EPA-NERL: 522: 1,4-Dioxane in water by SPE and GC/MS with SIM

Summary
Analytes
Revision
Data and Sites

Official Method Name

METHOD 522 DETERMINATION OF 1,4-DIOXANE IN DRINKING WATER BY SOLID PHASE EXTRACTION (SPE) AND GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS) WITH SELECTED ION MONITORING (SIM): EPA/600/R-08/101

Current Revision

Version 1, Sept. 2008

Media

WATER

Instrumentation

Gas Chromatography with Mass Spectrometry Detection

Method Subcategory

Organic

Method Source

EPA-NERL

Citation

METHOD 522 DETERMINATION OF 1,4-DIOXANE IN DRINKING WATER BY SOLID PHASE EXTRACTION (SPE) AND GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS) WITH SELECTED ION MONITORING (SIM): EPA/600/R-08/101

Brief Method Summary

A water sample that has been dechlorinated and preserved with a microbial inhibitor is fortified with the isotopically labeled SUR, 1,4-dioxane-d8. The sample is extracted by one of two SPE options. In option 1, a 500-mL sample is passed through an SPE cartridge containing 2 g of coconut charcoal to extract the method analyte and SUR. In option 2, a 100-mL sample is extracted on a Waters AC-2 Sep-Pak or Supelco Supelclean ENVI-Carb Plus cartridge. In either option, the compounds are eluted from the solid phase with a small amount of dichloromethane (DCM), approximately 9 mL or 1.5 mL, respectively. The extract volume is adjusted, and the IS, tetrahydrofuran-d8 (THF-d8), is added. Finally, the extract is dried with anhydrous sodium sulfate. Analysis of the extract is performed by GC/MS. The data provided in this method were collected using splitless injection with a high-resolution fused silica capillary GC column that was interfaced to an MS operated in the SIM mode. The analyte, SUR and IS are separated and identified by comparing the acquired mass spectra and retention times to reference spectra and retention times for calibration standards acquired under identical GC/MS conditions. The concentration of the analyte is determined by comparison to its response in calibration standards relative to the IS. Although the performance data presented in Section 17 of this method were obtained in the SIM mode for maximum method sensitivity, the sample extract analysis may also be performed in full scan mode if the sensitivity achieved meets the data user¿s requirements.

Scope and Application

This is a gas chromatography/mass spectrometry (GC/MS) method for the determination of 1,4-dioxane (CASRN 123-91-1) in drinking water. Accuracy and precision data have been generated in reagent water, finished ground and surface waters. Although this method was developed and demonstrated using selected ion monitoring (SIM) GC/MS for maximum sensitivity, it can also be used with full scan GC/MS if the sensitivity achieved meets the user¿s data requirements.

Applicable Concentration Range

Interferences

See Section 4.0 of the method.

Quality Control Requirements

See Section 9 of the method.

Sample Handling

See Section 8 of the method.

Maximum Holding Time

Samples must be chilled during shipment and must not exceed 10 degrees C during the first 48 hours after collection.

Relative Cost

Sample Preparation Methods

This method has 1 analyte associated with it.

Analyte	Detection Level	Bias	Precision	Pct False Positive	Pct False Negative	Spiking Level
p-Dioxane(123-91-1) 1,4-Diethylene dioxide 1,4-Diethylene oxide 1,4-Dioxacyclohexane 1,4-Dioxane Diethylene ether Glycol ethylene ether Tetrahydro-1,4-dioxin Tetrahydro-p-dioxin p-Dioxane	0.026 ug/L	110% Rec	19.00 % RSD			0.04 ug/L

Precision Descriptor Notes:	See Section 17 for tables, diagrams, flow charts, and validation data.
Detection Level Note:	The Minimum Reporting Level (MRL) is the lowest analyte concentration that meets Data Quality Objectives (DQOs) that are developed based on the intended use of this method. Two single laboratory Lowest Concentration Minimum Reporting Levels (LCMRLs) of 0.036 and 0.047 ug/L have been determined in reagent water. The single laboratory LCMRL is the lowest true concentration for which the future recovery is predicted to fall, with high confidence (99%), between 50 and 150% recovery.

Precision Descriptor Notes:

See Section 17 for tables, diagrams, flow charts, and validation data.

Detection Level Note:

The Minimum Reporting Level (MRL) is the lowest analyte concentration that meets Data Quality Objectives (DQOs) that are developed based on the intended use of this method. Two single laboratory Lowest Concentration Minimum Reporting Levels (LCMRLs) of 0.036 and 0.047 ug/L have been determined in reagent water. The single laboratory LCMRL is the lowest true concentration for which the future recovery is predicted to fall, with high confidence (99%), between 50 and 150% recovery.

Revision	PDF/Link
Version 1, Sept. 2008

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-NERL: 522: 1,4-Dioxane in water by SPE and GC/MS with SIM

WHO WE ARE

LEGAL