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Graphite Furnace Atomic Absorption Spectroscopy For Ceramic Materials

Posted on:2011-11-22Degree:MasterType:Thesis
Country:ChinaCandidate:G P LuFull Text:PDF
GTID:2191330332972922Subject:Chemical processes
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Advanced ceramics have been utilized in various important fields such as information science, eronautics and astronautics, life sciences. However, the mechanical, thermal, electrical, magnetic, and optical properties of ceramics are significantly affected by the chemical composition and impurities existed in the material even at very low concentration level. Thus,it is essential to determine trace impurities to characterizes the quality of ceramics.Routine analysis demands the sample in form of solution. However, it is chemically difficult to bring sample into dissolution because of physical and chenmiatry properties. Slurry sampling was already considered as a mature technique, due to combining the significant advantages of the solid and liquid sampling methods and allowing several replicates from just only one slurry and higher amounts of sample can be weighted. It was widely utilized for metal determination in trace and even ultra trace analysis in organic and inorganic complicated matrix, even for routine analysis.Graphite Furmace Atomic Absorption Spectrometry (GFAAS) has been shown to be the most attractive technique for the direct analysis of solid samples, mainly by the absence of a nebulizer system which simplifies the introduction of the solid material into the atomizers. Additionally, the large residence time of the sample into the GFAAS atomizer allows the particles to be atomized whatever their size or volatility. Moreover, it shows quite low limits of detection,high selectivity and sensitivity, which is highly desirable in trace analysis. Due to all these attributes solid analysis by GFAAS is now an accepted methodology and a very convenient way for the determination of trace elements in a broad range of solid materials.The slurry analysis involves by far more problems related to non-specific absorption than the analysis of solutions (or acid extracts) does. Accordingly, the graphite furnace temperature programme is really difficult to avoid the analyte and matrix simultaneous atomization, so an efficient background corrector is imperative. In this wok, Smith-Hieftje background correction (S-H) and Zeeman effect corrector were used.High-purity alumina and silicon carbides was considered to be the most refractory ceramic materials. Direct determination the inpurities in ceramics of was performed by slurry-GFAAS with subsequent to decomposition by sulfuric acid in PTFE pressure vessels and slury sampling. The silicon carbides slurry sample was prepared with adding dispersant Polyacrylic amine (NH4PAA) polyethyleneimine (PEI),respectively,and agitation in an vortex mixer to ensure for the dispersion,stabilization and homogenization of suspension, Zirconium coating as a permanent modifier showed that the improvement in analytical firings of the tube.Instrument conditions of GFAAS such as pyrolysis, atomization and hollow cathode lamp current has been optimized, the optimal experimental conditions were selected. Calibration was performed using aqueous standards method for sample analysis. The accuracy of the proposed method was shown up for the case of Al2O3 (AKP-30),SiC (BAM-S003), and compared with those obtained by GFAAS, the results were in agreement well with values found in the literature by different methods. The linear regression coefficients of the calibration curves were better than 0.999. The detection limits were low, with a relative standard deviation were being not more than 6.6%.It is a simple, convenient and accurate method and it is suitable for the rapid analysis of trace element in ceramics.
Keywords/Search Tags:Advanced ceramics, Slurry, Graphite Furnace Atomic Absorption Spectrometry, Smith-Hieftje background correction, Zeeman effect corrector, permanent modifier
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