Simultaneous Analysis of SbIII, SbV and TMSb by High Performance Liquid Chromatography–Inductively Coupled Plasma–Mass Spectrometry Detection: Application to Antimony Speciation in Soil Samples

Abstract

This study was conducted to develop a method for the simultaneous separation and detection of antimonite (Sb(III)), antimonate (Sb(V)) and trimethyl antinmony (TMSb) species in soils, using ultrasonic-aided citric acid extraction and high-performance liquid chromatography-inductively coupled plasma-mass spectrometry separation and detection. The extractions were performed using various chemical solutions. The separation was conducted on a PRP-X100 anion exchange column (25 cm × 4.1 mm i.d., 10 µm) using an isocratic elution program. The various factors of the elution procedure, e.g., pH, elution concentration and retention time, were optimized for the best separation of the three Sb species. It was found that two consecutive extractions using 100 mmol/L citric acid at pH 2.03 resulted in the highest extraction efficiency, 53%. The optimal elution procedure was obtained by using 200 mmol/L ammonium tartrate with 4% methanol as the mobile phase at pH 5.0. Under these conditions, the retention times for Sb(III), Sb(V) and TMSb species were 3.8, 2.1 and 6.8 min with detection limits of 0.03, 0.02 and 0.05 µg/L, respectively. Spiked recoveries for Sb(III), Sb(V) and TMSb ranged from 88 to 118%. The proposed method is reliable for antimony speciation in soil samples.

Speciation of antimony and arsenic in the soils and plants in an old antimony mine

“…Briefly, a solution of 100 mmol/L citric acid at pH 2.03 was used for extraction of Sb from the soil and plant samples (Ge and Wei, 2013). A solution of 2 mol/L trifluoroacetic acid was used for As extraction from the plant samples, and a mixture of 1 mol/L phosphoric acid and 0.1 mol/L ascorbic acid was added to the soil samples to extract the As (Wang and Wei, 2010).…”

“…The chromatographic system (PerkinElmer Series 200) was equipped with an auto-sampler and a quaternary pump that was coupled via a peek capillary to a cross nebulizer of an ICP-MS system. The conditions for the analyses of the speciation of Sb and As were previously developed by our group (Ge and Wei, 2013;Wang and Wei, 2010) and are summarized in Table 2. The pH levels in the mobile phases were adjusted using formic acid or ammonia solutions.…”

Release and Biomethylation of Antimony in Shooting Range Soils upon Flooding

“…The concentrations of Sb species (Sb(III), Sb(V) and TMSb) were measured through coupling a High-Pressure Liquid Chromatograph (HPLC 1200 Series, Agilent Technologies, Santa Clara, CA, USA) to the ICP-MS. The details of the method, initially developed by Ge and Wei [46], are presented in Mestrot et al [37] and in Table S2. Briefly, the mobile phase was 150 mM AT with 4% methanol at pH 5 and was used at a flow rate of 1 mL/min.…”

“…First, we assessed the extraction of Sb species from the soils by different methods from the literature [45][46][47], using a sediment CRM (PACS-3: 14.7 ± 2.2 mg kg −1 Sb, Figure 1a). The total Sb recovery from the CRM with 200 mM AT as an extractant was 21.4 ± 1.8% (n = 3), while, when using a mixture of 200 mM OA and 100 mM AA, it was 45.2 ± 4.6% (n = 4).…”

Speciation of Antimony(III) and Antimony(V) in Bottled Water by Hydride Generation-Inductively Coupled Plasma Optical Emission Spectrometry

“…Various analytical methods have been used for the determination and speciation of the inorganic antimony, such as high-performance liquid chromatography with inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) (Smichowski et al 1995;Zheng, Iijima, and Furuta 2001;Ge and Wei 2013;Jablońska-Czapla et al 2014), atomic absorption spectrometry (AAS) (Fan 2005;Zheng et al 2006;Flores et al 2007;Matusiewicz and Krawczyk 2008;Ferreira et al 2011), atomic fluorescence spectrometry (Deng, Chen, and Belzile 2001), inductively coupled plasma optical emission spectrometry (ICP OES) (Menegario et al 2006;Menegario et al 2008;Depoi and Pozebon 2012), and inductively coupled plasma-mass spectrometry (ICP-MS) (Westerhoff et al 2008). Spectrometric techniques have been used for the speciation of Sb (Feng et al 1999;Menegario et al 2006;Zheng et al 2006;Flores et al 2007;Menegario et al 2008 Ferreira et al 2011) using hydride generation (HG) systems with adequate sensitivity.…”