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A simple and inexpensive chromium-reducible sulfur method for acid-sulfate soils

- Burton, Edward, Sullivan, Leigh, Bush, Richard, Johnston, Scott, Keene, Annabelle

  • Authors: Burton, Edward , Sullivan, Leigh , Bush, Richard , Johnston, Scott , Keene, Annabelle
  • Date: 2008
  • Type: Text , Journal article
  • Relation: Applied Geochemistry Vol. 23, no. 9 (2008), p. 2759-2766
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  • Description: A new chromium-reducible sulfur (CRS) method suitable for the quantification of reduced inorganic S (RIS) in acid-sulfate soils is presented. The new method utilises the reduction of RIS by an acidic Cr(II) solution within a sealed reaction chamber and diffusion of the produced H2S(g) into an alkaline Zn solution. It offers rapid sample processing times, without the need for large volumes of high-purity N2(g) or for specialized, expensive glassware. Examination of pyrite-talc mixtures containing up to 11.8% pyrite, revealed that the method achieves 95-98% recovery of RIS. A comparison between CRS measured by the new diffusion-based method and that measured by a standard purge-and-trap method for 25 pyritic soil samples shows a very strong (r2 = 0.996) linear relationship with a slope of 0.995. The ability of the new diffusion-based CRS method to achieve accurate and precise quantification of RIS in acid-sulfate soils is demonstrated. © 2008 Elsevier Ltd. All rights reserved.

Iron(III) accumulations in inland saline waterways, Hunter Valley, Australia : Mineralogy, micromorphology and pore-water geochemistry

- Isaacson, Lloyd, Burton, Edward, Bush, Richard, Mitchell, David, Johnston, Scott, Macdonald, Bennett, Sullivan, Leigh, White, Ian

  • Authors: Isaacson, Lloyd , Burton, Edward , Bush, Richard , Mitchell, David , Johnston, Scott , Macdonald, Bennett , Sullivan, Leigh , White, Ian
  • Date: 2009
  • Type: Text , Journal article
  • Relation: Applied Geochemistry Vol. 24, no. 10 (2009), p. 1825-1834
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  • Description: Discharge of Fe(II)-rich groundwaters into surface-waters results in the accumulation of Fe(III)-minerals in salinized sand-bed waterways of the Hunter Valley, Australia. The objective of this study was to characterise the mineralogy, micromorphology and pore-water geochemistry of these Fe(III) accumulations. Pore-waters had a circumneutral pH (6.2-7.2), were sub-oxic to oxic (Eh 59-453 mV), and had dissolved Fe(II) concentrations up to 81.6 mg L-1. X-ray diffraction (XRD) on natural and acid-ammonium-oxalate (AAO) extracted samples indicated a dominance of 2-line ferrihydrite in most samples, with lesser amounts of goethite, lepidocrocite, quartz, and alumino-silicate clays. The majority of Fe in the samples was bound in the AAO extractable fraction (FeOx) relative to the Na-dithionite extractable fraction (FeDi), with generally high FeOx:FeDi ratios (0.52-0.92). The presence of nano-crystalline 2-line ferrihydrite (Fe5HO3·4H2O) with lesser amounts of goethite (α-FeOOH) was confirmed by scanning electron microscopy (SEM) coupled with energy dispersive X-ray analysis (EDX), and transmission electron microscopy (TEM) coupled with selected area electron diffraction (SAED). In addition, it was found that lepidocrocite (γ-FeOOH), which occurred as nanoparticles as little as ∼5 lattice spacings thick perpendicular to the (0 2 0) lattice plane, was also present in the studied Fe(III) deposits. Overall, the results highlight the complex variability in the crystallinity and particle-size of Fe(III)-minerals which form via oxidation of Fe(II)-rich groundwaters in sand-bed streams. This variability may be attributed to: (1) divergent precipitation conditions influencing the Fe(II) oxidation rate and the associated supply and hydrolysis of the Fe(III) ion, (2) the effect of interfering compounds, and (3) the influence of bacteria, especially Leptothrix ochracea. © 2009 Elsevier Ltd. All rights reserved.

