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Diflubenzuron(35367-38-5) Diflubenzuron	0.035 ug/L	100% Rec (SL)	2.00 % RSD (SL)	1.00 ug/L
Diuron(330-54-1) Diuron Urea, N'-(3,4-dichlorophenyl)-N,N-dimethyl- (9CI)	0.018 ug/L	102% Rec (SL)	1.80 % RSD (SL)	1.00 ug/L
Fluometuron(2164-17-2) Fluometuron	0.028 ug/L	99% Rec (SL)	2.20 % RSD (SL)	1.00 ug/L
Herbicides(E-12839) Herbicide formulations Herbicides	N/A	N/A	N/A
Linuron(330-55-2) Linuron	0.032 ug/L	108% Rec (SL)	1.60 % RSD (SL)	1.00 ug/L
Propanil(709-98-8) Propanil	0.071 ug/L	96% Rec (SL)	3.60 % RSD (SL)	1.00 ug/L
Siduron(1982-49-6) Siduron	0.067 ug/L	100% Rec (SL)	3.00 % RSD (SL)	1.00 ug/L
Tebuthiuron(34014-18-1) Brulan Graslan Perflan Spike Tebuthiuron Tebuthiuron (graslan) Terbuthiuron Urea, N-[5-(1,1-dimethylethyl)-1,3,4-thiadiazo	0.046 ug/L	100% Rec (SL)	1.80 % RSD (SL)	1.00 ug/L
Thidiazuron(51707-55-2) Thidiazuron	0.047 ug/L	103% Rec (SL)	2.40 % RSD (SL)	1.00 ug/L

Precision Descriptor Notes:	Precision and accuracy values were calculated using data from the analyses of seven replicate fortified reagent water samples in a single laboratory using conditions specified in Table 4 of the method. Additional data 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 a 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 from the analyses of seven replicate fortified reagent water samples in a single laboratory using conditions specified in Table 4 of the method. Additional data 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 a 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

The Water Quality Portal contains sample results from sites that use this method.

Download WQP data

Select data:

Sites only
Sample results only

File format:

Comma-separated
Tab-separated
MS Excel 2007+

Sites where this method was used

Loading Sites ...

EPA-OGWDW/TSC: 532: Phenylurea Compounds in Water by HPLCUV

WHO WE ARE

LEGAL