五酸和硝酸微波消解法结合ICP-OES技术测定多金属矿中多种元素的对比研究
| 1. | 河南省有色金属地质勘查总院, 河南 郑州 450052 |
| 2. | 河南省有色金属深部找矿勘查技术研究重点实验室, 河南 郑州 450052 |
Determination of Multi-elements in Polymetallic Ores by ICP-OES with Mixed Acids and Nitric Acid Microwave Digestion
| 1. | General Institute for Nonferrous Metals and Geological Exploration of Henan Province, Zhengzhou 450052, China |
| 2. | Key Laboratory of Deep Ore-prospecting Technology Research for Non-ferrous Metals of Henan Province, Zhengzhou 450052, China |
摘要：快速、准确测定多金属矿中的主次量元素需要根据多金属矿的具体类型选择不同的预处理方法。本文采集我国典型区域的铅锌、锡、钼、钒和铜镍等5种多金属矿, 对比了盐酸-硝酸-高氯酸-氢氟酸-硫酸五酸微波消解和硝酸微波消解的溶样效果, 应用电感耦合等离子体发射光谱法(ICP-OES)测定铜铅锌锡钨钼锰钛钒9种元素。通过国家标准物质分析验证, 五酸微波消解的溶样时间较长, 但一次可测定铜铅锌钼锰钒6种元素; 硝酸微波消解的溶样时间短, 但一次只能测定铜铅锌钼4种元素; 两种方法的准确度和精密度高(RSD < 5%), 检出限低(5.3~30 mg/kg), 均适合在地质行业推广应用。而由于锡钨钛3种元素不能完全被酸溶解, 上述两种消解方法均不适合。
Determination of Multi-elements in Polymetallic Ores by ICP-OES with Mixed Acids and Nitric Acid Microwave Digestion
ABSTRACT Different pretreatment methods should be used for quick and accurate determination of major and minor elements in different types of polymetallic ores. In this study, five types of polymetallic ores including Pb-Zn, Sn, Mo, V, and Cu-Ni polymetallic ores were collected from typical metallogenic areas of China. Comparison of microwave digestion using mixed acids of hydrochloric-nitric-perchloric-hydrofluoric-sulphuric acids with digestion using nitric acid only was performed. Nine elements, Cu, Pb, Zn, Sn, W, Mo, Mn, Ti, and V were determined by the Inductively Coupled Plasma-Optical Emission Spectrometry technique. Analytical results of National Standards Reference indicate that digestion with a mixture of five acids has a long digestion time and can simultaneously determine the 6 elements of Cu, Pb, Zn, Mo, Mn, and V. Digestion with nitric acid needs only 1 h and can determine 4 elements, Cu, Pb, Zn, and Mo. Two methods have good accuracy and precision (RSD < 5%) and low detection limits of 5.3-30 mg/kg, which are suitable for application in geological analyses. However, neither of these two methods are suitable for analyzing Sn, W, and Ti, because these elements cannot be digested completely by acids.
本文参考文献
| [1] |
蒯丽君, 樊兴涛, 詹秀春, 等. 酸消解-车载偏振能量色散X射线荧光法现场测定祁曼塔格多金属矿中高品位铜铅锌[J]. 岩矿测试, 2013, 32(4): 538-546. Kuai L J, Fan X T, Zhan X C, et al. On-site Analysis of Cu, Pb and Zn in Polymetallic Ores from Qimantage Area by Vehicle-loaded Polarized Energy Dispersive X-ray Fluorescence Spectrometer with Acid Digestion[J]. Rock and Mineral Analysis, 2013, 32(4): 538-546. |
| [2] |
岩石矿物分析编委会. 岩石矿物分析(第四版第三分册)[M] . 北京: 地质出版社, 2011: 185-325. The Editorial Committee of Rock and Mineral Analysis . Rock and Mineral Analysis (The Fourth Edition:Volume Ⅲ)[M] . Beijing: Geological Press, 2011: 185-325. |
