2016年8月22日星期一

TZM Alloy Ti and Zr Determination by ICP-AES Method

In TZM alloy Ti and Zr content have great impact on its performance and through ICP-AES (Inductively Coupled Plasma - Atomic Emission Spectrometry) method can accurate measurement Ti and Zr content. ICP-AES has high sensitivity, high precision and wide linear working range and other properties, so it has widely application range.
Experimental Method: Weighed 0.2000g sample in 100ml beaker, added 2ml of sulfuric acid and 1g ammonium sulfate, and then placed on electric hot plate for heating. After the sample dissolved and cooled, poured into 100ml volumetric flask, diluted with water to the mark, for analysis.
Dissolving acid selection: The molybdenum alloy can dissolve by sulfuric acid - ammonium sulfate or nitrate - hydrofluoric acid mixture, but using nitric acid - hydrofluoric acid should ensure that sufficient amount of acid can make the sample completely dissolved. The viscosity of sulfuric acid is large, which is difficult to improve during lifting injections, but the amount is small, the results less affected. Overall consideration, the experiments will 2ml of sulfuric acid and 1g ammonium sulfate to dissolved molybdenum alloy.
Analytical line selection: To scan the spectral line by molybdenum, titanium, zirconium solution provided with the spectrum library, according to the shape of the peak, and condition of the peak value and matrix line to compare the interference of the matrix to the peak to chose small interference spectrum line, so choose 336.1nm as titanium determination spectral line, 343.8nm as zirconium determination spectral line.
Used ICP-AES method for Ti and Zr measurement and the values shows on the table. The recovery rate 98.33% -110.00%, RSD (n = 5) were less than 2.0%. This method avoids the conventional chemical analysis cumbersome process and greatly reduces the analysis time, which can simultaneously to measure Ti and Zr elements, so this method not only has fast, flexible and convenient features, but also can save a lot of manpower, reducing reagent consumption, improving the detection efficiency.

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