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中国无机分析化学:2022,12(3):102-119
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微波消解—电感耦合等离子体原子发射光谱法测定天然微晶石墨中铝铁钙镁钠钛钾
肖刘萍[], 周智勇-, 谢丽芳, 杨华东
(郴州市产商品质量监督检验所)
Determination of aluminum, iron, calcium, magnesium, sodium, titanium and potassium in natural amorphous graphite by microwave digestion and inductively coupled plasma atomic emission spectrometry
XIAO Liuping, ZHOU Zhiyong, XIE Li-fang, YANG Hua-dong
(ChenZhou Product and Commodity Quality Supervision and Inspection Institute)
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投稿时间:2022-01-25    修订日期:2022-02-07
中文摘要: 针对传统微波消解法存在的消解温度过高、样品消解不完全等问题,实验在常规微波消解温度下,从提高体系的氧化性入手,对消解方法进行改进。探讨了消解体系、消解温度、升温时间,并对消解机理进行了分析。结果表明,以2mL硝酸—5mL硫酸—1 mL高氯酸—1 mL氢氟酸为消解体系、升温时间为25 min、消解温度为200 ℃时,能实现样品的完全消解。消解后的溶液经赶酸处理,盐类析出,为了使盐类复溶,比较了硝酸、盐酸、王水的复溶效果,选定盐酸为复溶酸。对分析谱线进行了优化,确定的各成分分析谱线为铝308.2 nm、铁259.9{129} nm、钙317.933 nm、镁280.2 nm、钠589.5 nm、钛336.1 nm、钾766.4 nm。基于以上研究,建立了微波消解—电感耦合等离子体发射光谱法测定微晶石墨中铝铁钙镁钠钛钾的分析方法。结果表明,标准曲线的线性良好,相关系数不小于0.9994,方法检出限在0.00003%~0.0007%之间。用标准物质GBW03120验证了方法的正确度,结果满意。将方法应用于实际样品分析,测定结果的相对标准偏差(n=8)为0.72%~3.5%,加标回收率在98.2%~104.1%之间,均满足GB/T 27417—2017的要求。建立的方法能在常规微波消解温度下完全消解样品,适用于微晶石墨中主量金属元素的测定。
Abstract:Aiming at the problems of high digestion temperature and incomplete sample digestion in the traditional microwave digestion method, the method was improved by improving the oxidation of the system at the conventional microwave digestion temperature. The digestion system, heating time and digestion temperature were discussed. The results showed that the sample could be completely digested when 2ml nitric acid-5ml sulfuric acid-1ml perchloric acid-1ml hydrofluoric acid was used as digestion system, the heating time was 25 min and the digestion temperature was 200 ℃. Excess acid in the solution after digestion was removed by heating, and the salts were separated out. In order to redissolve salt, the redissolve effect of nitric acid, hydrochloric acid and aqua regia was discussed, and hydrochloric acid was selected as redissolve acid. The analytical spectral lines were optimized. The analytical spectral lines of each component were 308.2 nm for aluminum, 259.9{129} nm for iron, 317.933 nm for calcium, 280.2 nm for magnesium, 589.5 nm for sodium, 336.1 nm for titanium and 766.4 nm for potassium. Based on the above research, an analytical method was established for the determination of aluminum, iron, calcium, magnesium, sodium, titanium and potassium in amorphous graphite by microwave digestion and inductively coupled plasma emission spectrometry. The results showed that the linearity of the standard curve was good, and the correlation coefficient was not less than 0.9994. The detection limit of the method was 0.00003% ~ 0.0007%. The correctness of the method was verified by standard substance GBW03120 and results were satisfactory. The method was also applied to actual sample analysis. The relative standard deviations (RSD,n =8) of the determination results were in the range of 0.72% and 3.5%, and the recovery rates were between 98.2% and 104.1%%, which all met the requirements of GB/T 27417—2017. The established method could completely digest the sample at the conventional microwave digestion temperature, and was suitable for the determination of major metal elements in microcrystalline graphite.
文章编号:     中图分类号:O657.3;TF03    文献标志码:
基金项目:湖南省市场监管科技计划项目(2021KJJH86)
引用文本:
肖刘萍[],周智勇-,谢丽芳,杨华东.微波消解—电感耦合等离子体原子发射光谱法测定天然微晶石墨中铝铁钙镁钠钛钾[J].中国无机分析化学,2022,12(3):102-119.
XIAO Liuping,ZHOU Zhiyong,XIE Li-fang,YANG Hua-dong.Determination of aluminum, iron, calcium, magnesium, sodium, titanium and potassium in natural amorphous graphite by microwave digestion and inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(3):102-119.

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