Graduate Thesis Or Dissertation
 

Part I : development and application of an arsenic speciation technique using ion-exchange solid phase extraction coupled with GFAAS ; Part II : investigation of zinc amalgam as a reductant

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  • Two related techniques, based upon ion-exchange solid phase extraction, have been developed for the determination of arsenic speciation. The inorganic arsenic species arsenite (As(III)) and arsenate (As(V)) are separated by anion-exchange and detected with graphite furnace atomic absorption spectrophotometry (GFAAS) with a nickel matrix modifier. The first separation technique, which is based on a published method, utilizes a strong anion-exchange resin in a column format. The method was refined to achieve a cleaner and more rapid separation of the As species. In the second separation technique, the recently available Empore[superscript TM] anion-extraction disks are used. In both cases, rapid separations of several samples are achieved with the use of a vacuum manifold. The simplicity of the separation techniques allows them to be applied in the field which eliminates potential problems due to sample storage. In the pH range of most natural water samples (5-9), As(III) exists as a neutral species which is not retained by the resin, while As(V) exists as a monovalent or divalent species which are subsequently retained by the resin. The two arsenic species are collected in 3 to 4 fractions with As(III) appearing in the first two fractions. The As(V) species is eluted from the resin with 0.1 M HCl and collected in the last one or two fractions. Percent recoveries for each species range from 94 to 99%. The detection limit for each species with GFAAS is 2 μg/L. The speciation techniques were used successfully in several applications. First, the resin technique was used to monitor the oxidation of As(III) by 0₂, H₂0₂, and δ-Mn0₂. The technique was also used to monitor the reduction of As(V) by Fe(II) and in solutions containing combinations of Fe(II), Fe(III), and a scorbic acid. Second, the resin technique was used to monitor the redox behavior of arsenic in soil slurries in bio-reactor systems. Upon spiking the soil slurry to a level of 500 μg/L As(V), 80 to 90% of the As(V) was immediately adsorbed, presumably to hydrous Fe(III) oxides. In general, as conditions became more reducing, total soluble arsenic increased as a result of either abiotic or biotic reduction of the As(V) to the more soluble As(III). Third, the disk technique was applied in the field to determine arsenic speciation in creek water at Sutter Creek, Ca., where homes are built upon a large pile of mine tailings containing arsenic. In the creek water, no As(III) was detected but As(V) was detected at a level of 8 μg/L. Fourth and finally, the resin technique was used to determine arsenic speciation when a sample of the mine tailings was placed in a reactor and combined with a soil slurry thus simulating a flooded condition. As conditions became more reducing, up to 800 μg/L As was detected in solution with As(III) accounting for almost 90% of total soluble species. Also presented here is an investigation of zinc amalgam as a reducing agent for Cr(III) and selected redox indicators. Zinc amalgam, in a column format, also known as the classic Jones Reductor, provides an efficient means for production of Crap and reduced forms of various redox indicators. Finally, the reduction capabilities of Ti(III) citrate and zinc amalgam were compared.
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