| dc.contributor.author | Goodwin, Wayne Eldon. | en_US |
| dc.date.accessioned | 2014-10-21T12:35:09Z | |
| dc.date.available | 1997 | |
| dc.date.issued | 1997 | en_US |
| dc.identifier.other | AAINQ24741 | en_US |
| dc.identifier.uri | http://hdl.handle.net/10222/55478 | |
| dc.description | Reversed-phase extraction chromatographic (RPEC) methods have been developed for the simultaneous determination of trace elements in natural and potable water samples. The elements are collected on a column of Amberlite XAD-4 resin impregnated with 1-(2-thiazolylazo)-2-naphthol (TAN), and then determined by neutron activation analysis (NAA). | en_US |
| dc.description | The synthesis of the resin involves the equilibration of precleaned XAD4 resin with a solution of TAN in methanol for two hours, followed by the addition of water to the mixture and a second two-hour equilibration. The adsorption isotherms for TAN on XAD4 have been evaluated using a variety of solvent systems. The various factors such as solvent polarity, concentration of TAN in solution, and shaking time, which control the loading of TAN on the resin have been investigated. An optimized synthesis procedure has been developed which yields a high-capacity TAN-XAD-4 resin reproducibly. The TAN-loaded support has a copper exchange capacity of 0.1-0.2 mmol g$\sp{-1}$ resin, and is therefore suitable for the concentration of trace elements from water samples. | en_US |
| dc.description | Several parameters which can influence the recovery of trace elements have been studied in detail. These include pH, flow rate, column height, and salinity. It has been found that cadmium, cobalt, copper, manganese, mercury, nickel, and zinc can be simultaneously and quantitatively recovered from solutions of pH $>$ 7.5. Silver (pH 6.1-7.3) and uranium (pH 4.5-5.5) were also quantitatively retained by the resin at appropriate pH. The preconcentration NAA (PNAA) method developed is simple, rapid, and provides a solid sample free of major and interfering elements such as Na and Mg, so that quantification of trace elements in saline samples such as seawater is also feasible. | en_US |
| dc.description | An internal quality assessment procedure of the PNAA method has been devised. Various steps of the method have been critically examined using comparator standards. All chemicals and reagents used have been analyzed for elemental contaminants. Procedural blanks have been routinely determined. The precision of the method has been evaluated by replicate analysis of spiked samples and tap water, and found to be generally within $\pm$6% RSD. External quality assessment of the PNAA procedure has been carried out by analyzing reference materials. The results obtained in this study are in good agreement with the certified values, generally within $\pm$10%. The detection limits of the PNAA methods have been found to range between 0.014 $\mu$g for uranium and 7.57 $\mu$g for nickel. Enrichment and decontamination factors for the PNAA method have been calculated. | en_US |
| dc.description | One of the main advantages of coupling the RPEC procedure to NAA is the ability to quantify elements in a solid sample Consequently, the resin can be irradiated directly, thereby eliminating the need for an elution step which can give irreproducible recoveries and high reagent blanks. The PNAA method has been applied to the determination of trace elements in river water and tap water to demonstrate its practical applicability. | en_US |
| dc.description | Thesis (Ph.D.)--Dalhousie University (Canada), 1997. | en_US |
| dc.language | eng | en_US |
| dc.publisher | Dalhousie University | en_US |
| dc.publisher | | en_US |
| dc.subject | Chemistry, Analytical. | en_US |
| dc.title | Preconcentration neutron activation analysis of trace elements with 1-(2-thiazolylazo)-2-naphthol using reversed-phase extraction chromatography. | en_US |
| dc.type | text | en_US |
| dc.contributor.degree | Ph.D. | en_US |
