环境和生物样品中铂族金属的分析研究进展

评述了近年来环境和生物样品中痕量铂族金属的分析研究进展，重点介绍了样品的预处理和分离富集技术以及检测手段等。     

乳化技术-火焰原子吸收光谱法测定清漆中的猛、铅

1引言 清漆中的微量元素主要来自添加的催干剂，催干剂能加速清漆基料中的不饱和双键经空气氧化而固化成膜。常用的催干剂为锰、铅、钙等金属的环烷酸盐或异辛酸盐。涂料样品的预处理方法通常是将样品在105～129℃烘干、研细，然后采用灰化法或消化法处理，其缺点是耗时长、污染环境。本文将清漆样品制成乳浊液，样品处理全过程只需十几分钟，方法简便。用乳化技术火焰原子光谱法测定清漆中的微量元素还未见报道。     

电感耦合等离子体-原子发射光谱测定再生加氢催化剂中活性组分Mo、Ni及金属杂质

针对再生加氢催化剂中残余的积炭对活性金属含量测定的影响,建立了一种以硝酸-高氯酸体系溶解样品,电感耦合等离子体原子发射光谱(ICP-AES)测定再生加氢催化剂中活性金属Mo、Ni含量的方法。该方法亦可同时测定运转过程中沉积在催化剂表面的金属杂质Fe、Na、Ca、Mg的含量。实验考察了仪器工作参数、不同预处理方法、介质酸度、基体A1对测量结果的影响。本法对Mo、Ni、Fe、Na、Ca、Mg 6种元素的检出限分别为0.1797、0.0026、0.0014、0.0220、0.0022、0.0013μg/g,回收率在95%~107%之间。该法准确、可靠,精密度好,可用于实际样品分析。     

不同预处理方法对巴戟中砷限量检查的影响

采用５种不同预处理方法对巴戟药材进行处理，并用古蔡氏砷斑法检测其含量，发现不同处理方法的检测结果相差甚大，为中药砷限量检查中正确选择样品预处理方法提供了参考。     

石墨炉原子吸收光谱法直接测定液压油中铬

分析机械的液压油、润滑油中磨损金属的含量 ,可以适时监控机械运转、预测机械故障[1] 。目前 ,测定液压油中痕量金属元素一般都需要对油样进行预处理后再测定。常用的干灰化法[2 ] 等预处理方法 ,操作繁琐、分析时间长。在石墨炉原子吸收光谱法 (ＧＦＡＡＳ)直接进样测定液压油中金属元素方法中 ,稀释剂常用二甲苯等有机物 ,因此 ,配制标准溶液必须用金属有机化合物[3] 。而有机金属化合物稳定性较差 ,容易分解。本法基于石墨炉本身对样品基体具有灰化处理能力这一特点[4 ] ,在液压油中加无机标准溶液和混合有机溶剂组成均相体系 ,直接进样…     

一种基于近红外光谱技术的不同品种及掺假三七的无损鉴别分析研究

基于近红外光谱技术与化学计量学方法,提出了一种不同品种及掺假三七的快速无损鉴别方法。分别采集景天三七、菊三七、血三七、田三七完整、粉末及掺假样品的近红外光谱,采用单一和组合预处理方法消除光谱中的干扰,筛选出最佳的预处理方法;结合主成分分析法建立不同品种以及掺假三七样品的鉴别模型。结果表明：结合主成分分析,采用原始光谱即可实现粉末及掺假样品的100%鉴别分析,而完整样品由于受到物理性状的干扰,其原始光谱数据的品种鉴别率仅为9.38%;而经连续小波变换预处理后可达93.75%。采用组合预处理方法可以进一步消除光谱存在的多种干扰,显著提高完整样品的鉴别准确性,采用去偏移 + 一阶导数、去偏移+连续小波变换以及二阶导数+标准正态变量变换预处理方法预处理后,完整样品的鉴别准确率达到了93.75%。以上结果表明,采用近红外光谱技术与化学计量学方法可有效实现对不同品种以及掺假三七的快速无损鉴别分析。     

石墨炉原子吸收法测定肼类推进剂中九种金属杂质

建立了石墨炉原子吸收法测定肼类推进剂中锌、铁、铬、锰、铅、镍、铝、铜、钛等金属含量的检测方法 ,无需样品预处理过程 ,灵敏度高且快速、准确。各元素测定方法的精密度小于 1 0 % ,回收率在 82 %～ 1 1 6%之间。     

一种金属含量分析用的样品预处理方法

一种金属含量分析用的样品预处理方法，包括将油样在惰气中升温至450-700℃进行蒸发灰化，使其中的可挥发物蒸发，金属元素保留在蒸发后的残余物中；将残余物氧化，使其中的金属元素转化为金属氧化物；     

