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    碱熔-离子交换树脂分离-电感耦合等离子体原子发射光谱法测定钨钼矿石中的钨、钼、硼、硫和磷

    Determination of Tungsten, Molybdenum, Boron, Sulfur and Phosphorus in Tungsten Molybdenum Ores by Inductively Coupled Plasma Atomic Emission Spectrometry Combined with Alkali Fusion and Separation using Ion Exchange Resin

    • 摘要: 称取0.500 0 g样品置于镍坩埚中,加入2.5 g氢氧化钠,再覆盖0.5 g过氧化钠,盖好坩埚盖,置于马弗炉中,升温至700℃并保持7 min,取出冷却,用50 mL热水溶解熔融物,将溶液转移至100 mL塑料容量瓶中,用水定容,摇匀后静置。移取10 mL上清液,加入5 mL已处理好的732树脂溶液,振荡20 min,用水定容至20 mL,再振荡10 min,离心,上清液供电感耦合等离子体原子发射光谱分析。选择B 249.772 nm,W 207.912 nm,Mo 203.846 nm,P 213.618 nm,S 181.972 nm为分析线。钨、钼、硼、硫和磷的质量浓度在一定范围内与其发射强度呈线性关系,检出限(3s)分别为15,11,6,34,23 μg·g-1。方法用于测定钨钼矿石国家一级标准物质中的钨、钼、硼、硫和磷,测定值与认定值的相对误差在-3.2%~2.0%之间,测定值的相对标准偏差(n=11)小于3.0%。方法用于同时测定钨钼矿石样品中的钨、钼、硼、硫和磷,结果与采用传统方法分别测定上述5种元素的结果相符。

       

      Abstract: The sample (0.500 0 g) was palced in a nickel crucible, and 2.5 g of sodium hydroxide was added, and the sample was covered with 0.5 g of sodium peroxide. The crucible was covered with the lid, and then placed in a muffle furnace, warmed up to 700℃ and kept at 700℃ for 7 min. After the crucible was taken out and cooled, the molten material was dissolved with 50 mL of hot water, the solution was transferred to a 100 mL plastic volumetric flask and diluted to 100 mL with water. The solution was shaken for mixing well, and let stand. 10 mL of the supernatant was taken and 5 mL of the treated 732 resin solution was added. The mixture was shaken for 20 min, diluted to 20 mL with water, and shaken for another 10 min. After centrifuge, the supernatant was analyzed by inductively coupled plasma atomic emission spectrometry. B 249.772 nm, W 207.912 nm, Mo 203.846 nm, P 213.618 nm, and S 181.972 nm were selected as analytical lines. Linear relationships were found between the emission intensity and the mass concentrations of tungsten, molybdenum, boron, sulfur and phosphorus within definite ranges, and the detection limits (3s) were 15, 11, 6, 34, 23 μg·g-1, respectively. The method was used for the determination of tungsten, molybdenum, boron, sulfur and phosphorus in the national primary standard materials of tungsten molybdenum ore, giving the relative error between the measured values and the certified values in the range of -3.2%-2.0%, and RSDs (n=11) less than 3.0%. The method was applied to the simultaneous determination of tungsten, molybdenum, boron, sulfur and phosphorus in tungsten molybdenum ore samples, giving results consistent with those obtained by conventional methods.

       

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