样品中痕量元素的分析及其容器的选择和清洗

绪言对痕量元素的测定,特别是液体样品,由于空白分析产生的偏差,通常认为大部分是由于采样和贮藏容器的污染而引起的。对于液体样品中痕量元素的测定的改进取决于所用的塑料以及使用前所用的清洗方法。关     

痕量分析中容器的选择与洗涤

在痕量分析中,为获得准确的分析结果,容量材质以及洗涤方法的选择至关重要。试验分析表明:聚乙烯是较好的容器材料,它玷污最小、易洗涤、价廉、容器清洗。经实验证明:蒸汽法效果好,但需要相应装置;浸泡法简单易行,但消耗较大。其他方法则各有利弊,因此可根据不同的分析元素及特征,选择合适的洗涤方法。     

甲醛法测定空气中二氧化硫影响因素分析

甲醛吸收-副玫瑰苯胺分光光度法是测定环境空气中的二氧化硫的常用方法,该方法具有灵敏度高、选择性好等优点,但在实验分析过程中发现,该方法对实验室环境条件、反应条件、试剂的质量和实际操作要求严格。文章通过对影响空白值及检测结果的显色温度、显色时间、实验试剂、样品的采集及保存等关键因素进行实验分析,使校准曲线斜率和试剂空白吸光度值在给定的检测条件下满足检测方法标准的要求,为提高甲醛法测定空气中二氧化硫测量结果的准确性提供参考。     

中药川附子非金属元素分析

本文论述了川附子非金属元素的分析：用ICP—AES法测定S、P和Si；离子色谱法测定Cl、S、P；极谱法和HG—AFS法测定痕量砷；ICP—AES和荧光法测定硒；GB法测定氯、氟和碘。应用提出的方法弄清了川附子用传统工艺食盐-胆巴混合溶液炮制前后非金属元素的含量与浓度变化，从而为中药化学成分进一步研究增添新内容一非金属元素及检测方法。     

搅拌棒吸附萃取技术在环境样品分析中的应用

搅拌棒吸附萃取(SBSE)是继固相微萃取(SPME)之后的又一种无溶剂的用于痕量有机物分离和浓缩的技术,其萃取涂层体积大,具有灵敏度高、检出限低、重现性好、不使用有机溶剂等优点。适用于环境样品中挥发性及半挥发性有机物的痕量分析。本文综述了SBSE在环境样品分析中的应用,以及该技术的应用展望。     

混合酸水浴消解-原子荧光光谱法测定土壤和沉积物中痕量汞、砷、硒、铋和锑元素

为改进环境标准HJ 680-2013检测方法,采用原子荧光光谱法测定混合酸水浴消解法前处理土壤和沉积物样品中痕量汞、砷、硒、铋和锑元素。以GBW07430、GBW07446、GBW07452探讨15种混合酸消解体系对不同类型样品痕量元素测定结果的影响,筛选得到采用盐酸-硝酸-硫酸-高氯酸-过氧化氢（体积比为4∶2∶0.5∶0.5∶0.5）体系为消解液的痕量检测最佳实验条件。水浴法消解前处理,消解时间为1.0h,处理时间为2.5h。5种元素的质量浓度范围在0.10～10.0 mg/kg线性相关系数大于0.999,检出限范围0.002～0.025 mg/kg,定量限范围0.008～0.100 mg/kg,测定结果的相对标准偏差范围为1.45%～5.19%,样品加标回收率范围为89.2%～119%。经国家一级土壤成分分析标准物质验证该方法,并成功应用于环境中农业与建筑用土壤及管道淤泥沉积物实际样品的前处理,结果准确可靠,适用多元素一次处理,解决高通量样品的测定需求,满足环境检测分析工作。     

实验用水对总氮检测结果的影响

用RO纯水与超纯水分别作为实验用水,通过标准曲线及空白、标准样品、水样等总氮测定对比实验,发现两种实验用水的标准曲线及空白值、标准样品的检测均受控,但两种纯水对比实验显示相对于超纯水而言,RO纯水中有一定浓度的总氮,同时在水样检测中用RO纯水作实验用水测定值明显低于用超纯水作实验用水的测定值,其差值与RO纯水中总氮值相符。实验结果表明总氮检测中不能只以标准曲线、空白值和标准样品测定值作为受控标准,要考虑实验用水中硝酸根离子的影响。     

