Method Development for the Analysis of 1,4-Dioxane in Drinking Water Using Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

Abstract

1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The United States Environmental Protection Agency's (U.S. EPA) National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of an activated carbon solid-phase extraction of 500-mL or 100-mL water samples using dichloromethane as the elution solvent. The extracts are analyzed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. In the NERL laboratory, recovery of 1,4-dioxane ranged from 94-110% in fortified laboratory reagent water and recoveries of 96-102% were demonstrated for fortified drinking water samples. The relative standard deviations for replicate analyses were less than 6% at concentrations exceeding the minimum reporting level.

Determination of 1,4‐dioxane in water samples using freeze‐assisted liquid–liquid extraction and gas chromatography‐mass spectrometry with select reaction monitoring

“…Many other methods for determination of 1,4‐dioxane in groundwater exist, including purge and trap [19, 25‐31]; SPE [18, 20, 32–35]; SPME [21–22]; and LLE [19‐20, 35]. These methods can produce LODs at sub part per billion (μg/L) levels, but all also require sample sizes of at least 1 milliliter (Table 1).…”

Rapid Analysis of 1,4‐Dioxane in Groundwater by Frozen Micro‐Extraction with Gas Chromatography/Mass Spectrometry

“…EPA 2000), and compares well with the MDLs for other analytical methods (Table 1). Based on the assessment of the method performance, even lower detection limits and higher sensitivities might be possible to achieve by reducing the concentration of the IS (to reduce peak broadening), increasing injection volume, calibrating with a lower level curve (e.g., 5 to 50 μg/L), excluding the secondary ions for SIM detection (i.e., m / z 58 for dioxane and m / z 64 for dioxane‐d 8 ), and increasing the GC column film thickness (e.g., 1.4 μm) (Grimmett and Munch 2009). Several pretreatment parameters are also adjustable to meet different experimental needs.…”

“…Usually, acetone and methylene chloride were used as the solvent eluent and the extract was analyzed by GC/MS, which yielded notably enhanced recoveries (>90%) and low limits of detection (<1 μg/L), but still required a relatively large water sample volume (80 to 500 mL) (Kawata et al 2001; Kawata et al 2003; Park et al 2005; Isaacson et al 2006; Tanabe et al 2006; Grimmett and Munch 2009; Kawata and Tanabe 2009). In these cases the high water content in the eluates must be managed, either by pretreatment using air drying or centrifugation of the SPE materials (Kawata et al 2001; Park et al 2005; Isaacson et al 2006; Grimmett and Munch 2009), or by post‐treatment using freezing separation of the water layer from organic extracts (Kawata et al 2003; Tanabe et al 2006; Tanabe and Kawata 2008; Kawata and Tanabe 2009). Moreover, matrix interferences and total suspended solids in water samples have been shown to hinder the successful application of this technique (Park et al 2005).…”

Measurement of 1,4-dioxane in surface water by headspace GC-MS

“…[13][14][15][16][17][18][19] Recently, a specific and highly sensitive headspace solid phase microextraction (SPME) [20][21][22][23] and a isotopic dilution headspace (IDHS) 24 …”