Comparison of SPME headspace analysis to U.S. EPA method 5030/8260B for MTBE monitoring

Abstract

Methyl tert‐butyl ether (MTBE) is one of the most common ground water contaminants in the United States. Ground water contaminated with MTBE is also likely to be contaminated with tert‐butyl alcohol (TBA) because TBA is a component of commercial‐grade MTBE, can also be used as a fuel oxygenate, and is a biodegradation product of MTBE. In California, MTBE is subject to reporting at concentrations >3 μg/L, and TBA has a drinking water action level of 12 μg/L. We describe a simple, automated solid‐phase microextraction (SPME) method for the analysis of MTBE and TBA in water. The headspace (HS) of a water sample is extracted with a carboxen/polydimethylsiloxane SPME fiber and the MTBE and TBA are desorbed into a gas chromatograph (GC) and detected using a mass spectrometer (MS). The method is optimized for the routine analysis of MTBE and TBA, with a level of quantitation of 0.3 and 4 μg/L, respectively, in water. The lower level of detection for MTBE is 0.03 μg/L using this method. This HS extraction SPME is applicable to the measurement of both MTBE and TBA at concentrations below regulatory action levels. This method was compared with the certified U.S. EPA Method 5030/8260B (purge and trap/GC/MS) using split samples. Results from the SPME‐HS/GC/MS method were directly comparable to those from the U.S. EPA Method 5030/8260B. This method provides a simple, inexpensive, accurate, and sensitive alternative to the U.S. EPA Method 5030/8260B for the analysis of MTBE and TBA in water samples.

Analysis of tert-Butanol, Methyl tert-Butyl Ether, Benzene, Toluene, Ethylbenzene and Xylene in Ground Water by Headspace Gas Chromatography-Mass Spectrometry

“…Recently, a specific and highly sensitive method for MTBE analysis has been developed that relies on headspace solid phase microextraction (SPME). [11][12][13][14][15][16][17][18][19] The methods have many advantages in it being convenient and having rapid and automatic extraction, but its low recovery due to the volatility and long loading time of the SPME fibre.…”

Separation and Enhanced Detection of Anesthetic Compounds Using Solid Phase Micro-Extraction (SPME)–Raman Spectroscopy

“…Techniques that benefit from SPME pre-concentration are well documented in the literature. 16,21–24 In addition to signal enhancement, SPME has the potential to separate macromolecules that may interfere with the detection of smaller target analytes. This sort of separation could prove very useful when dealing with analytes in a complex system such as blood or serum.…”

Quantitative Solid-Phase Microextraction (SPME)–Raman Spectroscopy for the Detection of Trace Organics in Water

“…8 The partitioning of these organics into PDMS polymer has been extensively characterized by techniques based on mass spectrometry. 9,10 Techniques such as purge and trap GC/MS and MIMS have enhanced sensitivity because of the use of a polymer pre-concentration step and are also capable of extracting crucial quantitative parameters that dictate analyte permeation. 10,11 One such parameter that influences how non-polar organics interact with PDMS is the equilibrium partition coefficient ( K ).…”

“…9,10 Techniques such as purge and trap GC/MS and MIMS have enhanced sensitivity because of the use of a polymer pre-concentration step and are also capable of extracting crucial quantitative parameters that dictate analyte permeation. 10,11 One such parameter that influences how non-polar organics interact with PDMS is the equilibrium partition coefficient ( K ). The partition coefficient is the thermodynamic parameter that quantitatively relates the analyte preference for the polymer phase over the polar aqueous phase.…”