| 液氮冷凝吸收热解-电感耦合等离子体质谱法测定岩石土壤沉积物中的溴碘 |
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| 引用本文： | 宋萍,温宏利.液氮冷凝吸收热解-电感耦合等离子体质谱法测定岩石土壤沉积物中的溴碘[J].岩矿测试,2016,35(4):384-388. |
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| 作者姓名： | 宋萍 温宏利 |
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| 作者单位： | 国家海洋局第一海洋研究所, 山东 青岛 266061,国家海洋局第一海洋研究所, 山东 青岛 266061,国家海洋局第一海洋研究所, 山东 青岛 266061,国家海洋局第一海洋研究所, 山东 青岛 266061,国家海洋局第一海洋研究所, 山东 青岛 266061 |
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| 基金项目： | 中央级公益性科研院所基本科研业务费专项资金（2013G11, 2011T10）；青岛市创新人才资金（13-CX-20）；山东省泰山学者海外特聘人才项目 |
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| 摘 要： | 分析地质样品中的溴碘,目前常用的提取方法有半熔法、稀氨水密封溶样法和热解法,但由于元素含量低、易损失,样品分解和溴碘的提取过程是主要的误差来源。本文改进了传统热解法的吸收装置,用液氮冷凝吸收代替常规的碱溶液吸收,提取地质样品中的溴碘,用电感耦合等离子体质谱法测定其含量。以标准偏差的10倍计算,稀释倍数为50,溴碘的检出限分别为0.06μg/g、0.01μg/g,低于传统热解法和半熔法,略高于稀氨水密封溶样法;精密度(RSD)为6.4%~21.0%。本方法相对于传统的碱溶液吸收热解法,减少了碱试剂的引入,降低了基体空白和稀释倍数,提高了精密度,操作较半熔法简便,可作为稀氨水密封溶样法的一种补充方法。因此,对于土壤和水系沉积物,宜采用稀氨水密封溶样法;对于岩石以及采用稀氨水密封溶样法难以完全提取的样品,可采用本方法。
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| 关 键 词： | 海洋沉积物 有机碳 自动电位滴定仪 滴定终点判定 氧化还原电位 |
| 收稿时间： | 2/8/2015 12:00:00 AM |
| 修稿时间： | 5/5/2016 12:00:00 AM |
Determination of Bromine and Iodine in Rock, Soil, and Sediments by Inductively Coupled Plasma-Mass Spectrometry Using Pyrohydrolysis with Liquid Nitrogen Trap |
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| SONG Ping and WEN Hong-li.Determination of Bromine and Iodine in Rock, Soil, and Sediments by Inductively Coupled Plasma-Mass Spectrometry Using Pyrohydrolysis with Liquid Nitrogen Trap[J].Rock and Mineral Analysis,2016,35(4):384-388. |
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| Authors: | SONG Ping and WEN Hong-li |
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| Institution: | The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China,The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China,The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China,The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China and The First Institute of Oceanography, State Oceanic Administration, Qingdao 266061, China |
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| Abstract: | The automatic potentiometric titrator has the advantages of being simple to operate and giving fast measurement results, which could reduce artifical influence due to manual operation. In this study, organic carbon content of marine sediments was determined by Automatic Potentiometric Titrator. In order to investigate if the Automatic Potentiometric Titrator could accurately determine the titration end-point, this method was compared with the national standard method (GB 17378.5-2007) in which the titration end-point was visually determined through color change. Results show that the detection limits of the automatic potentiometric titrator and manual methods were 0.029% and 0.086%, respectively. There are no significant differences between the two methods in titration end-point determination. However, the Automatic Potentiometric Titrator has better accuracy and precision than manual operation. Therefore, under certain circumstances, Automatic Potentiometric Titrator can take over the visual method to determine the titration end-point. It is also noteworthy that there are some problems in measuring real samples. For example, the Automatic Potentiometric Titrator might be unable to accurately determine the target titration end-point when there are complex electrical potential changes due to redox reactions and chelating interactions in the reaction system. On this occasion, the titration end-point can be determined visually. |
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| Keywords: | marine sediment organic carbon automatic potentiometric titrator determination of the titration end-point redox potential |
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