水浴浸提-氢化物发生-原子荧光光谱法同时测定地质样品中痕量砷和汞

采用盐酸-硝酸混合酸(盐酸-硝酸-水体积比3∶1∶4)水浴浸取地质样品,在样品消解后的母液中直接加入硫脲-抗坏血酸混合溶液,以氢化物发生-原子荧光光谱法同时测定地质样品中的痕量砷和汞。方法检出限为砷0.033 6 ng/mL,汞0.003 7 ng/mL;相对标准偏差(RSD,n=1)为砷1.1%,汞3.0%。对国家一级标准物质GBW 07109~GBW 07114、GBW 07301~GBW 07312、GBW 07401~GBW 07408中的砷和汞进行测定,测定值与标准值相吻合。     

液闪法测量水中氚放射性活度的淬灭效应

采用液体闪烁计数法进行放射性同位素测量时存在淬灭效应,而且几乎每个样品的淬灭程度都不同,并影响测量精度。采用液体闪烁计数法测量水中氚的放射性活度,淬灭是难以避免的,因此要进行淬灭校正,才能使不同淬灭程度的样品的测量结果具有可比性。淬灭校正的方法有很多,外标准校正法是一种比较可靠的方法。文章采用氚外标准校正法进行实验,得出淬灭校正曲线即探测效率E与淬灭参数SQP(E)的关系式为E=0.001 3SQP(E)-0.707 6,经过样品验证,该曲线是可靠的。采用外标准校正法适合于大批样品的测量。     

水下荧光光谱探测装置控制系统的设计与实现

海水中有色可溶性有机物(CDOM,Chromophoric Dissolved Organic Matter,常称之为黄色物质)是影响海洋水色的三大成分之一,海水中CDOM的研究具有重要的意义。本文针对CDOM水下原位探测激光诱导荧光光谱探测装置开发了一套控制系统,该控制系统分为水上甲板控制和水下数据采集两部分,水上甲板控制部分通过8芯电缆与水下数据采集部分实现供电及通信,水下数据采集部分以PC104嵌入式工控机为核心,控制整体采集部分的工作,甲板控制部分通过远程控制软件来操控PC104以实现水下数据的采集和存储。实验室环境测试及近海现场实验表明,该系统能够可靠完成水下荧光光谱装置的控制和数据的采集及通信需求,实现海水中有色可溶性有机物的水下原位探测。     

原子荧光测定食品中总砷方法的改进与探讨

针对国标《GB 5009.11—2003食品中总砷及无机砷的测定》中的原子荧光-湿法消解测定总砷的方法中存在的难于控制完全消解样品、测定结果不稳定,试剂用量大的问题,对原方法进行了3点改进。一是利用浓硫酸沸点高,能脱水碳化破坏有机物的特性,通过高温浓缩硫酸对样品进行两次脱水碳化消解,使样品消解的更完全,且节省试剂;二是针对样品中砷形态的多样性,加强温度控制,低温消解、降低易挥发砷化合物的损失,高温加速样品消解,缩短操作时间;三是加盖小漏斗制造回流,减少易挥发砷化合物的损失,使方法易操作、节省试剂。用改进的方法测定菠菜粉(GBW10015)、海带粉(GBW08517)和虾粉(CNAS T0442)中的总砷,不少于6个平行样的测定结果均位于参考值范围的中间部分,且RSD值均小于7%,表明改进的方法准确、稳定。结果还表明,200℃的硫酸、高氯酸的混合酸和高温浓硫酸均能有效消解样品中砷甜菜碱和砷糖类化合物。     

Field experiments of multi-channel oceanographic fluorescence lidar for oil spill and chlorophyll-a detection

