EPA-EAD: 606: Phthalate Esters in Water by GCECD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Phthalate Esters

Current Revision

40 CFR Part 136, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection

Method Subcategory

Organic

Method Source

EPA-EAD

Citation

EPA Method Guidance CD-ROM (includes MCAWW Methods, and most current EPA Methods)

Brief Method Summary

A 1-L sample is extracted with methylene chloride using a separatory funnel. The methylene chloride extract is dried and exchanged to hexane during concentration to a volume of 10-mL or less. The concentrations of esters in the extract are measured using a gas chromatography (GC) system equipped with an electron capture detector (ECD).

Scope and Application

This method determines certain phthalate esters in wastewater and other waters.

Applicable Concentration Range

Ranges differ for each analyte depending on matrix and interferences.

Interferences

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

(B) Reagent contamination: Use high purity reagents.

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

(D) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by performing a cleanup procedure.

Quality Control Requirements

Each laboratory that uses this method is required to operate a formal quality control program. The minimum requirements of this program consist of an initial demonstration of laboratory capability and an ongoing analysis of spiked samples to evaluate and document data quality. The laboratory must maintain records to document the quality of data that is generated. Ongoing data quality checks are compared with established performance criteria to determine if the results of analyses meet the performance characteristics of the method. When results of sample spikes indicate atypical method performance, a quality control check standard must be analyzed to confirm that the measurements were performed in an in-control mode of operation.

Sample Handling

Grab samples must be collected in glass containers. [Note: Do NOT pre-rinse bottles]. Composite samples should be collected in refrigerated glass containers in accordance with the requirements of the program. Automatic sampling equipment must be as free as possible of Tygon tubing and other potential sources of contamination.

All samples must be iced or refrigerated at 4^oC from the time of collection until extraction.

Maximum Holding Time

Extract w/in 7 days; Analyze extracts w/in 40 days.

Relative Cost

$201 to $400

Sample Preparation Methods

This method has 6 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
Butyl benzyl phthalate(85-68-7) 1,2-Benzenedicarboxylic acid, butyl phenylmeth 1,2-Benzenedicarboxylic acid, butyl phenylmethyl ester BBP Benzenedicarboxylic acid,1,2-, butyl phenylmethyl ester Benzyl butyl phthalate Benzyl butyl phthalate--1,2-Benzenedicarboxylic acid ... Benzyl-N-butyl phthalate Butyl benzyl phthalate N-Butyl benzyl phthalate Phthalic acid, benzyl butyl ester Phthalic acid, butylbenzylester	0.340 ug/L	82% Rec (ML)	25.00 % RSD (ML)	20.00 ug/L
Di-n-butyl phthalate(84-74-2) 1,2-Benzenedicarboxylic acid, dibutyl ester Benzenedicarboxylic acid,1,2-, dibutyl ester DBP Di-n-butyl phthalate Dibutyl phthalate Phthalic acid, dibutyl ester	0.360 ug/L	80% Rec (ML)	29.00 % RSD (ML)	20.00 ug/L
Di-n-octyl phthalate(117-84-0) 1,2-Benzenedicarboxylic acid, dioctyl ester Benzenedicarboxylic acid,1,2-, dioctyl ester Benzenedicarboxylic acid,o-, dioctyl ester Di-n-octyl phthalate Dioctyl phthalate Dioctyl-o-benzenedicarboxylate Dioctyl-o-phthalate n-Dioctylphthalate	3.000 ug/L	31% Rec (ML)	67.00 % RSD (ML)	20.00 ug/L
Diethyl phthalate(84-66-2) 1,2-Benzenedicarboxylic acid, diethyl ester Benzenedicarboxylic acid,1,2-, diethyl ester DEP Diethyl phthalate Phthalic acid, diethyl ester o-Diethyl phthalate	0.490 ug/L	71% Rec (ML)	46.00 % RSD (ML)	20.00 ug/L
Dimethyl phthalate(131-11-3) 1,2-Benzendicarboxylic acid, dimethyl ester 1,2-Benzenedicarboxylic acid, dimethyl ester Benzenedicarboxylic acid,1,2-, dimethyl ester DMP Dimethyl phthalate Phthalic acid, dimethyl ester o-Dimethyl phthalate	0.290 ug/L	74% Rec (ML)	46.00 % RSD (ML)	20.00 ug/L
bis(2-Ethylhexyl) phthalate(117-81-7) 1,2-Benzenedicarboxylic acid, bis(2-ethylhexyl 1,2-Benzenedicarboxylic acid, bis(2-ethylhexyl)ester BEHP BEHP, DEHP DEHP Di(2-ethylhexyl) phthalate Di(2-ethylhexyl)orthophthalate Di(sec-octyl) phthalate Di-(2-ethylhexyl)phthalate Di-sec-octyl phthalate Diethylhexyl phthalate Phthalic acid dioctyl ester Phthalic acid, bis(2-ethylhexyl) ester bis(2-Ethylhexyl) phthalate bis(2-Ethylhexyl)-1,2-benzenedicarboxylate bis(2-Ethylhexyl)-o-phthalate	2.000 ug/L	63% Rec (ML)	72.00 % RSD (ML)	20.00 ug/L

Precision Descriptor Notes:	The precision and accuracy values were determined using regression equations derived from a 16 laboratory validation study. The study determined analytes at six concentrations in the range of 0.7 to 106 ug/L in multiple matrix types (including wastewaters, drinking waters, surface waters, and reagent water).
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
40 CFR Part 136, Appendix A (Current Edition)

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EPA-EAD: 606: Phthalate Esters in Water by GCECD

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