EPA Method 613


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EPA Method 613:
2,3,7,8-Tetrachloro Dibenzo-p-Dioxin

Summary:
A 1 L sample is spiked with an internal standard of 2,3,7,8-TCDD and extracted with methylene chloride using a separatory funnel. The extract is exchanged to hexane at a concentration of 1.0 mL or less. The extract is then analyzed by capillary column GC/MS to separate and measure 2,3,7,8-TCDD.

Scope:
This is a GC/MS method that qualitatively confirms and quantifies the presence of 2,3,7,8-TCDD scanned using Method 625 for municipal and industrial discharges as provided under 40 CFR part 136.1.

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

Interferences:
(A) Glassware: Must be scrupulously cleaned. Prior to detergent washing, the glassware should be rinsed with the last solvent used and then placed in a muffle furnace to remove any thermally unstable organic compounds. Some thermally organic compounds, such as PCBs may still remain. A rinse with acetone or pesticide quality hexane may be substituted in place of the muffle furnace. Store glassware inverted or capped with aluminum foil. (B) Co-extraction: The extraction process will sometimes extract certain analytes, such as chlorinated compounds, that may cause possible interference with the target compounds. If these compounds present interference, a cleanup procedure is described in Section 11 of the method.

QC Requirements:
Initial demonstration of laboratory capability and the periodic analysis of laboratory reagent blanks, fortified blanks, and other laboratory solutions as a continuing check on performance.

Maximum Holding Time:
All samples must be extracted within 7 days of collection and completely analyzed within 40 days if extraction.

Media:
WATER

Subcategory:
Organic

Concentration:
MDL to 1000xMDL (ug/L)

Sample Prep:
None.

Precision:
The precision and accuracy values were determined using regression equations derived from a 11 laboratory validation study. The study determined the analyte using reagent water, drinking water, surface water, and three industrial wastewaters spiked at six concentrations over the range 0.02 to 0.20mg/L.

Detection:
MDL procedure is equivalent to the procedure at 40 CFR part 136, Appendix B. MDLs were determined using the standard deviation of 7 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for 6 degrees of freedom at the 99% confidence level (3.14). Detailed instructions for how MDLs are determined are found in Section 12.1 of the Method.

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

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Examples:  8260
TO-15

Examples:  Dioxin
Mercury
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