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. |
相似文献（共19条）
| [1] |
杜米芳. 电感耦合等离子体发射光谱法同时测定玻璃中铝钙铁钾镁钠钛硫. 岩矿测试, 2008, 27(2): 146-148. |
| [2] |
罗磊, 付胜波, 肖洁, 魏灵巧, 戴伟峰, 丁晓晓. 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. 岩矿测试, 2014, 33(2): 203-207. |
| [3] |
谭雪英, 张小毅, 赵威. 电感耦合等离子体发射光谱法测定煤及煤灰样品中21个主次微量元素. 岩矿测试, 2008, 27(5): 379-382. |
| [4] |
王琰, 孙洛新, 张帆, 张华, 陈志慧. 电感耦合等离子体发射光谱法测定含刚玉的铝土矿中硅铝铁钛. 岩矿测试, 2013, 32(5): 719-723. |
| [5] |
胡德新, 武素茹, 刘跃勇, 王虹, 王向东, 李权斌, 谷松海. 改进BCR法-电感耦合等离子体发射光谱法测定矿产品堆场土壤中镉砷铅的化学形态. 岩矿测试, 2014, 33(3): 374-378. |
| [6] |
赵庆令, 李清彩. 电感耦合等离子体发射光谱法同时测定土壤样品中54种组分. 岩矿测试, 2011, 30(1): 75-78. |
| [7] |
于阗, 张连起, 陈小迪. 电感耦合等离子体发射光谱法和火焰原子吸收光谱法连续测定化探样品中12个元素. 岩矿测试, 2011, 30(1): 71-74. |
| [8] |
王龙山, 胡建平, 王光照, 郝辉. 偏硼酸锂熔矿-超声提取-电感耦合等离子体发射光谱法测定岩石水系沉积物土壤样品中硅铝铁等10种元素. 岩矿测试, 2008, 27(4): 287-290. |
| [9] |
盛献臻, 张汉萍, 李展强, 李海萍, 何光涛. 电感耦合等离子体发射光谱法同时测定地质样品中次量钨锡钼. 岩矿测试, 2010, 29(4): 383-386. |
| [10] |
秦晓丽, 田贵, 李朝长, 蒋智林. 电感耦合等离子体发射光谱法同时测定地质样品中的钍和氧化钾. 岩矿测试, 2019, 38(6): 741-746. doi: 10.15898/j.cnki.11-2131/td.201812290142 |
| [11] |
姚玉玲, 吴丽琨, 刘卫, 李刚. 乙醇增敏-电感耦合等离子体发射光谱法测定矿石及选冶样品中的铌钽. 岩矿测试, 2015, 34(2): 224-228. doi: 10.15898/j.cnki.11-2131/td.2015.02.012 |
| [12] |
沙艳梅, 赵学沛, 张歌, 焦万里, 张丹阳. 多向观测电感耦合等离子体发射光谱法同时测定土壤和水系沉积物中常量和微量元素. 岩矿测试, 2008, 27(4): 291-294. |
| [13] |
何海洋, 董学林, 于晓琪, 任小荣, 曾慧美. 内标校正-电感耦合等离子体发射光谱法测定磷矿石中的磷. 岩矿测试, 2017, 36(2): 117-123. doi: 10.15898/j.cnki.11-2131/td.2017.02.004 |
| [14] |
汪君, 王頔, 邓长生, 张建梅, 羊鸫, 王斌堂, 朱素霞. 电感耦合等离子体发射光谱法测定地球化学样品中的钍. 岩矿测试, 2014, 33(4): 501-505. |
| [15] |
汪静玲, 覃然, 唐艳霞, 黄玉龙, 袁爱萍. 电感耦合等离子体发射光谱法测定锑精矿中多种微量元素. 岩矿测试, 2008, 27(4): 316-318. |
| [16] |
贺攀红, 杨珍, 荣耀, 龚书浩, 龚治湘. 氢化物发生-电感耦合等离子体发射光谱法测定铀矿地质样品中痕量硒. 岩矿测试, 2016, 35(2): 139-144. doi: 10.15898/j.cnki.11-2131/td.2016.02.005 |
| [17] |
王学伟, 彭南兰, 唐琦平, 金婷婷. 四酸溶样电感耦合等离子体发射光谱法测定地质样品中的钪. 岩矿测试, 2014, 33(2): 212-217. |
| [18] |
王蕾, 温宏利, 马新荣, 张保科, 马生凤, 许俊玉, 巩爱华. 电感耦合等离子体发射光谱法测定硫化物矿中的高含量铅. 岩矿测试, 2011, 30(3): 305-309. |
| [19] |
刘昌岭, 林学辉. 单道扫描电感耦合等离子体发射光谱法测定珊瑚礁中主量和微量元素. 岩矿测试, 2003, (3): 225-227. |
计量
- PDF下载量(1182)
- 文章访问量(2298)
- HTML全文浏览量(65)
- 被引次数(0)