EPA Method 604


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EPA Method 604:
Phenols

Summary:
A 1-L sample is acidified and extracted with methylene chloride using a separatory funnel. The methylene chloride extract is dried and exchanged to 2-propanol during concentration to a volume of 10-mL or less. The concentrations of phenols in the extract are measured using a gas chromatography (GC) system equipped with a flame ionization detector (FID). The method also provides for a derivatization and column chromatography cleanup procedure to aid in the elimination of interferences. Using this approach, the concentrations of phenols in the extract are measured by detecting derivatives using a GC system with an Electron Capture Detector (ECD).

Scope:
This method covers the determination of phenol and certain substituted phenols 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 the derivitization cleanup procedure in the method.(D) Basic-sample wash: The wash can significantly reduce recovery of phenol and 2,4-dimethylphenol.

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 40 days.

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 20 laboratory validation study. The study determined analytes at six concentrations in the range of 12 to 450 ug/L in multiple matrix types (including reagent water, drinking water, surface water, and three industrial wastewaters).

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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