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  • 1
    Publication Date: 2014-02-04
    Description: A neutral polystyrene resin column, dynamically loaded with dipicolinic acid at a concentration of 0.1 mM in 1 M potassium nitrate eluent, was investigated for the separation characteristics of a number of high valence metal cations over the pH range 0-3. The metal species studied were Th(IV), U(VI), Zr(IV), Hf(IV), Ti(IV), Sn(IV), V(IV) and V(V), Fe(III) and Bi(III), of which Ti(IV), Sn(IV), V(IV) and Fe(III) did not show any retention. For the remaining metal ions, significant retention was obtained with good peak shapes, except for Th(IV), which moved only slightly from the solvent front with some tailing. The retention order at pH 0.3 was Th(IV) 〈 V(V) 〈 Bi(III) 〈 U(VI) 〈 Hf(IV) 〈 Zr(IV). A notable feature of this separation system was the high selectivity shown for uranium, zirconium and hafnium, the last two being nearly resolved in 15 min on the relatively short 10 cm column.
    Type: Article , PeerReviewed
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  • 2
    Publication Date: 2014-02-04
    Description: Flow injection with chemiluminescence detection (FI-CL) was used to determine cobalt and iron in estuarine and coastal waters. Cobalt(II) was determined by means of a pyrogallol-hydrogen peroxide-sodium hydroxide reaction in the presence of methanol and the surfactant cetyltrimethylammonium bromide (CTAB). With pyrogallol, the sensitivity was enhanced compared with the traditional reagent, gallic acid. The practical limit of detection in sea-water was 5 pM (3s) and there was good agreement with certified values for the sea-water CRMs NASS-5 (0.16 ± 0.01 nM), CASS-3 (0.60 ± 0.09 nM) and SLEW-2 (0.93 ± 0.13 nM). Results for an Irish Sea sample gave good agreement with data obtained using cathodic stripping voltammetry. Iron(II + III) was determined using a luminol reaction with dissolved oxygen as the oxidant. The practical limit of detection was 40 pM (3s) and results from shipboard analysis of the CRM NASS-4 (1.95 ± 0.14 nM) were in good agreement with the certified value (1.88 ± 0.29 nM). Field evaluation of the instrumentation and analytical methods was achieved through a series of local surveys in the Tamar Estuary (UK), from which environmental data are presented.
    Type: Article , PeerReviewed
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  • 3
    Publication Date: 2014-02-04
    Description: This work presents the optimisation, validation and field deployment of a voltammetric in situ profiling (VIP) system for the simultaneous determinations of dynamic Cd(II), Cu(II) and Pb(II) in estuarine and coastal waters. Systematic studies in NaNO3 (as a supporting electrolyte) and seawater, indicated that variations in ionic strength, pH and dissolved oxygen did not affect the response of the instrument, whereas an Arrhenius type temperature response was observed. The VIP instrument allows the determination of 2-3 samples h-1, and has a detection limit (defined as 3σ) in seawater for Cd(II): 23 pM, Cu(II): 1.13 nM, and Pb(II): 23 pM. The VIP system accurately measured the total dissolved concentrations of Cd(II), Cu(II) and Pb(II) in two certified reference materials; SLRS-3, a river water, and SLEW-2, an estuarine water. Field evaluation of the instrumentation and analytical methods was achieved through a series of surveys in the Plym Estuary (Devon, UK), from which environmental data are presented.
    Type: Article , PeerReviewed
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  • 4
    Publication Date: 2014-02-04
    Description: The applicability of environmental scanning electron microscopy (ESEM; imaging of hydrated samples) and conventional high vacuum scanning electron microscopy (SEM; imaging of dried samples at high vacuum) for the observation of natural aquatic colloids and particles was explored and compared. Specific attention was given to the advantages and limitations of these two techniques when used to assess the sizes and morphologies of complex and heterogeneous environmental systems. The observation of specimens using SEM involved drying and coating, whereas ESEM permitted their examination in hydrated form without prior sample preparation or conductive coating. The two techniques provided significantly different micrographs of the same sample. SEM provided sharper images, lower resolution limits (10 nm or lower), but more densely packed particles, suggesting aggregation, and different morphological features than ESEM, suggesting artefacts due to drying. ESEM produced less easily visualised materials, more complex interpretation, slightly higher resolution limits (30-50 nm), but these limitations were more than compensated for by the fact that ESEM samples retained, at least to some extent, their morphological integrity. The results in this paper show that SEM and ESEM should be regarded as complementary techniques for the study of aquatic colloids and particles and that ESEM should be more widely applied to aquatic environmental systems than hitherto. © The Royal Society of Chemistry 2005.
    Type: Article , PeerReviewed
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  • 5
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    Royal Society of Chemistry
    In:  In: Metallothioneins and Related Chelators. , ed. by Sigel, A., Sigel, H. and Sigel, R. K. O. Royal Society of Chemistry, Cambridge, UK, pp. 441-482. ISBN 978-1-84755-899-2
    Publication Date: 2017-10-24
    Type: Book chapter , NonPeerReviewed
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