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Biodiesel purification processes generate wastewater streams that require a large amount of energy when distillation is used as a treatment technology. Process simulation software was used to show that an alternative water treatment process involving ion exchange would require only 31% of the energy used by distillation. Experiments showed that multiple washing stages were required to meet the standard specification for sodium, an impurity present in crude biodiesel, when washing biodiesel made from used frying oil. A comparison was made between washing biodiesel in a cross-current washing configuration and a counter-current configuration. Both configurations met the specification for sodium within three washing stages; however, the counter-current configuration required less water, making it the more efficient process. Lastly, the removal of sodium from wastewater samples using an ion exchange resin was experimentally investigated. The results validated the use of ion exchange to reduce energy consumption in biodiesel purification.

In order to increase the current efficiency in copper electrowinning tankhouses, iron can be removed from the electrolyte using ion exchange. While this is a proven technology, very little data is available for the application of this technology to copper electrowinning electrolytes containing antimony and bismuth. The feasibility of utilizing iron ion exchange for the removal of iron from copper electrowinning electrolytes containing antimony and bismuth was studied in the laboratory. Apicolylamine, a sulphonated diphosphonic, an aminophosphonic and three sulphonated monophosphonic resins were tested. The picolylamine resin was found to be completely impractical as it loaded high levels of copper. All the phosphonic resins tested loaded an appreciable amount of antimony, however, only the aminophosponic resin loaded an appreciable amount of bismuth. Tests to determine whether or not the sulphonated monophosphonic Purolite S957 resin would continue to load antimony with time and, hence, reduce the resin's ability to remove iron gave inconclusive results. In the event that the resin's ability to remove iron is hampered due to antimony loading, testing has shown that the resin performance may be restored via a regeneration with a solution containing sulphuric acid and sodium chloride. A case study for the application of this technology to the CVRD Inco CRED plant has shown that, while iron removal by ion exchange is technically feasible, it will upset the plant's acid balance in electrolyte. Therefore, an acid removal process would need to be implemented in tandem with an iron ion exchange system. Additionally, preliminary calculations suggest that a system with a single ion exchange column may have difficulty removing sufficient iron for the CRED design conditions. Therefore, consideration should be given to the possibility of utilizing a two column system (one column loading, one column stripping).

Biodiesel purification processes generate wastewater streams that require a large amount of energy when distillation is used as a treatment technology. Process simulation software was used to show that an alternative water treatment process involving ion exchange would require only 31% of the energy used by distillation. Experiments showed that multiple washing stages were required to meet the standard specification for sodium, an impurity present in crude biodiesel, when washing biodiesel made from used frying oil. A comparison was made between washing biodiesel in a cross-current washing configuration and a counter-current configuration. Both configurations met the specification for sodium within three washing stages; however, the counter-current configuration required less water, making it the more efficient process. Lastly, the removal of sodium from wastewater samples using an ion exchange resin was experimentally investigated. The results validated the use of ion exchange to reduce energy consumption in biodiesel purification.

Thesis (Ph. D.)--University of Texas at Austin, 2001. / Vita. Includes bibliographical references. Available also in a digital version from Dissertation Abstracts.

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This investigation has produced four major results: (1) Thermodynamic properties of chromium metal, aqueous ions, hydrolysis species, oxides and hydroxides were compiled. Data were critically evaluated, some data were recalculated, and thermodynamic properties were selected. (2) A method was developed for separating chromium from its natural water matrix using sequential anion and cation exchange chromatography. (3) A method for determining the ⁵³Cr/⁵²Cr ratio using solid-source thermal ionization mass spectrometry with the silica gel-boric acid ionization- - enhancement technique was developed. (4) Ground water samples from six locations were analyzed for their ⁵³Cr/⁵²Cr ratio using the above methods. Results from carefully measured electromotive force (emf) values for the reduction of Cr³⁺ to Cr²⁺ were recalculated for compatibility with the infinite dilution standard state, and a revised ∆G°(f) for Cr²⁺(aq) was calculated. Equilibrium constants for chromium(III) hydrolysis were taken from Rai, et al. (1987) and for chromium(VI) hydrolysis from Palmer, et al. (1987). The ion exchange method is based on retention of chromium(VI) on strongly basic anion exchange resin at pf1 4 and its reductive elution with 2N HNO₃ . Chromium(III) is retained on strongly acidic cation exchange resin at pH 1.3 and eluted with 5N HNO₃. Possible interferents include metals that form both oxyanions and cations. High-purity reagents and containers made of rigorously cleanable noncontaminating materials are required. Samples for mass spectrometry are pretreated with aqua regia and concentrated nitric acid, then mixed with silica and boric acid and transferred to the tantalum filament of a stainless steel and glass sample holder. The ⁵³Cr/⁵²Cr ratio was measured to avoid isobaric interferences with iron. To be significantly different from each other, isotopic signatures must differ by at least 0.5 per mil. Samples from six locations were examined for their ⁵³Cr/⁵²Cr ratio. For the samples with natural origin, the spread in δ⁵³Cr values of-2.0 to +3.0 per mil suggests that samples of chromium derived from differing source materials or from different geographic locations have distinct isotopic signatures. Conclusions regarding source-related variations in the isotopic signature of contaminant chromium are problematic, because specific information about the respective source materials is lacking.

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The aim of the work described in this thesis was to study the removal of ammonium ions from water by ion exchange. The classical technique is to use biological nitrification and denitrification to convert ammonia into nitrogen gas. Removal by ion exchange offers a number of advantages, such as the ability to handle shock loadings and to polish water to a very high specification. The ion exchanger used in this project was clinoptilolite, a naturally occurring zeolite. Previous research has included characterisation of clinoptilolite, the effect of other common cations on uptake, biological regeneration, and a few other studies. A comparison with other exchangers was also conducted. Much of the available literature is concerned with clinoptilolite and occasionally with mordenite, however modern ion exchangers are polymer based. Two polymeric ion exchangers (Dowex 50w-x8, and Purolite MN500) were evaluated in this project. The main scope of this thesis was to look at the effect that organic pollutants has on ammonium ion removal during ion exchange. The results of batch equilibrations of NH4+ and the three exchanger resins can be seen in chapter 4.0. They show that the presence of an organic compound enhanced the uptake of NH4+ in most cases onto clinoptilolite and Purolite MN500. There was no apparent uptake onto Dowex 50w-x8. Further experiments with a sample of real industrial wastewater (woolscour wastewater) showed varied results, showing that each site should carry out its own pilot scale testing during plant design. Other experimental work showed that the exchanger resins adsorb little or none of the organic compounds in solution. These results can be seen in chapter 5.0. ii Removal of ammonia from wastewater by ion exchange in the presence of organics. Studies in a packed column showed that the presence of organic compounds had little or no effect on NH4+ removal. There was however an increase in capacity after each regeneration of the bed and continued removal after breakthrough. The same results were achieved in the control experiment with no organic compounds present, hence these results are not related to the presence of an organic compound. The presence of NH4+ and various compounds did however provide micro-organisms with substrates from which to grow causing hydraulic difficulties in the column. See chapter 6.0 for these results. The final section of experimental work studied whether the presence of organic compounds changed the rate of uptake of NH4+. The results in chapter 7.0 show that there was no effect on the rate of NH4+ uptake.