| [3] |
王虹, 冯宇新, 苏明跃, 等. 火焰原子吸收光谱法测定红土镍矿中的铬[J]. 冶金分析, 2007, 27(9): 54-56. Wang H, Feng Y X, Su M Y, et al. Determination of Chromium in Laterite-Nickel Ore by Flame Atomic Absorption Spectrometry[J]. Metallurgical Analysis, 2007, 27(9): 54-56. |
| [4] |
高亮. 碱熔-电感耦合等离子发射光谱法测定红土镍矿中硅钙铝锰钛铬镍钴[J]. 冶金分析, 2013, 33(2): 51-54. Gao L. Determination of Silicon, Calcium, Magnesium, Aluminium, Manganese, Titanium, Chromium, Nickel and Cobalt in Laterite-Nickel Ore by Alkali Fusion-Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Metallurgical Analysis, 2013, 33(2): 51-54. |
| [5] |
汤淑芳, 符斌, 李华昌, 等. 矿物分析技术及进展[J]. 分析试验室, 2004, 23(3): 82-92. Tang S F, Fu B, Li H C, et al. Development of Mineral Analysis[J]. Chinese Journal of Analysis Laboratory, 2004, 23(3): 82-92. |
| [6] |
Al-Harahsheh M, Kingman S, Somerfield C, et al. Microwave-assisted Total Digestion of Sulphide Ores for Multi-element Analysis[J].Analytical Chemical Acta, 2009, 638: 101-105. doi: 10.1016/j.aca.2009.02.030 |
| [7] |
陈安明. 电感耦合等离子体发射光谱法测定低合金钢中的痕量硼[J]. 理化检验(化学分册), 2007, 43(8): 644-646. Chen A M. Determination of Boron in Low-alloy Steel by ICP-AES[J]. Physical Testing and Chemical Analysis Part B:Chemical Analysis, 2007, 43(8): 644-646. |
| [8] |
Thangavel S, Dash K, Dhavile S M, et al. Determination of Traces As, B, Bi, Ga, Ge, P, Pb, Sb, Se, Si and Te in High-purity Nickel Using Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES)[J].Talanta, 2015, 131: 505-509. doi: 10.1016/j.talanta.2014.08.026 |
| [9] |
黎香荣, 陈永欣, 刘顺琼, 等. 电感耦合等离子体发射光谱法测定多金属矿中的主次量元素[J]. 冶金分析, 2012, 32(8): 38-41. Li X R, Chen Y X, Liu S Q, et al. Determination of Major and Minor Elements in Polymetallic Ore by Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Metallurgical Analysis, 2012, 32(8): 38-41. |
| [10] |
张翼明, 张立锋, 周凯红, 等. 电感耦合等离子体质谱法测定硫化矿中金[J]. 冶金分析, 2014, 34(12): 44-47. Zhang Y M, Zhang L F, Zhou K H, et al. Determination of Gold in Sulphide Ore by Inductively Coupled Plasma Mass Spectrometry[J]. Metallurgical Analysis, 2014, 34(12): 44-47. |
| [11] |
金献忠, 陈建国, 梁帆, 等. 碱熔融-ICP-AES法对锰矿石中主量、次量与痕量元素的同时测定[J]. 分析测试学报, 2009, 28(2): 150-156. Jin X Z, Chen J G, Liang F, et al. Determination of Major, Minor and Trace Elements in Manganese Ores by Alkali Fusion-ICP-AES[J]. Journal of Instrumental Analysis, 2009, 28(2): 150-156. |
| [12] |
胡德新, 肖葵, 王向东, 等. 微波消解-电感耦合等离子体发射光谱法测定高碳铬铁中硅锰磷[J]. 岩矿测试, 2014, 33(2): 208-211. Hu D X, Xiao K, Wang X D, et al. Determination of Silicon Manganese and Phosphorus in High Carbon-Chrome Iron by Inductively Coupled Plasma-Atomic Emission Spectrometry after Microwave Digestion[J]. Rock and Mineral Analysis, 2014, 33(2): 208-211. |
