EPA Method 605


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EPA Method 605:
Benzidines

Summary:
A 1-L sample is extracted with chloroform in a separatory funnel. The chloroform extract is extracted with acid. The acid extract is then neutralized and extracted with chloroform. The final chloroform extract is exchanged to methanol while being concentrated using a rotary evaporator. The extract is mixed with buffer and the concentrations of benzidines are measured using a high performance liquid chromatography (HPLC) system equipped with an electrochemical detector (ED).

Scope:
This method determines certain benzidines in wastewater and other waters.

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

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) Compounds in dye plant effluents: Interference with benzidine determination by compounds in dye plant effluents can be avoided by reducing the electrode potential.

QC 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.

Maximum Holding Time:
Extract w/in 7 days; Analyze extracts w/in 7 days if held properly.

Media:
WATER

Subcategory:
Organic

Concentration:
Ranges differ for each analyte depending on matrix and interferences.

Precision:
The precision and accuracy values were determined using regression equations derived from a 17 laboratory validation study. The study determined analytes at six concentrations in the range of 1.0 to 70 ug/L in multiple matrix types (including wastewaters, drinking waters, surface waters, and reagent water).

Detection:
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 Number:
40 CFR Part 136, Appendix A (Current Edition)

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Examples:  8260
TO-15

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Mercury
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