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EPA Method 524.2:

Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry – Revision 4.1.

Summary:
Inert gas is bubbled through a water sample to purge volatile organic compounds with low water solubility. Purged compounds are trapped in a tube containing suitable sorbent materials. When purging is complete, the sorbent tube is heated and backflushed with helium to desorb the trapped compounds into a capillary gas chromatography (GC) column. The concentrations of compounds from the trap are measured using a capillary column GC system equipped with a mass spectrometer (MS).

Scope:
This method determines purgeable volatile organic compounds (including some disinfection byproducts) in surface water, ground water, and drinking water in any stage of treatment.

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

Interferences:
(A) Contamination of samples with volatiles in the laboratory and impurities in the purge gas and sorbent trap: Use PTFE/Teflon or metal gas lines and plumbing (no out-gassing plastics), and analyze blanks to minimize risk of contamination.(B) Contamination from sample carryover: Rinsing apparatus with water and purging equipment between analyses can minimize contamination.(C) Contamination from methylene chloride (MeCl): When determining MeCl (a ubiquitous solvent) wear clothes that have not been exposed to MeCl fumes and use stainless steel or copper carrier gas and plumbing lines (MeCl permeates PTFE) to minimize contamination.(D) Contamination of methanol: Ketones, methylene chloride, and other organic solvents often contaminate even high purity methanol.

QC Requirements:
Initial demonstration of laboratory capability followed by regular analyses of laboratory reagent blanks (LRBs), field reagent blanks (FRBs), and laboratory fortified blanks (LFBs). Initial demonstration of laboratory capability includes the analysis of four to seven replicates of an LFB containing each analyte of concern at a concentration in the range of 2 – 5 ug/L depending upon the calibration range of the instrumentation. Additional QC procedures are recommended. A method detection limit (MDL) must be determined for each analyte.

Maximum Holding Time:
14 days.

Media:
WATER

Subcategory:
Organic

Concentration:
Approximate range is 0.02 – 200 ug/L for wide-bore thick-film capillary columns and 0.02 – 20 ug/L for narrow-bore thick-film capillary columns. Range is analyte and instrument dependent.

Sample Prep:
Dechlorination, pH adjustment.

Precision:
Precision and accuracy values were determined using 7 replicate analyses of fortified reagent water. Two instrument configurations were used. One configuration used cryogenic interface (cryogenic trapping), a quadrapole mass spectrometer, and a narrow capillary bore column (see Table 3 of the Method). The other configuration used an ion trap mass spectrometer with a wide-bore capillary column (see Table 7 of the Method). Consult the method to determine how the data for specific analytes were generated and for additional information. NOTE: Total trihalomethanes (TTHMs) and total xylenes are regulatory parameter that represents the sum of compounds. See specific compounds for information on method performance, and see regulatory data for more information.

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:
Revision 4.1, 1995

Test Description:
Purgeable organic co

Instrument used for this test:
GCMS