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中国无机分析化学:2023,13(11):1209-1214
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电感耦合等离子体原子发射光谱(ICP-AES)法测定锂辉石中总铁含量
姚 洵1, 卢志琴2, 单经宇3
(1.张家港海关综合技术中心;2.张家港检验认证有限公司;3.张家港海关后勤管理中心)
Determination of Total Iron Content in Spodumene by Inductively Coupled Plasma-atomic Emission Spectrometry
Yao Xun1, Lu Zhiqin2, Shan Jingyu3
(1.Comprehensive Technology Center of Zhangjiagang Customs;2.Zhangjiagang Inspection and Certification Co., Ltd;3.Logistics Management Center of Zhangjiagang Customs)
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投稿时间:2023-02-01    修订日期:2023-10-14
中文摘要: 锂辉石作为最具有工业价值的锂矿物资源,常伴生有金属杂质。其中铁杂质的含量直接影响其生产工艺,为了解锂辉石中铁元素的含量水平,提升检测效率,建立了一种电感耦合等离子体光谱发射(ICP-AES)法测定锂辉石中总铁含量的测定方法。对样品前处理方式和加热工具进行了比对研究,对电感耦合等离子体光谱工作条件进行了优化,确定了波长为259.940nm为铁元素的分析谱线,发射功率为1300W,蠕动泵流速为1.5mL/min,载气流量为0.7 L/min,样品介质溶液为3%硝酸溶液。本方法全铁含量的检出限为0.004mg/L,相对标准偏差为1.4%,对锂辉石有证标准物质的检测结果在标准值允许的范围内。该方法检出限低、灵敏度高,准确性好,特别适合批量样品中总铁含量的测定。
Abstract:As the most valuable lithium mineral resource, spodumene is often associated with metal impurities. The content of iron impurities directly affects its production process. In order to measure the content of iron in spodumene and improve the detection efficiency, a method for the determination of total iron in spodumene by Inductively coupled plasma-atomic emission spectrometry has been established. The pretreatment methods and heating tools are compared. The working conditions of the Inductively coupled plasma spectrum has been optimized. The spectral line with a wavelength of 259.940 nm is selected as the analysis line for iron determination. The emission power is 1300 W, the flow rate of peristaltic pump is 1.5 ml/min, the flow rate of carrier gas is 0.7 L/min, and the sample medium solution is 3% nitric acid solution. The detection limit of this method is 0.004 mg/L, the relative standard deviation is 1.4% , and the detection result of spodumene certified reference material is within the allowable range of the standard value. The method has the advantages of low detection limit, high sensitivity and good accuracy, and is especially suitable for the determination of total iron in bulk samples.
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基金项目:南京海关科研项目(2023KJ31)
引用文本:
姚 洵,卢志琴,单经宇.电感耦合等离子体原子发射光谱(ICP-AES)法测定锂辉石中总铁含量[J].中国无机分析化学,2023,13(11):1209-1214.
Yao Xun,Lu Zhiqin,Shan Jingyu.Determination of Total Iron Content in Spodumene by Inductively Coupled Plasma-atomic Emission Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(11):1209-1214.

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