Determination of total antimony and inorganic antimony species by hydride generation in situ trapping flame atomic absorption spectrometry: a new way to (ultra)trace speciation analysis

Abstract

The analytical performance of non-chromatographic coupled hydride generation, integrated atom trap (HG-IAT) atomizer flame absorption spectrometry (FAAS) systems were evaluated for the speciation analysis of antimony in environmental samples. Antimony, using formation of stibine (SbH 3 ) vapors were atomized in an air-acetylene flame-heated IAT. A new design of HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangements (a water-cooled single silica tube, double-slotted quartz tube or an ''integrated trap'') was investigated. For the estimation of Sb(III) and Sb(V) concentrations in samples, the difference between the analytical sensitivities of the absorbance signals obtained for antimony hydride without and with previous treatment of samples with L-cysteine can be used. The concentration of Sb(V) was calculated by the difference between total Sb tot and Sb(III). A dramatic improvement in detection limit was achieved compared with that obtained using either of the atom trapping techniques, presented above, separately. This novel approach decreases the detection limit down to low pg mL À1 levels. The concentration detection limit, defined as 3 times the blank standard deviation (3sigma), was 0.2 ng mL À1 . For a 120 s in situ pre-concentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 550 fold for Sb, using hydride generation-atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed by RSD, was 8.0% (n = 6) for Sb. The designs studied include slotted tube, water-cooled single silica tube and integrated atom traps. Reference and real sample materials were analyzed. The accuracy of the method was verified by the use of certified reference materials (NIST SRM 2704 Buffalo River Sediment, SRM 2710 Montana Soil, SRM 1633a Coal Fly Ash, SRM 1575 Pine Needles, SRM 1643e Trace Elements in Water) and by aqueous standard calibration technique (solutions). The measured Sb content, in reference materials, were in satisfactory agreement with the certified values. The hyphenated technique was applied for antimony determinations in soil, sediment, coal fly ash, sewage and river water.

Vapor generation and atom traps: Atomic absorption spectrometry at the ng/L level

“…The research group of Matusiewicz in Poland continues to study the development and application of integrated atom traps (IAT) in conjunction with vapor generation techniques; the device has recently been used for the determination of Cd and Pb [56], In and Tl [57], Te [58], Sb [59], Bi [60], As and Se [61]; in these studies a flame atomizer was used.…”

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.…”

“…In order to generate volatile hydrides, the most common procedure for the determination and speciation of antimony involves the use of sodium tetrahydroborate (Feng et al 1999;Deng, Chen, and Belzile 2001;Flores et al 2002;Menegario et al 2006;Matusiewicz and Krawczyk 2008;Menegario et al 2008;D'Ulivo et al 2011;Ferreira et al 2011). The method is based on the reduction of Sb(III) in acid or neutral solution to produce volatile stibine (SbH3).…”

“…Hence, these differences in the oxidation states of Sb are extremely important in speciation. Consequently, the analytical conditions for the hydride generation have been studied for speciation (Feng et al 1999;Deng, Chen, and Belzile 2001;Flores et al 2002;Fuentes et al 2003;Menegario et al 2006;Matusiewicz and Krawczyk 2008; (Smichowski 2008;Ferreira et al 2014). However, no discrimination is made between Sb(III) and Sb(V) in drinking water, with a level of 6.0 g L 1 for total antimony by the United States Environmental Agency (EPA 2014) and 5.0 g L 1 by the Health Ministry in Brazil (Brazil 2011).…”

Surface-enhanced Raman spectra of a complex of antimony with phenylfluorone and their interpretation

“…These are spectrophotometry [4], atomic absorption spectrometry [5][6][7], atomic fluo rescence spectrometry [8,9], optical emission and mass spectrometry with inductively coupled plasma [10], fluorometry [11], neutron activation analysis [12], and so on. Many of these techniques are charac terized by a high efficiency and accuracy of the analy sis and good selectivity, with the volume of the sample under study being comparatively small.…”