Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of gasoline oxygenates, selected degradates, and BTEX in water by heated purge and trap/gas chromatography/mass spectrometry
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Abstract
A method for determination of the alkyl ethers u sed as gasoline oxygenates [ethyl tert-butyl ether (ETBE), methyl tert-butyl ether (MTBE), diisopropyl ether (DIPE), and tert-amyl methyl ether (TAME)], some of their main degradates [acetone, methyl acetate, tert-butyl alcohol (tBA), and tert-amyl alcohol (tAA)], and BTEX (benzene, toluene, ethylbenzene, and xylenes) at low concentrations (<5 micrograms per liter) in water samples was developed. The compounds are determined using heated extraction to improve purging of polar compounds in a standard gas chromatography/ mass spectrometry (GC/MS) method for volatile compounds. Volatile compounds in this method are extracted (purged) from the sample b y bubbling helium through a 25-mL (milliliter) sample heated at about 65°C. Volatile compounds are trapped on a sorbent and then thermally desorbed into a GC/MS system for identification and quantitation. The calibration range for this method is 0.1 to 200 μg/L (micrograms per liter). Mean gasoline oxygenate recoveries from volatile-grade blank-water samples analyzed at concentrations from 0.5 to 5.0 μg/L were 95 to 105 percent, with relative standard deviations (RSDs) from 1.9 to 3.2 percent. Mean oxygenate degradate recoveries ranged from 88 to 107 percent, with RSDs of 3.2 to 7.4 percent, at concentrations from 1 to 50 μg/ L. Mean BTEX recoveries ranged from 91 to 107 percent, with RSDs of 1.1 to 6.6 percent, at concentrations from 0.5 to 10 μg/L . The method detection limits range from 0.035 to 0.052 μg/L for the gasoline oxygenates, 0.216 to 0.62 μg/L for the oxygenate degradates, and 0.005 to 0.036 μg/L for BTEX. Calculated holding times using American Society for Testing and Materials (ASTM) procedure D 4841-88 indicate that all of the analytes are stable for a minimum of 40 days at pH 2 and pH 7, except for methyl acetate, which is only stable for 7 days at pH 2.
| Publication type | Report |
|---|---|
| Publication Subtype | USGS Numbered Series |
| Title | Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory-Determination of gasoline oxygenates, selected degradates, and BTEX in water by heated purge and trap/gas chromatography/mass spectrometry |
| Series title | Water-Resources Investigations Report |
| Series number | 2003-4079 |
| DOI | 10.3133/wri034079 |
| Year Published | 2003 |
| Language | English |
| Publisher | U. S. Geological Survey |
| Contributing office(s) | National Water Quality Laboratory |
| Description | vii, 31 p. |
| Google Analytic Metrics | Metrics page |