Battery-Operated and Self-Heating Solid-Phase Microextraction Device for Field Detection and Long-Term Preservation of Mercury in Soil

Abstract

The application of headspace solid-phase microextraction (HS-SPME) for mercury preservation and detection still has several shortcomings, including the use of high-temperature desorption chamber, the consumption of expensive reagent (NaBEt4 or NaBPr4), and analyte loss during sample storage. Herein, a self-heating HS-SPME device using a gold-coated tungsten (Au@W) fiber was developed for the field detection of mercury in soil by miniature point discharge optical emission spectrometry (μPD-OES). Hg2+ was reduced to Hg0 with NaBH4 solution and then preconcentrated with the Au@W fiber. The adsorbed Hg0 could be rapidly desorbed by directly heating the fiber with a mini lithium battery and subsequently detected by μPD-OES. A limit of detection (LOD) of 0.008 mg kg-1 was obtained with a relative standard deviation (RSD) of 2.4%. The accuracy of the self-heating HS-SPME was evaluated by analyzing a soil certified reference material (CRM) and nine soil samples with satisfactory recoveries (86-111%). Compared to the conventional external heating method, the proposed method reduces desorption time and power consumption from 80 s and 60 W to 20 s and 2.5 W, respectively. Moreover, the self-heating device enables the μPD-OES system to remove the high-temperature desorption chamber, making it more compact and suitable for field analytical chemistry. Interestingly, the Au@W SPME fiber can be also used for the long-term preservation of mercury with a sample loss rate <5% after 30 days of storage at room temperature.