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View Actual EPA Method 524.3 (PDF File)
EPA Method 524.3:MEASUREMENT OF PURGEABLE ORGANIC COMPOUNDS IN WATER BY CAPILLARY COLUMN GAS CHROMATOGRAPHY/MASS SPECTROMETRY
Summary:Headspace-free samples are collected in amber, glass vials with polytetrafluoroethylene (PTFE)- faced septa. Samples are dechlorinated with ascorbic acid and the pH is adjusted with maleic acid. A 5.0-milliliter (mL) aliquot of the sample is transferred to a glass sparging vessel along with appropriate amounts of internal standard and quality control compounds. The method analytes are purged from the water using helium and trapped on a sorbent material. After purging, the trap may be dry purged for a short period to remove water. Additional water management techniques may be applied. The trap is heated and backflushed with helium to transfer the analytes directly into a gas chromatographic inlet. The inlet is operated in the split mode in order to achieve the desired desorb flow rates and further reduce water transmission. Analytes are transferred onto a capillary GC column, which is temperature programmed to optimize the separation of method analytes. Compounds eluting from the GC are directed into a mass spectrometer for detection and quantitation. The method analytes are identified by comparing the acquired mass spectra and retention times to reference spectra and retention times for calibration standards acquired under identical GC/MS conditions. The concentration of each analyte is calculated using the internal standard technique and response curves obtained via procedural calibration.
Scope:This is a gas chromatography/mass spectrometry (GC/MS) method for the determination of purgeable organic compounds in finished drinking waters. Discontinuous scanning modes such as selected ion monitoring (SIM) and selected ion storage (SIS) are permitted for determining selected analytes that are monitored at levels too low for the full scan detection mode. Precision and accuracy data have been generated for the method analytes in reagent water, drinking water from a groundwater source, and drinking water from a surface water source. The single laboratory Lowest Concentration Minimum Reporting Level (LCMRL) has also been determined in reagent water.