A Multi-channel Oceanographic Fluorescence Lidar (MOFL), with a UV excitation at 355 nm and multiple receiving channels at typical wavelengths of fluorescence from oil spills and chlorophyll-a (Chl-a), has been developed using the Laser-induced Fluorescence (LIF) technique. The sketch of the MOFL system equipped with a compact multi-channel photomultiplier tube (MPMT) is introduced in the paper. The methods of differentiating the oil fluorescence from the background water fluorescence and evaluating the Chl-a concentration are described. Two field experiments were carried out to investigate the field performance of the system, i.e., an experiment in coastal areas for oil pollution detection and an experiment over the Yellow Sea for Chl-a monitoring. In the coastal experiment, several oil samples and other fluorescence substances were used to analyze the fluorescence spectral characteristics for oil identification, and to estimate the thickness of oil films at the water surface. The experiment shows that both the spectral shape of fluorescence induced from surface water and the intensity ratio of two channels (I ₄₉₅/I ₄₀₅) are essential to determine oil-spill occurrence. In the airborne experiment, MOFL was applied to measure relative Chl-a concentrations in the upper layer of the ocean. A comparison of relative Chl-a concentration measurements by MOFL and the Moderate Resolution Imaging Spectroradiometer (MODIS) indicates that the two datasets are in good agreement. The results show that the MOFL system is capable of monitoring oil spills and Chl-a in the upper layer of ocean water.     

基于三维荧光光谱-平行因子技术联用的浮游藻化学分类学技术研究

An in vivo three-dimensional fluorescence method for the determination of algae community structure was developed by parallel factor analysis(PARAFAC) and CHEMTAX. The PARAFAC model was applied to fluorescence excitation-emission matrix(EEM) of 60 algae species belonging to five divisions and 11 fluorescent components were identified according to the residual sum of squares and specificity of the composition profiles of fluorescent. By the 11 fluorescent components, the algae species at different growth stages were classified correctly at the division level using Bayesian discriminant analysis(BDA). Then the reference fluorescent component ratio matrix was constructed for CHEMTAX, and the EEM–PARAFAC–CHEMTAX method was developed to differentiate algae taxonomic groups. The correct discrimination ratios(CDRs) when the fluorometric method was used for single-species samples were 100% at the division level, except for Bacillariophyta with a CDR of 95.6%. The CDRs for the mixtures were above 94.0% for the dominant algae species and above 87.0% for the subdominant algae species. However, the CDRs of the subdominant algae species were too low to be unreliable when the relative abundance estimated was less than 15.0%. The fluorometric method was tested using the samples from the Jiaozhou Bay and the mesocosm experiments in the Xiaomai Island Bay in August 2007. The discrimination results of the dominant algae groups agreed with microscopy cell counts, as well as the subdominant algae groups of which the estimated relative abundance was above 15.0%. This technique would be of great aid when low-cost and rapid analysis is needed for samples in a large batch. The fluorometric technique has the ability to correctly identify dominant species with proper abundance both in vivo and in situ.     

微波消解—冷原子荧光光谱法测定植物样品中的汞

为了简化测量植物中汞含量的方法,提高灵敏度及结果的可信度,实验采用微波消解植物样品的办法,使样品经氯化亚锡还原,再用冷原子荧光测定出植物样品中汞的含量。确定了消解样品的方法和微波消解样品的条件,优化了仪器的最佳工作参数。方法检出限0.30×10-9(稀释因子100倍),精密度(n=12)在2.09%~6.05%,加标回收率94.1%~105.5%,方法经生物国家一级标准物质验证方法准确可靠。     

The Study Internal Structure of the Annual Layers in Lake Sediments Using Synchrotron Radiation with X-ray Focusing Optics

正1 Introduction Annually laminated(varve)sedimentary deposits are considered as one of the most important archives,since they offer precise temporal information(years)in combination with high time resolutions.Bottom sediments of the lakes contain detailed geochemical information on     

无色散原子荧光光谱法测定痕量汞

氯化亚锡还原冷蒸汽无色散原子荧光光谱法测定痕量汞,采用硫酸、双氧水、王水逐次加入低温分析样品,可以保证样品分解完全又可避免汞的损失。汞的检出限为6.0×10~(-10)g,精密度RSD％=4.1。该方法操作简便,快速、准确、费用低,可应用于大批量地球化学样品的分析。     

主成分分析法在油荧光光谱波段选择中的应用

355nm激光器发射激光入射到海水表面，激发海表面溢油的荧光光谱，运用高光谱图像降维中应用广泛的分段主成分分析算法对油荧光光谱进行波段选择。该算法把每个分段被映射到主成分的信息量的大小作为是否被选择的标准，保证了选择波段的信息丰富；通过分段分析消除了传统主成分分析的全局性引起的波段忽略问题，获得较为满意的降维效果。