Determination of lead in lead ore by Na2EDTA titration combined with inductively coupled plasma atomic emission spectrometry
FAN Lixin1,2
1. MTC Testing Technical CO., LTD., Beijing 102628, China; 2. Beijing Key Laboratory for Evaluation and Testing of Metallic Mineral Resources, Beijing 102628, China
Abstract：The determination of lead content in lead ore is of great significance for the trade settlement. When the lead content in lead ore is determined by lead sulfate precipitation separation-Na2EDTA titration, chromium, barium, arsenic, antimony, tin and bismuth in the sample will interfere with the determination. The sample was dissolved with ammonium fluoride-hydrochloric acid-nitric acid-perchloric acid system. The interference of chromium was eliminated by adding hydrochloric acid repeatedly in perchloric acid system. The interference of arsenic, antimony and tin was eliminated by adding hydrobromic acid in perchloric acid system. Sulfuric acid was added in hydrochloric acid system to react with barium to form barium sulfate precipitate. At this time, lead could react with chloride ions to form complex ions, and would not form precipitate with sulfuric acid. After filtration, the filtrate and insoluble slag were obtained. On the one hand, sulfuric acid was added into the filtrate to react with lead to form lead sulfate precipitate followed by refiltration. The precipitate of lead sulfate was dissolved with acetic acid-ammonium acetate buffer solution (pH 5.5) and thioglycolic acid was added to eliminate the interference of bismuth, then the content of lead was determined by Na2EDTA titration. On the other hand, the insoluble slag was treated by sodium peroxide fusion, and the content of lead was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The contents of lead in the filtrate and the insoluble slag were summed, realizing the determination of lead in lead ore and overcoming the interference of chromium, barium, arsenic, antimony, tin and bismuth in sample. The contents of lead in lead ore samples were determined according to the proposed method. The relative standard deviations (RSD, n=11) of determination results were 0.20%-0.31%, and the recoveries were 99.5%-100.6%. The lead contents in certified reference material/standard sample of lead concentrate were determined according to the proposed method, and the results were basically consistent with the certified value/standard value.
范丽新. Na2EDTA滴定法结合电感耦合等离子体原子发射光谱法测定铅矿中铅[J]. 冶金分析, 2023, 43(12): 78-84.
FAN Lixin. Determination of lead in lead ore by Na2EDTA titration combined with inductively coupled plasma atomic emission spectrometry. , 2023, 43(12): 78-84.
[1] 范丽新, 陆青.EDTA滴定法测定粗锡中铅[J].冶金分析, 2017, 37(5):68-72. FAN Lixin, LU Qing.Determination of lead in crude tin by EDTA titration method[J].Metallurgical Analysis, 2017, 37(5):68-72. [2] 穆岩, 赵亚明, 柳华丽.EDTA滴定法测定含锑铋白烟灰中铅[J].黄金, 2021, 42(12):86-88. MU Yan, ZHAO Yaming, LIU Huali, et al.Determination of lead in white ash containing antimony and bismuth by EDTA titration method[J].Gold, 2021, 42(12):86-88. [3] 张园.Na2EDTA滴定法测定粗二氧化碲中铅含量[J].中国无机分析化学, 2021, 11(4):72-75. ZHANG Yuan.Determination of lead in crude tellurium dioxide by Na2EDTA titration method[J].Chinese Journal of Inorganic Analytical Chemistry, 2021, 11(4):72-75. [4] 张越, 芦新根, 洪博, 等.EDTA滴定法测定矿石中铅含量的方法改进[J].中国无机分析化学, 2020, 10(6):23-27. ZHANG Yue, LU Xingen, HONG Bo, et al.Improved method for determination of lead in ores by EDTA titration[J].Chinese Journal of Inorganic Analytical Chemistry, 2020, 10(6):23-27. [5] 郝璐, 范丽新.EDTA滴定法测定分银渣中的铅含量[J].中国无机分析化学, 2019, 9(3):33-36. HAO Lu, FAN Lixin.Determination of lead content in silver separating residue by EDTA titration method[J].Chinese Journal of Inorganic Analytical Chemistry, 2019, 9(3):33-36. [6] 李腾飞, 刘君侠, 李先和, 等.沉淀分离-EDTA返滴定法测定卡尔多炉渣中的铅量[J].中国无机分析化学, 2019, 9(1):54-57. LI Tengfei, LIU Junxia, LI Xianhe, et al.Determination of lead content in Kaldor slag by EDTA back titration with precipitation separation[J].Chinese Journal of Inorganic Analytical Chemistry, 2019, 9(1):54-57. [7] 范丽新, 陆青.EDTA返滴定法测定铅玻璃中铅[J].冶金分析, 2017, 37(2):65-69. FAN Lixin, LU Qing.Determination of lead content in lead glass by EDTA back titration method[J].Metallurgical Analysis, 2017, 37(2):65-69. [8] 李志伟.EDTA络合滴定法快速测定含钡铅矿石中的铅[J].岩矿测试, 2013, 32(6):920-923. LI Zhiwei.Rapid determination of lead in barium-bearing ores by EDTA compleximetry[J].Rock and Mineral Analysis, 2013, 32(6):920-923. [9] 中国国家标准化管理委员会.YS/T 1314.3—2019 铜冶炼分银渣化学分析方法 第3部分:铅含量的测定Na2EDTA滴定法[S].北京:冶金工业出版社, 2019.