引证文献（本文共被引用8次）
| [1] |
过氧化钠碱熔-电感耦合等离子体发射光谱法测定多金属矿中的锡钨钛等主次量成分[J]. 王小强,夏辉,秦九红,王书勤,杨惠玲,宋志敏,杜天军. 岩矿测试.2017(01) |
| [2] |
不同微波消解剂对沉积物重金属检测的影响[J]. 施柳,何瑶,李飞鹏,陈玲,毛凌晨. 净水技术. 2016(06) |
| [3] |
ICP-OES测定区域地球化学样品多元素的研究[J]. 李娜,刘玖芬,赵正鹏,刘淑亮,柳晓丹. 黄金. 2016(09) |
| [4] |
四种酸体系对微波酸溶-电感耦合等离子体质谱法测定固体废物中16种金属元素含量的影响[J]. 宣肇菲,徐少才,房贤文,谭丕功. 岩矿测试. 2015(06) |
| [5] |
微波溶样在分析化学样品前处理中的应用[J]. 黎乔. 科技创新与应用. 2017(05) |
| [6] |
稻米重要矿质元素快速测定技术的创建与应用[D]. 张世玺.浙江大学 2016 |
| [7] |
一次溶样原子吸收光谱法检测地质样品银、铜、铅、锌的方法研究[J]. 迟朦,张雷,王振德,郭新元,黄娇. 当代化工. 2016(05) |
| [8] |
基于火焰原子吸收法实现多金属矿中铅锌铜的测定[J]. 张卫卫. 世界有色金属. 2016(23) |
相似文献（共18条）
| [1] |
李刚, 苏文峰. 焙烧分离-氢化物发生-原子荧光光谱法测定土壤样品中微量硒. 岩矿测试, 2008, 27(2): 120-122. |
| [2] |
王小强, 夏辉, 秦九红, 王书勤, 杨惠玲, 宋志敏, 杜天军. 过氧化钠碱熔-电感耦合等离子体发射光谱法测定多金属矿中的锡钨钛等主次量成分. 岩矿测试, 2017, 36(1): 52-58. doi: 10.15898/j.cnki.11-2131/td.2017.01.008 |
| [3] |
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. |
| [4] |
门倩妮, 沈平, 甘黎明, 冯博鑫. 敞开酸溶和偏硼酸锂碱熔ICP-MS法测定多金属矿中的稀土元素及铌钽锆铪. 岩矿测试, 2020, 39(1): 59-67. doi: 10.15898/j.cnki.11-2131/td.201905100060 |
| [5] |
马亮帮, 葛颖. 微波消解-电感耦合等离子体发射光谱法测定固体沥青中微量金属元素. 岩矿测试, 2013, 32(3): 441-444. |
| [6] |
王祝, 李明礼, 邵蓓, 卓玛曲西, 姜贞贞, 刘高令, 多吉. 电感耦合等离子体发射光谱法测定西藏日多温泉地热水中11种主次量元素. 岩矿测试, 2015, 34(3): 302-307. doi: 10.15898/j.cnki.11-2131/td.2015.03.007 |
| [7] |
孟时贤, 邓飞跃, 杨远, 苏卫汉, 闵晓芳, 雍伏曾. 电感耦合等离子体发射光谱法测定铅锌矿中15个主次量元素. 岩矿测试, 2015, 34(1): 48-54. doi: 10.15898/j.cnki.11-2131/td.2015.01.006 |
| [8] |
胡兰, 刘跃友, 黄安拉. 碱性模式氢化物发生-原子荧光光谱法测定多金属矿中的微量铋. 岩矿测试, 2010, 29(1): 87-88. |
| [9] |
杨惠玲, 夏辉, 杜天军, 白露, 秦九红, 铁锦林. 电感耦合等离子体发射光谱法同时测定锡矿石中锡钨钼铜铅锌. 岩矿测试, 2013, 32(6): 887-892. |
| [10] |
岑治宝, 任红灿, 王树喜, 杜米芳. 微波消解-电感耦合等离子体发射光谱法同时测定白云石中铁铝钙镁钾钠硫. 岩矿测试, 2006, 25(3): 276-278. |
| [11] |
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. |
| [12] |
刘磊, 杨艳, 彭秀峰, 曹宏杰, 李海明. 微波消解-电感耦合等离子体发射光谱法测定岩石和矿物中的钼. 岩矿测试, 2011, 30(3): 318-320. |
| [13] |
陈广志, 苏明跃, 王昊云. 微波消解-电感耦合等离子体发射光谱法测定煤中磷. 岩矿测试, 2011, 30(4): 477-480. |
| [14] |
黄靖, 王英滨, 周冠轩, 马真乾. 微波消解-电感耦合等离子体发射光谱法测定粉煤灰中的镓. 岩矿测试, 2020, 39(1): 92-98. doi: 10.15898/j.cnki.11-2131/td.201905190065 |
| [15] |
李志伟, 赵晓亮, 李珍, 王烨, 王君玉. 敞口酸熔-电感耦合等离子体发射光谱法测定稀有多金属矿选矿样品中的铌钽和伴生元素. 岩矿测试, 2017, 36(6): 594-600. doi: 10.15898/j.cnki.11-2131/td.201701030001 |
| [16] |
杨惠玲, 班俊生, 夏辉, 王书勤, 杜天军, 王小强. 微波消解电感耦合等离子发射光谱法测定三水铝土矿中的有效铝、活性铝和活性硅. 岩矿测试, 2017, 36(3): 246-251. doi: 10.15898/j.cnki.11-2131/td.201606120083 |
| [17] |
张杰芳, 闫玉乐, 夏承莉, 焦发存, 张海侠. 微波碱消解-电感耦合等离子体发射光谱法测定煤灰中的六价铬. 岩矿测试, 2017, 36(1): 46-51. doi: 10.15898/j.cnki.11-2131/td.2017.01.007 |
| [18] |
胡德新, 肖葵, 王向东, 王振坤, 刘敏, 李权斌. 微波消解-电感耦合等离子体发射光谱法测定高碳铬铁中硅锰磷. 岩矿测试, 2014, 33(2): 208-211. |
计量
- PDF下载量(1431)
- 文章访问量(2303)
- HTML全文浏览量(56)
- 被引次数(8)