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Applications Of Solution Cathode Glow Discharge-Atomic Emission Spectrometer In The Analysis Of Ceramic Material

Posted on:2016-12-12Degree:MasterType:Thesis
Country:ChinaCandidate:R Y GeFull Text:PDF
GTID:2191330464463092Subject:Chemical Engineering
Abstract/Summary:PDF Full Text Request
Glow discharge (GD) source has shown impressive analytical performance, cost effectiveness, and versatility in the earlier studies. The Glow discharge (GD) source has been used as the source of atomic emission spectroscopy and mass spectroscopy analysis. But the traditional Glow discharge (GD) source has been ill-suited for the analysis of liquids and solutions. In 1993, Cserfalvi introduced a new kind of Glow discharge (GD) source which one pole of the discharge if liquid. The new Glow discharge (GD) source was named as electrolyte cathode discharge (ELCAD) and was used as the source of atomic emission spectroscopy analysis at the same time. The electrolyte cathode discharge (ELCAD) source has been widely improved in the last two decades.The Solution Cathode Glow Discharge-Atomic Emission Spectroscopy (SCGD-AES) is a new kind of electrolyte cathode discharge (ELCAD) source. The SCGD-AES has shown high sensitivity, low operating cost and simple equipment in the earlier studies. The SCGD-AES has the potential in making up the shortfall of traditional analysis method, such as atomic absorption spectroscopy (AAS), inductively coupled plasma-atomic emission spectroscopy (ICP-AES), inductively coupled plasma-mass spectroscopy (ICP-MS).The author has improved the SCGD-AES which has been structured by the earlier researcher and determinate the trace elements in the Lutetium-Yttrium Orthosilicate (LYSO) and Titanium dioxide (TiO2) samples. The LYSO and TiO2 matrix tolerance of the SCGD-AES were investigated. The sensitivity enhancement for Pb with the addition of formic acid was researched at the same time.By the improvement of SCGD-AES, the SCGD-AES has shown better stability and determination become more convenient and less sample needed. The optimal conditions utilized 0.1 mol·L-1 HNO3 sample solutions and operated at a voltage of 1080 V with a flow rate of 2.0mL·min-1. The relative standard deviations are better than 5%for continuous eleven measurements of 10 ppm standard solution.The TiO2 matrix tolerance for SCGD source stability was optimized. The trace Ag, Ca, Cu, Fe, K, Li, Mg, Na, and Pb in TiO2 samples and certified reference material were determined. The enhancement of Pb sensitivity was also studied. Specifically, the limit of detection for Pb improved 6.5-fold with the addition of 3%(v/v) formic acid. The values obtained by SCGD-AES were close to those obtained by ICP-AES and the certified values. The detection limits of the trace elements such as Ag, Ca, Cu, Fe, K, Li, Mg, Na, and Pb in TiO2 powders were 0.08,2,2,5,0.04,0.02,0.04,0.02, and 0.4 g g-1, respectively.The LYSO matrix tolerance for SCGD source stability was optimized. The trace Ca, Fe, K, Li, Mg, Na in LYSO samples were determined. The values obtained by SCGD-AES were close to those obtained by ICP-AES. The detection limits of the trace elements such as Ca, Fe, K, Li, Mg, Na in LYSO samples were 1,3,0.02,0.01,0.02,1 g g-1, respectively.The SCGD-AES has showed many advantages in the determination of real samples, such as high sensitivity, less spectral interference, multi-element analyst at the same time, and so on. The SCGD-AES is a kind of analyst instrument which has showed potential.
Keywords/Search Tags:Solucion Cathode Glow Discharge, Lutetium-Yttrium Orthosilicate, Titanium dioxide
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