环境监测中仪器分析方法不确定度的评估(Ⅱ)——原子吸收光谱分析中的测量不确定度

通过对环境样品分析中常用的原子吸收光谱法测量不确定度分量的分析,探讨了原子吸收光谱法测量不确定度的评估方法,针对不同环境基体样品、不同测定组分以及不同前处理方法的扩展不确定度进行了评定。原子吸收光谱分析中的测量不确定度主要来源于样品称量、消化液定容、仪器漂移及由吸收值通过标准曲线拟合求浓度部分,其中最主要的分量是由吸收值通过标准曲线拟合求样品溶液浓度时引起的测量不确定度。     

煤炭资源开发过程中有害痕量元素的迁移

煤炭中含有多种痕量元素，这些痕量元素随着煤炭的采掘、煤矸石的堆放、洗煤废水的排放等过程进入环境。研究这些元索与环境之间相关关系及迁移速度对污染源调查及污染物防治具有重要的意义。在分别对六盘水市大河边、那罗、大湾、老鹰山、汪家寨等5个矿区煤炭及矿区废水中Li、Be、Cr等37种痕量元素分析的基础上，将这37种痕量元素的关系分为关联性强、较强和弱3种，其中关联性强的痕量元素迁移能力由强到弱依次是Zn、Cr、Be、Cd、Cu、Gd、Sm、Ho、Yb等9种。     

有机磷类农药残留分析检测技术研究进展

用样品前处理、样品分析检测两个方法,阐述近几年常用的有机磷类农药残留分析检测技术原理及优缺点,并提出未来样品前处理技术及有机磷类农药检测技术的发展趋势。     

HP6890色谱柱用于环境空气中微量恶臭硫化物的检测

利用HP6890型气相色谱仪进行环境空气中微量恶臭硫化物分析,实验结果表明:分离效果、峰形都很好,实验采用4种柱箱初始温度及升温程序,分别由初始温度70℃升温至90℃、120℃、130℃及由初始温度150℃,最后升温至190℃,相应分析一个样品的时间依次为:130.515min、63.419min、56.359min及11.116min,样品分析时间大大缩短,可提高分析效率。     

化学发光法在环境样品检测中的应用

综述了化学发光法用于分析检测的基本原理,化学反应过程中产生光的量与发光物质的含量成正比。化学发光方法对环境样品检测具有灵敏度高、线性响应范围宽、可以实现自动化等优点,通过发射光的比率可以推定未知成分的浓度,测定环境样品中被测物质的量。化学发光法已广泛应用到环境样品检测、药物分析等领域。     

电感耦合等离子体发射光谱法测定环境水样中总磷的干扰及消除

溶液稀释法是一种简单有效的消除非光谱干扰的方法,背景扣除法、干扰系数法是消除光谱干扰的简单常用方法;应用于实际水样分析,效果较好。电感耦合等离子体发射光谱法(ICP-OES)对水样中总磷的测定尚没有国家标准方法,本文对ICP-OES法测定磷的干扰及校正情况给以浅析,更适于环境水样的快速、批量分析。方法检出限、测定下限能满足环境水样的分析要求。     

Infrared analysis for counterfeit electronic parts detection and supply chain validation

Within the electronics industry, counterfeit electronic components entering the supply chain have steadily become an increasing threat accounting for more than 8 % of global merchandise trade and an annual $600 billion enterprise. Currently, there are not many cost-effective and nonintrusive solutions for counterfeit detection of electronic parts. In this paper, the authors present a statistical approach for detecting counterfeit components based on infrared (IR) analysis by the use of independent component analysis (ICA). As a prominent higher-order statistical analysis technique, ICA is capable of extracting relevant features from IR data. The latest applications and the extended algorithms of ICA have been elucidated for the purposes of classification and identification of counterfeit electronic parts. The theoretical framework of ICA is presented along with extensive experimental results to illustrate its feature extraction function in counterfeit electronic parts detection.     

The global greenhouse effect

The global warming caused by emissions of CO₂ and trace gases is expected to cause shifts in climatic zones and rainfall patterns, and possibly thermal expansion of oceans. There are likely to be impacts on global agriculture and the food security of low-income countries, as well as disruptions to major ecosystem complexes such as forests. Rising sea levels will threaten low-lying regions, coastal zones and islands. Policy-makers will therefore have to consider the relative costs and benefits of 'doing nothing', preventive measures and adaptive responses. Economics should play a key and innovative role in this analysis.     

