Determination of antimony in plant and peat samples by hydride generation-atomic fluorescence spectrometry (HG-AFS)

Abstract

A robust and sensitive analytical procedure for the determination of Sb in plant and peat samples using hydride generation-atomic fluorescence spectrometry (HG-AFS) has been developed. The hydride generation of Sb was carried out by using 1% (m/v) of NaBH 4 and 4 mol l 21 HCl. The analytical procedure was critically evaluated by analysing five certified plant reference materials (BCR CRM 281 Rye Grass, CTA-VTL-2 Virginia Tobacco Leaves, GBW 07602 Bush Branches and Leaves, SRM 1547 Peach Leaves and SRM 1515 Apple Leaves) and two in-house peat reference materials. The accuracy and precision (v3%) of the developed procedure was evaluated by the determination of Sb in certified reference materials, two in-house reference materials, and showed good agreement with the reference and information values. Prior to HG-AFS, 200 mg aliquots of dried samples were digested with 3 ml nitric acid, 0.5 ml hydrogen peroxide and 0.1 ml tetrafluoroboric acid (HBF 4 ) using closed-pressurized digestion in a microwave oven. The efficiency of applying HBF 4 for destroying silicates in the samples was also investigated. The digests of the samples were first diluted to 10 ml using high purity water, subsequently mixed with 1 ml of 50 g l 21 L-cysteine for the pre-reduction of Sb(V) in the digests, and finally diluted to 50 ml using 4 mol l 21 hydrochloric acid for measurement. A solution detection limit of 8 ng l 21 was obtained using the optimised experimental conditions which corresponds to a method detection limit of 2 ng g 21 in solid peat: this detection limit is far lower than those previously reported for this element using the identical HG-AFS instrument. The newly developed analytical procedure has been applied to the determination of Sb in ancient peat samples collected from remote Scottish peat bogs. The high sea salt content of these peat samples caused no matrix interferences. Comparison of the results obtained using HG-AFS with instrumental neutron activation analysis (INAA) data obtained previously shows that the lower limits of detection of INAA are unsuitable for measuring Sb in pre-anthropogenic samples.

Antimony in recent, ombrotrophic peat from Switzerland and Scotland: Comparison with natural background values (5,320 to 8,020 14C yr BP) and implications for the global atmospheric Sb cycle

“…(a) Sb or Sc concentrations (μg/g) in the peat profiles from LL and FL. Acid digests were measured twice using HG‐AFS [ Chen et al , 2003] and the results averaged. (b) Pb concentrations (μg/g) for the same profiles.…”

“…With respect to the 2P core (deeper, older peat layers), the HG‐AAS data is presented here because it is much more accurate than the INAA data at low Sb concentrations. Antimony was measured in the two peat cores from Scotland using HG‐AFS as described in detail by Chen et al [2003].…”

“…For comparison with these central European sites, we also present new Sb and Sc concentration data from peat bogs in NW Scotland and the Shetland Islands. The Sb concentration data for the Scottish peat cores was obtained using a new analytical procedure employing hydride‐generation atomic fluorescence spectrometry (HG‐AFS) which provides a detection limits for Sb in peat of only 2 ng/g [ Chen et al , 2003]. We show that the chronology of Sb contamination in Scotland is similar to that of Pb.…”

Antimony speciation in terrestrial plants. Comparative studies on extraction methods

“…4 Some research has been reported on the determination of total antimony in plants. [5][6][7][8][9][10][11][12][13][14][15][16][17][18] In terrestrial vascular plants, the background antimony content was found to range from 0.2 to 50 mg kg À1 . [5][6][7] Higher contents were found in grasses growing around lead and antimony smelters [8][9][10] and in plants grown on contaminated soils from mining activities.…”

Study on transformation and enrichment behavior of selenium in particulate matter in combustion flame

“…Hydride generation atomic fluorescence spectrometry HG-AFS has been widely used in the analysis of trace elements and was used to measure the samples at different heights in the flame (Chen, Yuan, and Wang 2012;Wu 2004). The carrier liquid for AFS consisted of HCl and KBH 4 , which can react to generate hydrogen.…”