An improved method for recovering and preconcentrating mercury in natural water samples for stable isotope analysis

• Published in: Journal of analytical atomic spectrometry Vol. 34; no. 11; pp. 233 - 2313
• Main Authors: Li, Kai, Lin, Che-Jen, Yuan, Wei, Sun, Guangyi, Fu, Xuewu, Feng, Xinbin
• Format: Journal Article
• Language: English
• Published: London Royal Society of Chemistry 01.11.2019
• Subjects: Activated carbon; Air filters; Argon; Carrier gases; Chlorine; Composition; Flow velocity; Isotopes; Mathematical analysis; Mercury (metal); Organic chemistry; Vacuum pumps
• ISSN: 0267-9477; 1364-5544
• DOI: 10.1039/c9ja00174c

The composition of stable mercury (Hg) isotopes provides important chemical signatures for tracing the sources and transformation pathways of Hg in the environment. However, such measurements are challenging for natural water samples due to the ultratrace levels of Hg and therefore preconcentration of Hg in water is needed prior to isotope measurements. In this study, we developed a preconcentration method using a modulated apparatus that can be deployed for field measurements. The system includes a 3 L bubbler, a chlorine-impregnated activated carbon (ClC) trap, a zero-air filter connected to the inlet, and a vacuum pump. Hg in aqueous phase samples is first oxidized with BrCl and then reduced with SnCl 2 . The produced Hg 0 is purged from the aqueous phase at a flow rate of 2.5 L min −1 for 1 hour and collected by a trap containing 550 mg of ClC. Hg collected in the ClC trap is then thermally desorbed in argon carrier gas and preconcentrated into a 40% mixed acid solution (4 M HNO 3 and 1.3 M HCl). This method was evaluated using solutions spiked with NIST SRM 3133, UM-Almadén and BCR 482 standards at Hg concentrations of 0.5 to 40 ng L −1 . The results showed an analytical recovery of 98.8 ± 3.7% (1SD, n = 37) with enrichment factors of up to 1000 times and no significant difference in isotope compositions between the recovered Hg and original standards ( t -test, p -δ 202 Hg = 0.24, p -Δ 199 Hg = 0.58, and p -Δ 200 Hg = 0.87). Duplicate experiments on field aqueous samples showed that the analytical precision was 0.13‰, 0.06‰ and 0.07‰ ( n = 16) for δ 202 Hg, Δ 199 Hg and Δ 200 Hg, respectively. The developed method is reliable and efficient for concentrating Hg in natural water samples for determining the Hg isotopic compositions. A new method is developed to meet the criteria for precise and efficient measurements of mercury isotopic composition in various water samples.