Abundance and fractionation of Al, Fe and trace metals following tidal inundation of a tropical acid sulfate soil

- Johnston, Scott, Burton, Edward, Bush, Richard, Keene, Annabelle, Sullivan, Leigh, Smith, Douglas, McElnea, Angus, Ahern, Col, Powell, Bernard

  • Authors: Johnston, Scott , Burton, Edward , Bush, Richard , Keene, Annabelle , Sullivan, Leigh , Smith, Douglas , McElnea, Angus , Ahern, Col , Powell, Bernard
  • Date: 2010
  • Type: Text , Journal article
  • Relation: Applied Geochemistry Vol. 25, no. 3 (2010), p. 323-335
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  • Description: Tidal inundation was restored to a severely degraded tropical acid sulfate soil landscape and subsequent changes in the abundance and fractionation of Al, Fe and selected trace metals were investigated. After 5 a of regular tidal inundation there were large decreases in water-soluble and exchangeable Al fractions within former sulfuric horizons. This was strongly associated with decreased soil acidity and increases in pH, suggesting pH-dependent immobilisation of Al via precipitation as poorly soluble phases. The water-soluble fractions of Fe, Zn, Ni and Mn also decreased. However, there was substantial enrichment (2-5×) of the reactive Fe fraction (FeR; 1 M HCl extractable) near the soil surface, plus a closely corresponding enrichment of 1 M HCl extractable Cr, Zn, Ni and Mn. Surficial accumulations of Fe(III) minerals in the inter-tidal zone were poorly crystalline (up to 38% FeR) and comprised mainly of schwertmannite (Fe8O8(OH)6SO4) with minor quantities of goethite (α-FeOOH) and lepidocrocite (γ-FeOOH). These Fe (III) mineral accumulations provide an effective substrate for the adsorption/co-precipitation and accumulation of trace metals. Arsenic displayed contrary behaviour to trace metals with peak concentrations (∼60 μg g-1) near the redox minima. Changes in the abundance and fractionation of the various metals can be primarily explained by the shift in the geochemical regime from oxic-acidic to reducing-circumneutral conditions, combined with the enrichment of reactive Fe near the soil surface. Whilst increasing sequestration of trace metals via sulfidisation is likely to occur over the long-term, the current abundance of reactive Fe near the sediment-water interface favours a dynamic environment with respect to metals in the tidally inundated areas. © 2009 Elsevier Ltd. All rights reserved.

Jarosite quantification in soils : An enhanced sequential extraction procedure

- Vithana, Chamindra, Sullivan, Leigh, Bush, Richard, Burton, Edward

  • Authors: Vithana, Chamindra , Sullivan, Leigh , Bush, Richard , Burton, Edward
  • Date: 2014
  • Type: Text , Journal article
  • Relation: Applied Geochemistry Vol. 51, no. (2014), p. 130-138
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  • Description: A two-step sequential extraction procedure established for the quantification of acidity producing ferric and ferrous sulfate minerals such as melanterite and jarosite in acid mine wastes was evaluated for quantification of jarosite spiked in soils. The procedure involves in sequence anoxic water extraction, roasting the solid residue after anoxic water extraction at 550. °C for 1. h, and 4. M HCl extraction of the roasted solid. Soil and quartz samples were spiked with known amounts of synthetic and natural jarosite and their recovery was measured using the suggested two-step sequential extraction procedure. The recoveries of synthetic and natural jarosite were calculated on the basis of the S contents of the initially spiked jarosite in soil and quartz samples. Less than 50% of the spiked jarosite was recovered. The missing S is partially attributable to the retention of jarosite by the Teflon filter membrane used during the filtration of the anoxic water extract. Further investigations also demonstrated a lower 4. M HCl-S extractability from jarosite samples roasted at 550. °C than those roasted at 450. °C. S recovery from jarosite-spiked quartz samples increased to 45-70% by replacing the Teflon filter membrane with the Cellulose Acetate filter membrane and including this filter paper in the second step roasting. This modified method is a step forward in the development of methods to accurately and reliably quantify jarosite in soil materials. © 2014 Elsevier Ltd.
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