| 光谱学与光谱分析 |
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| Study on Determination of Molybdenum in Molybdenum Concentrate by Atomic Absorption Spectrometry Indirectly |
| QU Wei, ZHOU Cheng-ying, CAI Liu-lu, LI Wen-juan |
| General Research Institute for Nonferrous Metals, National Engineering Lab of Biohydrometallurgy, Beijing 100088, China |
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Abstract For the determination of molybdenum in molybdenum concentrate，lead molybdate gravimetric method was considered as standard method. In order to ensure the lead ions to be washed thoroughly from the entrained precipitate, lead molybdate precipitate was washed, filtered repeatedly, then ashed and burned. This method cannot satisfy the rapid measurement demand of mineral processing and metallurgy scientific research due to its time consuming. In the present work, molybdenum was determined by atomic absorption spectrometry indirectly and a rapid analysis method for molybdenum in molybdenum concentrate was proposed. The sample was dissolved by nitric acid, potassium chlorate and sulfuric acid, pH was adjusted by acetic acid and ammonium acetate buffer solution to pH 5～7, then a certain amount and excess of lead standard was added. Based on lead molybdate was considered as undissolved electrolyte on room temperature, the solubility of lead molybdate was 1.16×10-5g, far less than 0.01 g, was considered as the undissolved electrolyte, the electrolyte insoluble at a certain temperature can complete precipitation, usually compared with the solubility production product Qc and the relative size of constant Ksp, when Qc>Ksp, solution was supersaturated, precipitation was precipitate completely, the content of molybdenum in molybdenum concentrate was 40%~60%, the amount of lead was 0.125 0~0.150 0 g, took the minimum calculated solution lead molybdate ion product, Qc＝[Pb2+][MoO2-4]=2.51×10-5，Ksp＝1.0×10-13，QcKsp，Therefore lead molybdate precipitate can be precipitated completely, after dry filtered, the excess of lead ions were determined by atomic absorption spectrometry, the content of molybdenum was calculated by subtraction method. In this paper, the amount of acetic acid-ammonium acetate buffer solution, the amount of lead standard, time of lead molybdate precipitation, heating time and maximum amount of coexisting ions such as W6+, Sn4+, Cu2+, etc were investigated. Compared with lead molybdate gravimetric method, repeatedly washing, ashing and burning with lead molybdate were eliminated by proposed method, which was simple, easy to master and was able to cut the analysis time in half. The control experiments were conducted by lead molybdate gravimetric method and proposed method. After the results were implemented by mathematical statistics, it can be concluded that it had good accuracy and precision for the proposed method, which can be applied to rapid analysis of molybdenum in molybdenum concentrate for mineral processing and metallurgy.
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Received: 2016-03-29
Accepted: 2016-08-04
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Corresponding Authors:
QU Wei
E-mail: quwei7017@163.com; quwei7017@sohu.com
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