双毛细管在线干扰校正-电感耦合等离子体发射光谱法测定含铀地质样品中微量铅
河南省核工业放射性核素检测中心, 河南 郑州 450002 |
Determination of Trace Lead in Uranium-bearing Geological Samples by Inductively Coupled Plasma-Optical Emission Spectrometry with Double Capillary On-line Interference Correction
Henan Radionuclide Detection Center of Nuclear Industry, Zhengzhou 450002, China |
摘要：应用电感耦合等离子体发射光谱法测定地质样品中的铅时, 基体元素的干扰会使测量结果偏低。本文用氢氟酸、硝酸、高氯酸、盐酸溶解样品, 采用等径双毛细管在线干扰校正的方法测定了含铀地质样品中的微量铅。首先通过双毛细管确定了样品溶液中的Fe、Al对铅有负干扰, 而一定浓度的U、Ba、Ti、Ca、Mn、K、Mg、Na等基体元素没有干扰或可以忽略, 由此在线双毛细管根据样品中Fe、Al的含量使用不同的校正试液建立标准曲线, 测定未知样品时同步进行稀释, 降低了Fe、Al的基体效应。方法检出限为1.5 μg/g, 精密度(RSD)小于5%。与普通干扰校正法相比, 双毛细管在线干扰校正法可根据不同基体的样品使用不同的干扰校正试液, 快速建立标准曲线进行复杂样品的测定, 且避免了二次稀释, 节省试剂, 适合测定基体成分接近的批量样品。
Determination of Trace Lead in Uranium-bearing Geological Samples by Inductively Coupled Plasma-Optical Emission Spectrometry with Double Capillary On-line Interference Correction
ABSTRACT Measured lead contents in geological samples were commonly lower than real values because of matrix elements interference during Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) analyses. In this study, U-bearing geological samples were dissolved by hydrofluoric acid, nitric acid, perchloric acid, and hydrochloric acid. Trace lead was determined by ICP-OES with double capillary on-line interference correction. The interferences of matrix elements on lead were studied using double capillary. Iron and Al had negative interferences on lead, whereas a specific concentration of U, Ba, Ti, Ca, Mn, Mg, K and Na almost had no interferences on lead. The standard curve was established using double capillary according to the contents of Fe and Al in different test solution. The unknown sample was diluted simultaneously, which reduced the matrix effects of Fe and Al. The detection limit was 1.5 μg/g, and the RSD was less than 5%. Compared with the common interference correction method, the double capillary on-line interference correction method can establish a standard curve quickly using different interference correction test solutions according to different matrices. Moreover, sample solution does not need to be secondly diluted, saving the reagent. This method is suitable for rapid determination of batch samples with similar matrices.
本文参考文献
| [1] |
胡德新, 王昊云, 王兆瑞, 等. 微波消解样品-电感耦合等离子体原子发射光谱法测定铅精矿中铅、砷、镉、汞[J]. 理化检验(化学分册), 2012, 48(7): 828-830. Hu D X, Wang H Y, Wang Z R, et al. ICP-AES Determination of Lead, Arsenic, Cadmium and Mercury in Lead Concentrates with Microwave Assisted Sample Digestion[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2012, 48(7): 828-830. |
| [2] |
闵国华, 张庆建, 刘稚, 等. 电感耦合等离子体原子发射光谱法测定铅矿、锌矿和铅锌矿中杂质元素[J]. 冶金分析, 2014, 34(5): 51-55. Min G H, Zhang Q J, Liu Z, et al. Determination of Impurity Elements in Lead Ore, Zinc Ore and Lead-Zinc Ore by Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Metallurgical Analysis, 2014, 34(5): 51-55. |
| [3] |
孙晓慧, 李章, 刘希良, 等. 微波消解-电感耦合等离子体原子发射光谱法测定土壤和水系沉积物中15种组分[J]. 冶金分析, 2014, 34(11): 56-60. Sun X H, Li Z, Liu X L, et al. Determination of Fifteen Components in Soil and Stream Sediment by Inductively Coupled Plasma Atomic Emission Spectrometry after Microwave Digestion[J]. Metallurgical Analysis, 2014, 34(11): 56-60. |
| [4] |
