EPA-EAD: 602: Purgeable Aromatics via GC with Photoionization Detector (PID)

Summary
Analytes
Revision
Data and Sites

Official Method Name

Purgeable Aromatics

Current Revision

40 CFR Part 136, Appendix A (Current Edition)

Media

WATER

Instrumentation

Gas Chromatography with Photoionization 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 sample is purged with an inert gas transforming the aromatics to the vapor phase which is collected on an absorbent trap at ambient temperature. After the sample is purged, the trap is then heated, backflushed, and desorbed with the inert gas onto a chromatographic column. The gas chromatograph is temperature programmed to separate the aromatics which are then detected by a photoionization detector. Method 624 can be used for GC/MS confirmation of compound match or interference.

Scope and Application

This method determines target compounds potentially found in municipal and industrial discharges.

Applicable Concentration Range

MDL to 1000xMDL (ug/L).

Interferences

(A) Impurities in gas and plumbing: Impurities in the inert gas and organic plumbing system of the purge and trap concentrator tend to be the main cause of interference in the analytical system. The use of non-Teflon tubing and fittings should be avoided.
(B) Contamination during collection: Samples can become contaminated by diffusion of volatile organic compounds across the septum seal during collection and storage. Use Field Blanks to verify possible contamination.
(C) Carryover: Contamination by carry-over in the analytical system can occur, especially in samples that are extremely concentrated. Frequent bakeout and cleaning of the purging system can help prevent carry-over.

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

Sample should be placed in a 25mL or larger glass vial; screw cap with a hole in the center for a Teflon-faced silicone septum. The sample should not have a headspace and should be kept refrigerated until analysis. If the sample is believed to contain free or combined chlorine, add 10mg/40mL of sodium thiosulfate upon collection and shake vigorously for one minute. Adjust the pH of the sample to that of about 2 with (1+1) HCl while stirring.

Maximum Holding Time

14 days

Relative Cost

$201 to $400

Sample Preparation Methods

None.

This method has 9 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
1,2-Dichlorobenzene(95-50-1) 1,2-Dichlorobenzene Benzene, 1,2-dichloro- Dilantin db Dowtherm e o-Dichlorobenzene ortho-Dichlorobenzene	0.400 ug/L	106% Rec (ML)	35.00 % RSD (ML)	4.00 ug/L
1,3-Dichlorobenzene(541-73-1) 1,3-Dichlorobenzene Benzene, 1,3-dichloro- Benzene, m-dichloro- m-Dichlorobenzene	0.400 ug/L	95% Rec (ML)	21.00 % RSD (ML)	4.00 ug/L
1,4-Dichlorobenzene(106-46-7) 1,4-Dichlorobenzene Benzene, 1,4-dichloro- Chlorinated benzenes, mono- and di- Di-chloricide PDB Paramoth p-Dichlorobenzene para-dichlorobenzene	0.300 ug/L	91% Rec (ML)	31.00 % RSD (ML)	4.00 ug/L
Benzene(71-43-2) Benzene Benzol Coal naptha Cyclohexatriene Phene Pyrobenzol	0.200 ug/L	106% Rec (ML)	34.00 % RSD (ML)	4.00 ug/L
Chlorobenzene(108-90-7) Benzene chloride Benzene, chloro- Chlorobenzene MCB Monochlorobenzene Phenyl chloride	0.200 ug/L	96% Rec (ML)	20.00 % RSD (ML)	4.00 ug/L
Ethylbenzene(100-41-4) Benzene, ethyl Ethyl benzene Ethylbenzene Ethylbenzol Phenylethane	0.200 ug/L	102% Rec (ML)	32.00 % RSD (ML)	4.00 ug/L
Organics, semivolatile(E-12884) Organics, semivolatile Semi-volatile organics Semivolatile organics	N/A	N/A	N/A
Toluene(108-88-3) Benzene, methyl Methacide Methylbenzene Methylbenzol Phenylmethane Toluene Toluol	0.200 ug/L	110% Rec (ML)	34.00 % RSD (ML)	4.00 ug/L
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 20 laboratory validation study.This study determined analytes in reagent water, drinking water, surface water, and three industrial wastewaters spiked at six concentrations over the range 2.1 to 550 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 12.1 of the Method.

Revision	PDF/Link
40 CFR Part 136, Appendix A (Current Edition)

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EPA-EAD: 602: Purgeable Aromatics via GC with Photoionization Detector (PID)

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