EPA-EAD: 611: Haloethers in Water by GCELCD

Summary
Analytes
Revision
Data and Sites

Official Method Name

Haloethers

Current Revision

40 CFR Part 136, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Electrolytic Conductivity 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 haloethers in the extract are measured using a gas chromatography (GC) system equipped with a halide specific detector, such as an electrolytic conductivity detector (ELCD) or a microcoulometric detector.

Scope and Application

This method determines certain haloethers 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) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by performing a cleanup procedure.

(D) Dichlorobenzenes: Extract samples with 2 different column packings to reduce interference from coelution of dichlorobenzes with haloethers.

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. Fill the sample bottles and, if residual chlorine is present, add 80 mg of sodium thiosulfate per liter of sample and mix well. EPA Methods 330.4 and 330.5 may be used for measurement of residual chlorine. Field test kits are available for this purpose.

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
4-Bromophenyl phenyl ether(101-55-3) 1-Bromo-4-phenoxybenzene 4-Bromodiphenylether 4-Bromophenyl phenyl ether Benzene, 1-bromo-4-phenoxy- Bromophenyl, 4-phenyl ether Phenyl-4-bromophenyl ether p-Bromodiphenyl ether p-Bromophenyl phenyl ether	2.300 ug/L	98% Rec (ML)	49.00 % RSD (ML)	20.00 ug/L
4-Chlorophenylphenyl ether(7005-72-3) 1-Chloro-4-phenoxybenzene 4-Chlorodiphenyl ether 4-Chlorophenyl ether 4-Chlorophenylphenyl ether Benzene, 1-chloro-4-phenoxy Chlorophenyl, 4-phenyl ether Monochlorodiphenyl oxide p-Chlorophenyl phenyl ether	3.900 ug/L	92% Rec (ML)	44.00 % RSD (ML)	20.00 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
bis(2-Chloroethoxy)methane(111-91-1) 1,1'-(methylenebis(oxy))bis(2-chloro-Ethane) Dichloromethoxy ethane Ethane, 1,1'-[methylenebis(oxy)]bis[2-chloro- Methane, bis(2-chloroethoxy)- bis(2-Chloroethoxy)methane	0.500 ug/L	74% Rec (ML)	36.00 % RSD (ML)	5.00 ug/L
bis(2-Chloroethyl) ether(111-44-4) 1,1'-Oxybis(2-chloro-ethane) 2,2'-Dichlorodiethyl ether 2,2'-Dichloroethyl ether BCEE Chlorex Dichloroethyl ether Dichloroethyl ether,beta,beta'- Ethane, 1,1'-oxybis[2-chloro- Ether, bis(2-chloroethyl) bis(2-Chloroethyl) ether sym-Dichloroethyl ether	0.300 ug/L	92% Rec (ML)	43.00 % RSD (ML)	5.00 ug/L
bis(2-Chloroisopropyl) ether(108-60-1) 2,2'-Dichloroisopropyl ether 2,2'-oxybis(1-chloropropane) DCIP Dichlorodiisopropyl ether Ether, bis(2-chloro-1-methylethyl) Propane, 2,2'-oxybis[1-chloro- bis(2-Chloro-1-methylethyl) ether bis(2-Chloroisopropyl) ether	0.800 ug/L	118% Rec (ML)	49.00 % RSD (ML)	5.00 ug/L

Precision Descriptor Notes:	The precision and accuracy values were determined using regression equations derived from a 20 laboratory validation study. The study determined analytes using reagent water, drinking water, surface water, and three industrial wastewaters with known additions at six concentrations over the range 1.0 to 626 ?g/L. Single operator precision, overall precision, and accuracy were found to be directly related to the concentration of the parameter and essentially independent of the sample matrix.
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.

Precision Descriptor Notes:

The precision and accuracy values were determined using regression equations derived from a 20 laboratory validation study. The study determined analytes using reagent water, drinking water, surface water, and three industrial wastewaters with known additions at six concentrations over the range 1.0 to 626 ?g/L. Single operator precision, overall precision, and accuracy were found to be directly related to the concentration of the parameter and essentially independent of the sample matrix.

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: 611: Haloethers in Water by GCELCD

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