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过氧化钠碱熔-电感耦合等离子体质谱法测定原生矿石中的锡

Determination of Tin in Primary Ores by Inductively Coupled Plasma-Mass Spectrometry with Sodium Peroxide Alkali Fusion

  • 摘要: 原生锡矿石主要存在的矿床类型有矽卡岩型锡矿、斑岩型锡矿、锡石硅酸盐脉型锡矿、锡石硫化物脉型锡矿、石英脉及云英岩型锡矿。锡矿石一般不溶于盐酸、硝酸及王水体系,采用硫酸、氢氟酸处理时无法全部溶解。苯芴铜分光光度法和碘量法等传统测试方法存在受样品中伴生元素干扰大、稳定性差、检出限高、分析效率低等不足。本文建立了电感耦合等离子体质谱法测定原生矿石中锡元素含量的分析方法,用过氧化钠对样品进行熔融分解处理,热水浸取后用酒石酸-盐酸酸化,采用铑作为内标进行仪器信号漂移校正,同时用高倍稀释的方式来克服基体干扰。方法检出限为0.1μg/g,精密度小于5%,最低检出浓度为0.4μg/g,测试范围为12.5~12700μg/g。本方法操作简便,分析速度和数据质量都优于传统分析方法。

     

    Abstract:
    BACKGROUNDThe main types of primary tin ore occur in skarn, porphyry, cassiterite silicate vein, cassiterite sulfide vein, quartz vein and greisen tin deposits. Tin ores are generally insoluble in hydrochloric acid, nitric acid and aqua regia, and tin ores cannot be dissolved completely when treated with sulfuric acid or hydrofluoric acid. Traditional measurement methods such as phenylfluorone-cetyltrimethyl ammonium bromide spectrophotometry and iodometry have disadvantages, such as the serious interference of the associated elements in the sample, poor stability, high detection limit and low analysis efficiency.
    OBJECTIVESTo establish a method for the determination of tin in primary ore by Inductively Coupled Plasma-Mass Spectrometry.
    METHODSThe sample was melted and decomposed by sodium oxide, and leached by hot water, followed by tartaric acid and hydrochloric acid acidification. 103Rh was used as the internal standard element to correct instrument signal drift, and the matrix effect was overcome by high-dilution factors.
    RESULTSThe detection limit of the method was 0.1μg/g for tin, the precision was less than 5%, the minimum detection concentration was 0.4μg/g, and the measurement range was 12.5-12700μg/g.
    CONCLUSIONSThe method has simple pretreatment and operation. The analysis efficiency and data quality are an improvement over traditional methods.

     

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