EPA-EAD: 609: Nitroaromatics and Isophorone via GC with Flame Ionization Detector (FID) and Electron Capture Detector (ECD)

Summary
Analytes
Revision
Data and Sites

Official Method Name

Nitroaromatics and Isophorone

Current Revision

40 CFR Part 136, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture 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 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 and Application

This is a GC method where nitroaromatics and isophorone are detected from municipal and industrial discharges listed under 40 CFR part 136.1.

Applicable Concentration Range

7xMDL to 1000xMDL (ug/L)

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.

Quality Control 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.

Sample Handling

Samples should be grabbed in 1 Liter or 1 Quart amber bottles with Teflon lined cap. Store samples away from direct sunlight. The bottles must be washed, rinsed with methylene chloride or acetone, and dried before use to minimize contamination. Samples should be iced or kept refrigerated at 4^oC from time of collection to time of extraction.

Maximum Holding Time

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

Relative Cost

$201 to $400

Sample Preparation Methods

None.

This method has 6 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
2,4-Dinitrotoluene(121-14-2) 1-Methyl-2,4-dinitrobenzene 2,4-DNT 2,4-Dinitrotoluene 2,4-Dinitrotoluol Benzene, 1-methyl-2,4-dinitro Benzene,2-methyl-2,4-dinitro- Dinitrobenzene,1-methyl-2,4- Dinitrotoluene, 2,4 Methyl-2,4-dinitrobenzene,1- Toluene, 2,4-dinitro-	0.020 ug/L	76% Rec (ML)	32.00 % RSD (ML)	2.00 ug/L
2,6-Dinitrotoluene(606-20-2) 2,6-DNT 2,6-Dinitrotoluene Benzene, 2-methyl-1,3-dinitro- Benzene,1-methyl-2,6-dinitro- Dinitrobenzene,1-methyl-2,6-	0.010 ug/L	76% Rec (ML)	36.00 % RSD (ML)	2.00 ug/L
Isophorone(78-59-1) 2-Cyclohexen-1-one, 3,5,5-trimethyl- 3,5,5-Trimethyl-2-cyclohexen-1-one 3,5,5-Trimethyl-2-cyclohexene-1-one 3,5,5-Trimethyl-2-cyclohexenone Isooctaphenone Isophorone	15.700 ug/L	196% Rec (ML)	54.00 % RSD (ML)	2.00 ug/L
Nitrobenzene(98-95-3) Benzene, nitro- EPA Pesticide Chemical Code 056501 Essence of mirbane Essence of myrbane Mirbane oil Mononitrobenzene Nitrobenzene Nitrobenzol Oil of mirbane Oil of myrbane RCRA waste number U169	13.700 ug/L	160% Rec (ML)	13.00 % RSD (ML)	2.00 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A

Precision Descriptor Notes:	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 Level Note:	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	PDF/Link
40 CFR Part 136, Appendix A (Current Edition)

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EPA-EAD: 609: Nitroaromatics and Isophorone via GC with Flame Ionization Detector (FID) and Electron Capture Detector (ECD)

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