ESTIMATING CENTRAL TENDENCY FROM UNCENSORED TRACE LEVEL MEASUREMENTS1

ABSTRACT: The statistical analysis of data which have trace level measurements has traditionally been a two-step process in which data are first censored using criteria based on measurement precision, and then analyzed with statistical methods for censored data. The process might be more informative if data were left uncensored. In this paper, information loss attributable to censoring and measurement noise are assessed by comparing the sample mean and median of uncensored measurements with a log regression mean and median based on censored data. Measurements are derived from lognormal parent distributions which have random variability characteristic of trace level measurement. The relative performance of estimators used with error-free samples and with samples having measurement noise can be explained by differences between the probability distributions of parents and measurements. Measurement introduces bias and dispersion and transforms lognormal parent distributions toward greater symmetry. Estimates using uncensored data are less biased and more accurate than the log regression mean and median when censoring exceeds about 50 percent, and are not much worse at any fraction censored. For data with many (80 percent) results below the limit of detection, bias may be quite severe.     

微波消解-ICP—MS测定土壤和水系沉积物中的重金属

建立了一种采用逆王水和氢氟酸的混合体系微波酸消解土壤与水系沉积物,电感耦合等离子体质谱法快速测定六种金属元素（As、Cd、Pb、Cu、Cr和Ni）含量的方法。本文研究了消解温度和消解时间对消解效果的影响。结果表明,在190℃下运行25分钟对土壤与水系沉积物中的六种金属元素均具有很好的消解能力,备元素的测定值与标准值相符。在对实际土壤与水系沉积物样品进行分析后得出采样区域的土壤与沉积物中这六种金属含量水平正常。     

Application of enzyme-linked immunosorbent assay analysis for determination of monensin in environmental samples

There is growing concern that antibiotic use in livestock production is contributing to contamination of soil and aquatic environments. Monensin, a polyether ionophore antibiotic, accounts for approximately 13% of total subtherapeutic livestock antibiotic usage in the USA and has been widely detected in aquatic environments. Due to insufficient ultraviolet absorbance, liquid chromatography analysis of monensin in environmental samples is limited to equipment with mass spectrometry (e.g., liquid chomatography-mass spectrometry [LC-MS]). However, LC-MS equipment is costly, and extensive sample preparation and clean-up is often required. Rapid, low-cost analytical techniques are needed to monitor for monensin residues in the environment. In this study, a commercially available enzyme-linked immunosorbent assay (ELISA) for detecting monensin in animal feed extracts was evaluated for determination of monensin in water, soil, and manure. The monensin ELISA was highly sensitive, with limits of detection and quantification at 1.5 and 3.0 microg L(-1), respectively. Recovery of monensin in spiked water samples was approximately 100%. Cross-reactivity was not observed with similar polyether ionophores, tetracyclines, macrolides, or sulfonamides. Concentrations of monensin using ELISA were greater than concentrations measured with LC-MS. This is attributed to cross-reactivity of the monensin ELISA toward structurally similar monensin compounds, such as factors (slight naturally produced structural variants) and metabolites. Results from this study showed that ELISA can be a reliable, rapid, and low-cost alternative to LC-MS analysis of environmental samples.     

Combined application of QEM-SEM and hard X-ray microscopy to determine mineralogical associations and chemical speciation of trace metals

We describe the application of quantitative evaluation of mineralogy by scanning electron microscopy in combination with techniques commonly available at hard X-ray microprobes to define the mineralogical environment of a bauxite residue core segment with the more specific aim of determining the speciation of trace metals (e.g., Ti, V, Cr, and Mn) within the mineral matrix. Successful trace metal speciation in heterogeneous matrices, such as those encountered in soils or mineral residues, relies on a combination of techniques including spectroscopy, microscopy, diffraction, and wet chemical and physical experiments. Of substantial interest is the ability to define the mineralogy of a sample to infer redox behavior, pH buffering, and mineral-water interfaces that are likely to interact with trace metals through adsorption, coprecipitation, dissolution, or electron transfer reactions. Quantitative evaluation of mineralogy by scanning electron microscopy coupled with micro-focused X-ray diffraction, micro-X-ray fluorescence, and micro-X-ray absorption near edge structure (mXANES) spectroscopy provided detailed insights into the composition of mineral assemblages and their effect on trace metal speciation during this investigation. In the sample investigated, titanium occurs as poorly ordered ilmenite, as rutile, and is substituted in iron oxides. Manganese's spatial correlation to Ti is closely linked to ilmenite, where it appears to substitute for Fe and Ti in the ilmenite structure based on its mXANES signature. Vanadium is associated with ilmenite and goethite but always assumes the +4 oxidation state, whereas chromium is predominantly in the +3 oxidation state and solely associated with iron oxides (goethite and hematite) and appears to substitute for Fe in the goethite structure.