钨精矿、焙烧钼精矿内控标样的研制和定值方法的研究

发布时间：2018-05-16 21:40

  本文选题：钨精矿 + 焙烧钼精矿　； 参考：《北京有色金属研究总院》2017年硕士论文

【摘要】：本文研究制备了一个黑钨精矿内控标样和一个焙烧钼精矿内控标样,并建立了使用微波辅助酸消解-电感耦合等离子体原子发射光谱法同时测定钨精矿样品中的七种共存元素的方法。本文对钨精矿、焙烧钼精矿的用途、前景以及主要分析方法进行了调研。钨矿、钼矿的主要分析方法有重量法、滴定法等经典化学分析方法,是矿物主量、常量元素分析的主要方法;电感耦合等离子体发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS),由于其具有可进行多元素同时分析、方法简便、灵敏度和准确度高等优点,逐渐成为矿物杂质分析的优选方法。本文研究建立了微波辅助酸消解-ICP-AES法同时测定钨精矿样品中锰、砷、铜、磷、钼、钡、硅等七种主要共存元素的新方法。研究表明:(1)采用盐酸、硝酸、氢氟酸(5+3+2)混酸作为微波消解酸,微波消解升温到160℃C后保持1Omin,可将样品完全溶解,溶液清亮,可用于直接测定,不需要分离钨基体。(2)仪器最优测试条件为射频功率1200W,雾化气流量0.75L/min,辅助气流量1.5L/min,冷却气流量15L/min,观察高度10mm,泵流量2.0L/min。(3)综合信噪比,谱线干扰等因素,选择的最佳分析线分别为 Mn(257.61 0nm),As(193.696nm),Cu(324.754nm),P(178.222nm),Mo(202.032nm),Ba(455.403nm),Si(250.690nm)。(4)本法的检出限为6×10-4μg/mL～7×10-2μg/mL,加标回收率在95.7%～110%之间,相对标准偏差为1%～7%。(5)用本法分析了美国国家标准与技术研究院(NIST)的黑钨精矿标样(SRM277)和白钨精矿标样(SRM2430),测定结果在标准值土扩展不确定度内。制备了黑钨精矿和焙烧钼精矿内控标样,具体步骤为:选取原料,成分设计、掺加、研磨、混匀、均匀性检验、稳定性检验、定值等。获得了粒度小于74μm,通过了均匀性检验的标准物质候选物料。
[Abstract]:In this paper, an internal standard sample of wolframite concentrate and an internal control standard sample of calcined molybdenum concentrate have been prepared. A method for simultaneous determination of seven coexisting elements in tungsten concentrate samples by microwave assisted acid digestion and inductively coupled plasma atomic emission spectrometry was established. In this paper, the application, prospect and main analytical methods of tungsten concentrate and roasted molybdenum concentrate are investigated. The main analytical methods of tungsten and molybdenum are gravimetric method, titration method and other classical chemical analysis methods. Inductively coupled plasma emission spectrometry (ICP-AESS) and inductively coupled plasma-mass spectrometry (ICP-MS) have become the best methods for mineral impurity analysis due to their advantages of multielement simultaneous analysis, simplicity, high sensitivity and accuracy. A new microwave assisted acid digestion ICP-AES method for simultaneous determination of manganese, arsenic, copper, phosphorus, molybdenum, barium and silicon in tungsten concentrate has been developed. The results showed that the mixture of hydrochloric acid, nitric acid and hydrofluoric acid was used as microwave digestion acid. The sample could be completely dissolved by microwave digestion at 160 鈩，

本文编号：1898517