赵刚, 谢璐, 龙军桥, 等. ICP-AES/AFS联合测定金矿地质样品中32种主次痕量元素[J]. 黄金, 2015, 36(1): 70-74. doi: 10.11792/hj201501019 Zhao G, Xie L, Long J Q, et al. Combined ICP-AES/AFS Method in Determining 32 Major and Minor Elements in Gold Geological Samples[J].Gold, 2015, 36(1): 70-74. doi: 10.11792/hj201501019 |
| [5] |
罗磊, 付胜波, 肖洁, 等. 电感耦合等离子体发射光谱法测定含重晶石的银铅矿中的铅[J]. 岩矿测试, 2014, 33(2): 203-207. Luo L, Fu S B, Xiao J, et al. Determination of Lead in Argentalium Ores Containing Barite by Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2014, 33(2): 203-207. |
| [6] |
陈永欣, 吕泽娥, 刘顺琼, 等. 电感耦合等离子体发射光谱法测定铜精矿中银砷铅锌[J]. 岩矿测试, 2007, 26(6): 497-499. Chen Y X, Lü Z E, Liu S Q, et al. Inductively Coupled Plasma-Atomic Emission Spectrometric Determination of Silver, Arsenic, Lead and Zinc in Copper Concentrates[J]. Rock and Mineral Analysis, 2007, 26(6): 497-499. |
| [7] |
莫桂花, 王志畅, 龚治湘, 等. 在线双毛细管火焰原子吸收法测定矿石中高含量铅[J]. 化学工程师, 2007, (5): 26. Mo G H, Wang Z C, Gong Z X, et al. Determination of High Contents of Pb in Ores by AAS with On-line Bi-capillary[J]. Chemical Engineer, 2007, (5): 26. |
| [8] |
王娟, 贺攀红, 杨珍, 等. 在线双毛细管火焰原子吸收法测定海带中的微量锶[J]. 食品科学, 2014, 35(10): 192-194. doi: 10.7506/spkx1002-6630-201410036 Wang J, He P H, Yang Z, et al. Determination of Trace Strontium in Kelp by Flame Atomic Absorption Spectrometry with On-line Binary Capillary[J].Food Science, 2014, 35(10): 192-194. doi: 10.7506/spkx1002-6630-201410036 |
| [9] |
辛仁轩. 等离子体发射光谱分析[M] . 北京: 化学工业出版社, 2005: 160-168. Xin R X. Plasma Emission Spectrum Analysis[M] . Beijing: Chemical Industry Press, 2005: 160-168. |
| [10] |
赵君威, 梅坛, 鄢国强, 等. 电感耦合等离子体原子发射光谱分析中的光谱干扰及其校正的研究进展[J]. 理化检验(化学分册), 2013, 49(3): 364-369. Zhao J W, Mei T, Yan G Q, et al. Recent Progress of Researches on Spectral Interference and Its Correction in ICP-AES Analysis[J]. Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2013, 49(3): 364-369. |
| [11] |
陈永欣, 黎香荣, 吕泽娥, 等. 电感耦合等离子体原子发射光谱法测定锰矿石中铝铜锌铅砷镉[J]. 冶金分析, 2009, 29(4): 46-49. Chen Y X, Li X R, Lü Z E, et al. Determination of Aluminium, Copper, Zinc, Lead, Arsenic and Cadmium in Manganese Ores by Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Metallurgical Analysis, 2009, 29(4): 46-49. |
| [12] |
邓全道, 许光, 林冠春, 等. 微波消解-耐氢氟酸系统进样电感耦合等离子体发射光谱法测定锰矿中铝磷镁铁锌镍[J]. 冶金分析, 2011, 31(1): 35-39. Deng Q D, Xu G, Lin G C, et al. Determination of Aluminum, Phosphorus, Magnesium, Iron, Zinc and Nickel in Manganese Ore by Inductively Coupled Plasma Atomic Emission Spectrometry with Hydrofluoric Acid Resistant Sampling System after Microwave Digestion[J]. Metallurgical Analysis, 2011, 31(1): 35-39. |
| [13] |
徐进力, 邢夏, 张勤, 等. 电感耦合等离子体发射光谱法直接测定铜矿石中银铜铅锌[J]. 岩矿测试, 2010, 29(4): 377-382. Xu J L, Xing X, Zhang Q, et al. Direct Determination of Silver, Copper, Lead and Zinc in Copper Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry[J]. Rock and Mineral Analysis, 2010, 29(4): 377-382. |
| [14] |
张微, 张丽微, 艾婧娇, 等. ICP-ES法同时测定地质样品中Cu-Pb-Zn-Sc-Mo[J]. 矿物学报, 2013, 33(4): 521-524. Zhang W, Zhang L W, Ai J J, et al. Simultaneous Determination of Cu-Pb-Zn-Sc-Mo in the Geological Samples with Inductively Coupled Plasma Optical Emission Spectrometer[J].Acta Mieralogica Sinica, 2013, 33(4): 521-524. |
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