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CHLORIDE GENERATION: APPLICATIONS TO SOLID SAMPLING AND SPECIATION IN ATOMIC SPECTROSCOPY

Posted on:1983-03-10Degree:Ph.DType:Dissertation
University:Arizona State UniversityCandidate:BURGE, SCOTT RUSSELLFull Text:PDF
GTID:1471390017963912Subject:Chemistry
Abstract/Summary:
A solid sample volatilizer has been developed for atomic emission spectroscopy. The volatilizer consists of an induction furnace to heat platinum crucibles in the presence of hydrogen chloride gas. The hydrogen chloride gas is used to quantitatively convert the analyte ion to its chloride.;A survey of the literature shows almost all elements will volatilize as their chlorides at temperatures below the maximum reached by the furnace.;A discussion is given on factors affecting the conversion of various salts of Ag, B, Na, Li, Ga, Mn, Ni, Mo, Cr, Ca, Fe, Cu and Pb to their chlorides. Plots of signal height versus absolute mass of analyte demonstrate that the volatilizer is capable of establishing linearity for most elements analyzed with percent relative standard deviation (RSD) better than 10%.;Included in the discussion is a method to separate and quantitate various salts of the same element: Co(NO(,3))(,2) from CoCl(,2), NiCl(,2) from Ni(SO(,4))(,2). In a mixed salt of cobalt containing 5 (mu)g of CoCl(,2) and 5 (mu)g of Co(NO(,3))(,2), the two salts were separated and quantitatively measured with 3% RSD.;(DIAGRAM, TABLE OR GRAPHIC OMITTED...PLEASE SEE DAI).;The volatilizer was used to analyze manganese in steel, and manganese in dunite. Determination of the elements in these matrices was done with better than 6% RSD.
Keywords/Search Tags:Chloride, Volatilizer
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