平台石墨炉原子吸收法直接测定柑桔皮提取物中的痕量硒

本文提出了一种以正丁醇为溶剂、平台石墨炉原子吸收法直接测定油状样品中硒的方法。该方法简单、快速、无需样品 预处理，既提高了分析效率，又避免了预处理过程中硒的损失。     

电极法测定废水中氨氮

介绍了采用电极法测定废水中氨氮时,以吹气法代替蒸馏法对废水水样进行预处理,简化了水样预处理的程序,样品中氨氮的释出率可达90%,加标回收率在60%-98.8%之间。对两种废水样各分析8次,得出其RSD值均小于5%。按3倍标准偏差计算方法的检出限为0.008 mg.L-1。定量测定的最高值为350 mg.L-1。     

钇对苯甲酸芳香体系的效应钇在镧系元素中的位置

钇对苯甲酸芳香体系的效应加以研究并与碱和碱土金属以及若干过渡金属和有毒的重金属的效应相比较。钇与镧系元素相似,具有稳定苯甲酸体系的效应。芳香体系的微扰作用随着金属离子势的减小而增大。红外谱带强度的详细分析表示钇的位置是在铒与铥之间。芳香环谱带的相对强度和频率对于镧系元素原子序数的依赖关系表明双-双效应的存在。     

钇对苯甲酸芳香体系的效应钇在镧系元素中的位置

钇对苯甲酸芳香体系的效应加以研究并与碱和碱土金属以及若干过渡金属和有毒的重金属的效应相比较。钇与镧系元素相似,具有稳定苯甲酸体系的效应。芳香体系的微扰作用随着金属离子势的减小而增大。红外谱带强度的详细分析表示钇的位置是在铒与铥之间。芳香环谱带的相对强度和频率对于镧系元素原子序数的依赖关系表明双-双效应的存在。     

AROMATIC AND HETEROCYCLIC DINITRILES AND THEIR POLYMERS ⅪⅤ. STUDY ON THE CATALYSTS OF THE POLYMERIZATION OF AROMATIC NITRILES*

Various catalysts for the polymerization ot aromatic nitriles were investigated. It was found that Lewis acid-metal is a preferable catalyst system for the polymerization of aromatic nitriles, and the polymerization rate is about 10 times faster than Lewis acid alone. The polymerization rate of benzonitrile catalyzed by Lewis acid and different metals was measured, and the activity of metals was in the following decreasing order ,magnesium, zinc, sodium, calcium. Furthermore, the polymerization of benzonitrile catalyzed by different Lewis acid and zinc was also investigated.     

On-line collection/concentration and determination of transition and rare-earth metals in water samples using Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry

On-line preconcentration and determination of transition and rare-earth metals in water samples was performed using a Multi-Auto-Pret system coupled with inductively coupled plasma-atomic emission spectrometry (ICP-AES). The Multi-Auto-Pret AES system proposed here consists of three Auto-Pret systems with mini-columns that can be used for the preconcentration of trace metals sequentially or simultaneously, and can reduce analysis time to one-third and running cost of argon gas and labor. A newly synthesized chelating resin, ethylenediamine-N,N,N′-triacetate-type chitosan (EDTriA-type chitosan), was employed in the Multi-Auto-Pret system for the collection of trace metals prior to their measurement by ICP-AES. The proposed resin showed very good adsorption ability for transition and rare-earth metal ions without any interference from alkali and alkaline-earth metal ions in an acidic media. For the best result, pH 5 was adopted for the collection of metal ions. Only 5 mL of samples could be used for the determination of transition metals, while 20 mL of samples was necessary for the determination of rare-earth metals. Metal ions adsorbed on the resin were eluted using 1.5 M nitric acid, and were measured by ICP-AES. The proposed method was evaluated by the analysis of SLRS-4 river water reference materials for trace metals. Good agreement with certified and reference values was obtained for most of the metals examined; it indicates that the proposed method using the newly synthesized resin could be favorably used for the determination of transition and rare-earth metals in water samples by ICP-AES.     

Determination of heavy metals by isotachophoresis

The suitability of isotachophoresis for the analysis of metals in, e.g., environmental samples was studied. In a cationic operational system the heavy metals Fe, Cu, Ni, Cd, Co, Zn, Pb and Mn were simultaneously determined. The separation was achieved through complex formation with one of the counter ions, hydroxyisobutyric acid. The other counter ion was acetic acid, the leading ion was 0.02 M potassium or sodium (pH 4.1) and the terminator was H+. The analysis time was 15 min at 60 microA in a 0.2 mm I.D. capillary. Aqueous samples containing ppm and ppb amounts were enriched on a cation exchanger with an extremely low affinity for sodium (Chelex 100). Good recovery, linearity, precision and accuracy were obtained even down to the ppb range. Although the sensitivity of the method is not greater than that of some of the more established methods for the individual metals, a great advantage of isotachophoresis is the simultaneous determination of the metals, with equal response factors. An example is given of the determination of metals, including aluminium, in serum.     

