EPA Method 609


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EPA Method 609:
Nitroaromatics and Isophorone

Summary:
A 1L sample is extracted using a liquid/liquid phase extraction technique with methylene chloride as the extracting solvent. The extract is dried through sodium sulfate, exchanged to hexane, and then concentrated down to a volume of less than 10mL. The extract is then separated using gas chromatography. Isophorone and nitrobenzene are measured with a FID and the dinitrotoluenes with an ECD. Method 624 can be used for GC/MS confirmation of compound match or interference. Guidelines for the use of alternative detectors are listed in section 12.1 of the method.

Scope:
This is a GC method where nitroaromatics and isophorone are detected from municipal and industrial discharges listed 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 that may cause possible interference with the target compounds. A Florisil 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:
7xMDL to 1000xMDL (ug/L)

Sample Prep:
None.

Precision:
The precision and accuracy values were determined using regression equations derived from a 18 laboratory validation study. This determined analytes using reagent water, drinking water, surface water, and three industrial wastewaters spiked at six concentrations over the range 1.5 to 515 mg/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 14 of the Method.

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

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