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| 海水中三价与六价铬高效液相色谱-三重四级杆电感耦合等离子体质谱法(HPLC-TQ-ICP-MS)的联用测定 |
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孙玲玲1,2, 宋金明1,3,4,2, 李宁1,3,4,2, 孙萱1,2, 刘瑶1,2, 于颖1,2
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1.中国科学院海洋研究所所级公共技术服务中心 山东青岛 266071;2.中国科学院海洋大科学中心 山东青岛 266071;3.中国科学院海洋研究所 海洋生态与环境科学重点实验室 山东青岛 266071;4.青岛海洋科学与技术试点国家实验室 海洋生态与环境科学功能实验室 山东青岛 266237
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| 摘要: |
| 基于高效液相色谱（HPLC）与三重四级杆电感耦合等离子体质谱（TQ-ICP-MS）联用技术，构建海水中三价铬与六价铬在线分离与测定的检测方法。采用TQ-ICP-MS碰撞反应池（KED）技术消除35Cl16O1H+、40Ar12C对52Cr同位素测定可能存在的质谱干扰。选用Dionex IonPac AG 7（4 mm×50 mm，10 μm）阴离子交换柱为分析柱，对流动相浓度及pH值进行优化，结果表明，当流动相浓度为0.08 mol/L NH4NO3、0.6 mmol/L EDTA，pH值7.5，流速1.0 mL/min时，仅需80 s就可以完成三价铬和六价铬的理想分离与测定。对络合剂EDTA的络合浓度、pH、温度及时间进行了深入研究，结果显示，当EDTA浓度为10 mmol/L、络合pH值7.5、络合温度50℃、络合时间2 h时，三价铬可以最大程度的被EDTA络合。在0.1~50.0 μg/L标准浓度范围内，三价铬和六价铬浓度与信号强度的线性相关系数大于0.999 9，检出限分别为0.010和0.015 μg/L，方法的回收率90.4%~107.9%，相对标准偏差RSD为1.66%~3.71%（n=6）。该方法灵敏度高，分离度高，分析时间短，准确性和精密度好，可作为海水及其他高盐样品中铬形态分析的理想方法，并可为海水环境质量评价提供科学依据。 |
| 关键词: 铬 形态分析 海水 高效液相色谱-电感耦合等离子体质谱法 |
| DOI：10.11693/hyhz20220600150 |
| 分类号:O657.31 |
| 基金项目:中科院仪器设备功能开发技术创新项目，E1KY07101L号，E2KY11101L号；“烟台双百”人才项目。 |
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| JOINT DETERMINATION OF TRIVALENT CHROMIUM AND HEXAVALENT CHROMIUM IN SEAWATER BY HPLC-TQ-ICP-MS |
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SUN Ling-Ling1,2, SONG Jin-Ming1,3,4,2, LI Ning1,3,4,2, SUN Xuan1,2, LIU Yao1,2, YU Ying1,2
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1.Public Tech-Supporting Center, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China;2.Center for Ocean Mega-Science, Chinese Academy of Sciences, Qingdao 266071, China;3.CAS Key Laboratory of Marine Ecology and Environmental Sciences, Institute of Oceanology, Chinese Academy of Sciences, Qingdao 266071, China;4.Functional Laboratory for Marine Ecology and Environmental Science, Pilot National Laboratory for Marine Science and Technology (Qingdao), Qingdao 266237, China
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| Abstract: |
| A method for the separation and determination of Cr(III) and Cr(VI) in seawater was established by high-performance liquid chromatography-triple quadrupole inductively coupled plasma mass spectrometry (HPLC-TQ-ICP-MS). The technology of kinetic energy discrimination (KED) in collision/reaction cell ICP-MS was used to effectively eliminate the mass spectrum interference of 35Cl16O1H+ and 40Ar12C on the determination of 52Cr. The Dionex IonPac AG7 (4 mm×50 mm, 10 μm) anion exchange column was selected as the analysis column to optimize the mobile phase concentration and pH value. Results show that under the conditions of the mobile phase concentration at 0.08 mol/L NH4NO3, 0.6 mmol/L EDTA, pH 7.5, and the flow rate at 1.0 mL/min, the ideal separation and determination of Cr(III) and Cr(VI) could be completed in 80 s. In addition, the complexing concentration, pH, temperature, and time of EDTA were also studied. In addition, under the conditions of the concentration of EDTA at 10 mmol/L, pH at 7.5, complexing temperature at 50℃, and complexing time in 2 h, Cr(III) could be fully complexed by EDTA. In the standard concentration range of 0.1~50.0 μg/L, the linear correlation coefficients of Cr(III) and Cr(VI) were greater than 0.999 9, and the detection limits were 0.010 and 0.015 μg/L, respectively. The recovery rate of the method was in the range of 90.4%~107.9%, and the relative standard deviations were between 1.66% and 3.71% (n=6). The method showed high sensitivity, selectivity, in high accuracy and precision, suitable for the determination of chromium speciation in seawater and other high salt samples, and provided a scientific basis for the quality evaluation of seawater. |
| Key words: chromium morphological analysis seawater high performance liquid chromatography-inductively coupled plasma mass spectrometry |