| 密闭溶样-电感耦合等离子体质谱法测定煅烧高岭土中微量重金属元素 |
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| 引用本文： | 邵坤,何启生,陈开旭,邵鑫,程先忠.密闭溶样-电感耦合等离子体质谱法测定煅烧高岭土中微量重金属元素[J].岩矿测试,2010,29(1):43-46. |
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| 作者姓名： | 邵坤 何启生 陈开旭 邵鑫 程先忠 |
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| 作者单位： | 1. 武汉工业学院化学与环境工程学院,湖北,武汉,430023
2. 国土资源部宜昌地质矿产研究所,湖北,宜昌,443003 |
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| 基金项目： | 湖北省科技厅自然科学基金重点项目资助，科技部科研院所技术开发研究项目资助 |
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| 摘 要： | 建立了密闭溶样-电感耦合等离子体质谱法同时测定煅烧高岭土中铜、铅、锌、铬、镉和锰等6个微量重金属元素的有效方法。实验中对仪器的最佳工作参数进行了优化,选择适当的同位素,并用铑作内标元素,有效地抑制了分析信号的漂移以及分子和多原子离子的质谱干扰;探讨了混合酸消解体系、消解液用量、密闭溶样的时间对测定结果的影响。以硝酸-氢氟酸作为消化试剂,在180℃下溶解4 h能完全消解样品。在选定的实验条件下,对煅烧高岭土样品进行了精密度和回收率试验,方法相对标准偏差(RSD,n=9)为0.96%~2.22%,加标回收率为98.0%~101.5%。
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| 关 键 词： | 电感耦合等离子体质谱法 煅烧高岭土 微量重金属元素 密闭溶样 |
| 收稿时间： | 6/6/2009 12:00:00 AM |
| 修稿时间： | 2009/9/15 0:00:00 |
Determination of Trace Heavy Metal Elements in Caclined Kaoline by Inductively Coupled Plasma-Mass Spectrometry with Pressurized Acid Digestion |
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| SHAO Kun,HE Qi sheng,CHEN Kai xu,SHAO Xin and CHENG Xian zhong.Determination of Trace Heavy Metal Elements in Caclined Kaoline by Inductively Coupled Plasma-Mass Spectrometry with Pressurized Acid Digestion[J].Rock and Mineral Analysis,2010,29(1):43-46. |
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| Authors: | SHAO Kun HE Qi sheng CHEN Kai xu SHAO Xin and CHENG Xian zhong |
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| Institution: | School of Chemistry and Environmental Engineering, Wuhan Polytechnic University;Yichang Institute of Geology and Mineral Resource,The Ministry of Land and Resources;Yichang Institute of Geology and Mineral Resource,The Ministry of Land and Resources;Yichang Institute of Geology and Mineral Resource,The Ministry of Land and Resources;School of Chemistry and Environmental Engineering, Wuhan Polytechnic University |
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| Abstract: | A method for the determination of copper, lead, zinc, chromium, cadmium and manganese in calcined kaoline samples by inductively coupled plasma-mass spectrometry (ICP-MS) with pressurized acid digestion was developed. The ICP-MS instrument operating parameters were optimized. The mass spectral interferences were eliminated by selecting ~(65)Cu, ~(208)Pb, ~(66)Zn, ~(52)Cr, ~(114)Cd and ~(55)Mn as analytical isotopes. And Rh was selected as internal standard to compensate the analytical signal drift. The factors affecting the analytical results such as selection of sample digestion system, dosage of the digestion solvents and digestion time were studied. Under the optimized condition with HNO_3-HF digestion system at 180℃ for 4 h, the recovery for these elements was 98.0%～101.5% with precision of 0.96%～2.22%RSD(n=9). The proposed method has been applied to the determination of these trace heavy metal elements in calcined kaoline samples with satisfactory results. |
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| Keywords: | inductively coupled plasma-mass spectrometry(ICP-MS) calcined kaoline trace heavy metal element pressure acid digestion |
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