Inductively Coupled Plasma-Mass Spectrometric Determination of Rare Earth Elements in Estuarine Water with Co-precipitation Pre-concentration

建立了氢氧化铟共沉淀预富集 -电感耦合等离子体质谱法测定河口水体中痕量稀土元素的方法。实验结果表明 ,在80mg·L -1的In3 +和pH9.5的实验条件下 ,在1.0L水样中添加5.0～200.0ng的混合稀土标准溶液 ,均能定量回收 ,回收率在82.2 %～106.9 %之间。方法的分析流程空白为0.04(Tb)～10.17(La)ng·L -1,检出限在0.17(Yb)～1.46(La)ng·L-1之间 ,精密度 (RSD ,n=3)小于11.7 % ,可满足河口淡水和海水样品中的痕量稀土元素定量分析的要求Amethod for the determination of rare earth elements(REEs)in estuarine water by inductively couˉpled plasma mass spectrometry(ICP-MS)using In(OH) 3 co-precipitation for pre-concentration has been deˉveloped.The optimized amount of In 3+ for the precipitation of the analytes in1.0L water sample was80mg at pH9.5.The recoveries were88.9%～106.9%by spiking5～200ng REEs standards into1.0L water sample.The blank values of the developed method ranged from0.04ng·L -1 for Tb to10.17ng·L -1 for La.The detection limits of the REEs ranged from0.17ng·L -1 (Yb)to1.46ng·L -1 (La)and the relative standard deviations were1.2%～11.7%(n=3).The developed method has been used for the determinaˉtion of REEs in Yangze estuarine water samples.国家自然科学基金资助项目 (40076023

BPSK调制高动态遥测接收机的设计

针对BPSK调制的高动态遥测接收机的多普勒频率漂移大和码元符号周期随着多普勒变化的问题, 提出了一种全数字的接收机结构, 研究了载波频率跟踪和码元符号定时跟踪的跟踪算法, 指出了跟踪环路的稳定条件。仿真验证了该算法和接收机结构的可行性, 结果表明, 该接收机在初始频偏23 kHz、加速度20g、载波初始相位π/2、码环初始偏差5/8个码元的条件下仍能稳定捕获和跟踪

Geochemical behaviors of rare earth elements in sediments of the estuary of Yangtze River

用电感耦合等离子体质谱法测定了2002年8~9月航次丰水期采集的长江口表层沉积物样品,对稀土元素(REEs)在沉积物的中含量分布、配分模式及其与某些常量矿物成份之间的相关关系进行了研究.结果表明,长江口表层沉积物中REEs含量在0.17μg/g(Lu)~78.9μg/g(Ce)之间,含量高低顺序为Ce>La>Nd>Sm>Yb>Eu>Tb>Lu;用PAAS和世界平均页岩的REEs含量进行Ce、Eu异常值的计算结果表明,长江口沉积物中Ce和Eu均表现出轻微正异常;沉积物中REEs在轻稀土元素(LREE)富集的基础上,表现出中稀土元素(MREE)相对富集的特征,其中用PAAS标准化后MREE富集程度比用世界平均页岩标准化后的结果要明显.通过比较沉积物和悬浮颗粒物的分馏表征值、REEs含量和浓度变化范围等,认为长江口沉积物的主要来源是水体悬浮颗粒物.本文对REEs与A l2O3和Mn的相关性研究还发现,两者与重稀土元素(HREE)有较明显的正相关关系,其中A l2O3与HREE的线性相关性较好.To assess the distribution pattern and the fraction during estuary mixing processes and river transportation,the concentrations of rare earth elements(REEs) in sediments of the estuary of Yangtze River,China,were measured using acid digestion and inductively coupled plasma mass spectrometry(ICP MS).As results,REEs contents in sediments are found in range of 0.17μg/g(Lu)～78.9μg/g(Ce).In sediments the concentration level of REEs follows the order:Ce>La>Nd>Sm>Yb>Eu>Tb>Lu.The lack of any significant anomalies for Ce and Eu suggests that redox processes did not play important roles in redistribution of REEs.Normalized patterns of REEs in sediments by PAAS are dominated by a distinct convexity centered on Eu,which suggests an enrichment of MREE over both LREE and HREE.Plots of PAAS-normalized REEs data in sediments are similar to that of the residual fraction in suspended matter.国家自然科学基金资助项目(40076023

Determination of Rare Earth Elements in Marine Organisms by Inductively Coupled Plasma-Mass Spectrometry with Microwave Digestion

建立了微波消解样品处理、电感耦合等离子体质谱法测定海洋生物体中稀土元素的方法。用人发标准参考物质(GBW09101)、植物标准参考物质(GBW07603)以及实际样品标准加入回收的方法对文中所述的分析流程进行确认。实验结果表明,所建立方法的测定结果与标准参考物质的标准值或推荐值一致;样品标准加入实验的回收率在97%~104%之间。方法的定量下限为0.01~0.31 ng.g-1(10σ,n=10,干样)。A method was developed for the determination of rare earth elements in marine organisms by inductively coupled plasma-mass spectrometry(ICP-MS) with microware digestion.The method was validated with human hair SRM(GBW09101),plant SRM(GBW07603),and standard spiked real samples.The results obtained by the proposed method agreed quite well with the certified or recommended values of SRM.The recoveries of REEs spiked to human hair SRM(GBW09101) and real sample ranged from 97% to 104%.The limits of quantification(LOQ) of REEs ranged from 0.01 to 0.31 ng·g(-1) in solid sample.国家自然科学基金资助项目(40076023

Geochemical behaviors of rare earth elements in the estuary of Changjiang River in China

国家自然科学基金资助项目(40076023)