逆王水微波消解–电感耦合等离子体质谱法测定地球化学样品中的碘和溴
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摘要
地球化学样品经微波辅助逆王水消解后,在氨性介质中采用电感耦合等离子体质谱法快速测定碘和溴的含量。取样量为0.1 g,逆王水的用量为1.6 mL,对样品进行程序化微波消解,通过在线加入内标校正基体效应和信号漂移对测定所造成的影响。碘、溴的检出限分别0.15,0.21μg/g,测定结果的相对标准偏差不大于5.0%(n=7),国家标准样品测定值与标示值相符。该方法在样品消解后加入定量氨水可直接分析,减小了碘测定的记忆效应,提高了分析速度,可应用于地球化学样品中碘和溴含量的测定。
A method was estiblished for quick determination of iodine and bromine in geochemical sample by using microwave digestion–ICP–MS after digested with invers aqua regia. With the dosage of 0.1 g and 1.6 mL inverse aqua regia, the sample was digested in the microwave digestion apparatus. The matrix effect and signal drift on the measurement was corrected by adding internal standard on-line. The detection limits of iodine and bromine were 0.15, 0.21 μg/g,respectively. The relative standard deviation was not more than 5.0%(n=7). The detection datas of national certi?ed standard material were consistent with the recommendation values. The method might perform directly after ammonia being added quantitatively, the memory effect in iodine detection could be reduced, and the analysis was speed up. The method can be applied to the determination of iodine and bromine in geochemical sample.
A method was estiblished for quick determination of iodine and bromine in geochemical sample by using microwave digestion–ICP–MS after digested with invers aqua regia. With the dosage of 0.1 g and 1.6 mL inverse aqua regia, the sample was digested in the microwave digestion apparatus. The matrix effect and signal drift on the measurement was corrected by adding internal standard on-line. The detection limits of iodine and bromine were 0.15, 0.21 μg/g,respectively. The relative standard deviation was not more than 5.0%(n=7). The detection datas of national certi?ed standard material were consistent with the recommendation values. The method might perform directly after ammonia being added quantitatively, the memory effect in iodine detection could be reduced, and the analysis was speed up. The method can be applied to the determination of iodine and bromine in geochemical sample.
引文
[1]李洪伟,刘晓端,李保山.地下水和土壤中不同形态碘的分离测定[J].岩矿测试,2009,28(4):337-341.
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[11]王旭日,贾振亚,陈盛,等.电感耦合等离子体质谱法测定水体中溴和碘量[J].理化检验(化学分册),2015,51(8):1 187-1 190.
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[13]DA S S,PICOLOTO R S,FLORES E M.Evaluation of bromine and iodine content of milk whey proteins combining digestion by microwave-induced combustion and ICP-MS determination[J].Food chemistry,2016,190:364-367.
[14]马新荣,李冰,韩丽荣.稀氨水密封溶解-电感耦合等离子体质谱测定土壤沉积物及生物样品中的碘溴[J].岩矿测试,2003,22(3):174-178.
[15]李海峰.检出限几种常见计算方法的分析和比较[J].光谱实验室,2010(6):2 465-2 469.
[16]田强兵.分析化学中检出限和测定下限的探讨[J].化学分析计量,2007,16(3):72-73.
[2]刘崴,杨红霞,李冰.电感耦合等离子体质谱在高碘区碘含量分布特征中的应用[J].内蒙古师范大学学报,2014,43(6):703-707.
[3]于志恒,陈崇义,谭凤珠.中国高碘地方性甲状腺肿的发现历程和分布概况[J].中华预防医学杂志,2001(5):351-352.
[4]刘崴,杨红霞,李冰.碘分析方法研究进展[J].岩矿测试,2008,27(2):127-136.
[5]SEKIMOTO S,EBIHARA M.Accurate determination of chlorine,bromine and iodine in U.S.geological survey geochemical reference materials by radiochemical neutron activation analysis[J].Geostandards&geoanalytical research,2016,41(2):124-126.
[6]BUCHERT S S A.Direct determination of copper and iodine in milk and powder in alkaaline solution by flow injection inductively coupled plasma mass spectrometry[J].Fresenius J Anal Chem,1996,354:323-325.
[7]张培新,黄光明,董丽,等.电感耦合等离子体质谱法同时测定地质样品中锗碘[J].岩矿测试,2005,24(1):36-39.
[8]李冰,何红蓼,史世云,等.电感耦合等离子体质谱法同时测定地质样品中痕量碘溴硒砷的研究[J].岩矿测试,2001,20(3):161-166.
[9]张连起.碱熔-离子树脂交换-ICP-MS法测试土壤中的溴、碘[J].世界有色金属,2016(13):75-77.
[10]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.
[11]王旭日,贾振亚,陈盛,等.电感耦合等离子体质谱法测定水体中溴和碘量[J].理化检验(化学分册),2015,51(8):1 187-1 190.
[12]刘敏.X射线荧光光谱法(XRF)测定环境地质样品中痕量氯、溴的试验研究[J].当代化工,2013(9):1 354-1 356.
[13]DA S S,PICOLOTO R S,FLORES E M.Evaluation of bromine and iodine content of milk whey proteins combining digestion by microwave-induced combustion and ICP-MS determination[J].Food chemistry,2016,190:364-367.
[14]马新荣,李冰,韩丽荣.稀氨水密封溶解-电感耦合等离子体质谱测定土壤沉积物及生物样品中的碘溴[J].岩矿测试,2003,22(3):174-178.
[15]李海峰.检出限几种常见计算方法的分析和比较[J].光谱实验室,2010(6):2 465-2 469.
[16]田强兵.分析化学中检出限和测定下限的探讨[J].化学分析计量,2007,16(3):72-73.