电感耦合等离子体质谱(ICP-MS)法检测市售鱿鱼中5种重金属

基于硝酸消解体系,建立了微波消解-电感耦合离子体质谱(ICP-MS)法同时测定市售鱿鱼中铅、砷、镉、汞、铬5种重金属元素的检测方法。样品加入HNO₃进行微波消解,优化ICP-MS 相关检测参数后,进行外标法定量。结果表明,5种重金属在各自浓度范围内线性关系均＞0.999,平均回收率为96%-101%,精密度RSD均小于5%。用该法检测广州市农贸市场随机购买的6个批次冰鲜鱿鱼,结果有1个批次砷含量超标,1个批次镉含量超标。该法前处理简单,检测准确、快速,适用于鱿鱼等水产品中铅、砷、镉、汞、铬等重金属的检测。     

应用绕丹宁衍生物测定贱金属研究的国内现状

绕丹宁衍生物是光度法测定贵金属的一类传统显色剂,这类试剂容易合成,近年来涌现出一批新型绕丹宁衍生物,除测定贵金属外,已拓展到一些贱金属的分析测定.分析手段已由传统的吸光光度法向荧光光度法和催化动力学荧光分析法转移,使测定的灵敏度和选择性大大提高.根据文献检索,将国内在这一领域的研究应用现状进行介绍.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定电镀废弃物中的七种元素

采用HCl-HNO3-HF-HClO4体系溶解试料,电感耦合等离子体原子发射光谱法测定电镀废弃物中的钙、铝、镉、钴、铁、锰、镁七种元素含量。通过加标回收实验,这几种元素的加标回收率为96.1%~102%,相对标准偏差均小于3%(n=7),此方法操作速度快、检测效率高,是一种理想的分析方法。     

Determination of trace metals in seawater by an automated flow injection ion chromatograph pretreatment system with ICPMS

A novel flow injection ion chromatograph (FI-IC) system has been developed to fully automate pretreatment procedures for multi-elemental analysis of trace metals in seawater by inductively coupled plasma mass spectrometer (ICPMS). By combining 10-port, 2 position and 3-way valves in the FI-IC manifold, the system effectively increase sample throughput by simultaneously processing three seawater samples online for: sample loading, injection, buffering, preconcentration, matrix removal, metal elution, and sample collection. Forty-two seawater samples can be continuously processed without any manual handing. Each sample pretreatment takes about 10 min by consuming 25 mL of seawater and producing 5 mL of processed concentrated samples for multi-elemental offline analysis by ICPMS. The offline analysis improve analytical precision and significantly increase total numbers of isotopes determined by ICPMS, which include the metals Al, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, Ti, V, and Zn. The blank value and detection limits of trace metals using the system with ICPMS analysis all range from 0.1 to 10 parts per trillion (ppt), except Al, Fe, and Zn. The accuracy of the pretreatment system was validated by measuring open-ocean and coastal reference seawater, NASS-5 and CASS-4. Using the system with ICPMS analysis, we have obtained reliable trace metal concentrations in the water columns of the South China Sea. Possessing the features of full automation, high throughput, low blank, and low reagent volume used, the system automates and simplifies rigorous and complicated pretreatment procedures for multi-elemental analysis of trace metals in seawater and effectively enhances analytical capacity for trace metal analysis in environmental and seawater samples.     

海水重金属电化学传感器检测系统

研制了一种新型的海水重金属电化学传感器流动分析系统.通过在线过滤、紫外线消解、电化学富集以及离子选择性电极电位测定等过程,实现对海水重金属的高灵敏、高选择性的快速检测.在海水基体条件下,对于镉、铅和铜的测定线性范围分别为1.0×10-9～1.0×10-7 mol/L,3.0×10-9～1.0×10-7 mol/L和1.0×10-9～1.0× 10-7 mol/L,相应检出限为2.8×10-10,6.6×10-10和5.1×10-10 mol/L,连续6次测定的RSD均小于5％,全程分析在25 min内完成.应用于实际海水样品分析,其测定结果与溶出伏安法一致.此传感器性能可靠、成本低廉,在海水重金属现场快速监测方面具有良好的应用前景.