岛津C－R2A全自动高效液相色谱分析程序的设计

 利用Ｃ－Ｒ２Ａ色谱处理机的编程功能，实现了液相色谱法（主机为ＬＣ－４Ａ和ＳＩＬ－２ＡＳ自动进样器）全自动分析，即通过程序实现按设定的样品顺序、进样量、重复次数对样品进行测定，每个样品分析完后，进行数据处理。     

岛津C－R2A全自动高效液相色谱分析程序的设计

利用Ｃ－Ｒ２Ａ色谱处理机的编程功能，实现了液相色谱法（主机为ＬＣ－４Ａ和ＳＩＬ－２ＡＳ自动进样器）全自动分析，即通过程序实现按设定的样品顺序、进样量、重复次数对样品进行测定，每个样品分析完后，进行数据处理，并打印出结果表     

含7—氨基—4—甲基香豆素的蛋白酶荧光底物

本文设计并合成了一系列含７－氨基－４－甲基香豆素的肽类荧光底物，通过动力学测定研究了氨基酸结构对底物专一性的影响，发现Ｓｕｃ－Ａｌａ－Ａｌａ－Ｐｈｅ－ＡＭＣ和Ｓｕｃ－Ａｌａ－Ｐｒｏ－Ｐｈｅ－ＡＭＣ是较好的胰凝乳蛋白酶荧光底物。     

CS2水解催化反应动力学补偿效应

考察了常压下ＣＳ２水解催化剂活性组分含量和温度对ＣＳ２水解的综合影响，并进行了ＣＳ２水解动力学研究，发现在所研究的４个系列催化剂中都存在着补偿效应，在反应温度范围内，Ａ、Ｅ两类催化剂符合“顺Ａｒｒｈｅｎｉｕｓｆｗｔｖ”；而Ｏ、Ｃ两类催化剂符合“反Ａｒｒｔｈｅｎｉｕｓ规律”，另外，针对多相表面催伦反应过程，提出了修正的阿累尼乌斯公式，即：ｋ＝Ａ‘ｅｘｐ（△Ｅ／ＲＴ）ｅｘｐ（－Ｅａ／ＲＴ），且从此角度     

含氢聚甲基硅氧烷/丙烯酸丁酯/羟甲基丙烯酰胺复合乳液的研究——原料配比对乳液及胶膜性能的影响

采用含氢聚甲基硅氧烷（ＰＨＭＳ）与丙烯酸酯类单体进行接枝共聚，制得兼具二者优异性能的新型ＰＨＭＳ／丙烯酸丁酯（ＢＡ）／羟甲基丙烯酰胺（ＮＭＡ）复合聚合物乳液．讨论了ＰＨＭＳ、ＮＭＡ和引发剂用量对该复合乳液的聚合反应转化率、稳定性及粘度的影响．采用透射电子显微镜和粒度测试仪对不同反应条件下制备的乳液的粒度进行了测定．同时对聚合反应的机理、产物的结构及胶膜性能作了考察．结果表明：通过乳液聚合，得到了ＰＨＭＳ／ＢＡ／ＮＭＡ共聚物，控制ＰＨＭＳ、ＮＭＡ、引发剂等用量可制得粒度和粘度适中，具有较高转化率的稳定ＰＨＭＳ／ＢＡ／ＮＭＡ复合聚合物乳液，该乳液所制得的胶膜具有优良的性能     

在邻菲罗啉类试剂存在下银与卟啉显色反应的研究

本文研究了三种邻菲罗啉类试剂对银（Ⅰ）与六种不同取代基卟啉试剂显色反应的影响。研究结果表明：于ｐＨ９．２时在３５～４０℃放置１０～１５ｍｉｎ，银与邻菲罗啉类试剂和卟啉试剂能形成多元络合物。我们分别测定了Ａｇ－ｐｈｅｎ－ＴＰＰＳ４、Ａｇ－ｐｈｅｎ－Ｔ（４－ＭＯＰ）ＰＳ４和Ａｇ－ｐｈｅｎ－Ｔ（４－ＨＰ）ＰＳ４体系的络合比及稳定常数，详细讨论了Ａｇ－ｐｈｅｎ－Ｔ（４－ＭＯＰ）ＰＳ４体系的光度性质，把所确     

晶性3，4－聚异戊二烯的结构研究

采用ＷＡＸＤ、ＳＡＸＳ和Ｘ－射线平板照相法研究了不同聚合条件和拉伸倍数下的晶性３，４－聚异戊二烯的结构．结果发现，降低催化体系反应速度有利于产物结晶；不同的含氮类给电子试剂对聚合物的结晶结构影响较大．取向样品随着拉伸倍数的增加结晶度和长周期增大，微晶尺寸变小．ＳＡＸＳ的散射强度计算表明，该聚合物属多分散非均一粒子体系，微孔半径在３．５－１６．４ｎｍ间．     

混合物和溶液的组成标度和组成变量

组成标度按５类逐一给出了名称，符号，定义和ＳＩ单位，并指出了一些常见的错误，按混合物和溶液讨论了组成变量的选择。量纳一的量的ＳＩ单位１的字母符号问题也作了讨论。     

晶性3，4－聚异戊二烯的结构研究

采用ＷＡＸＤ、ＳＡＸＳ和Ｘ－射线平板照相法研究了不同聚合条件和拉伸倍数下的晶性３，４－聚异戊二烯的结构，结果发现，降低催化体系反应速度有利于产物结晶；不同的含氮类给电子试剂对聚合物的结是昌结构影响较大，取向样品随着拉伸倍数的增加结晶度和长周期增大，微晶尺寸变小，ＳＡＸＳ的散射哟度计算表明，该聚合物属多分散非均一粒子体系，微孔半径在３．５－１６．４ｎｍ间。     

类立方烷型簇合物[Bu4N]3[WAg3S4I4]的固相合成和晶体结构

由（ＮＨ４）２ＷＳ４，ＡｇＩ和Ｂｕ４ＮＢｒ用低热温固相反应合成了类立方烷簇合物＜Ｂｕ４Ｎ＞３．＜ＷＡｇ３Ｓ４Ｉ４＞。用Ｘ射线单晶衍射法测定其晶体结构。     

Simple methods for characterization of metals in historical textile threads

Characterization of metal threads on historical textile materials is important for preservation of valuable cultural heritage. Obtained results dictate decisions on cleaning, conservation and restoration steps. The most important part of characterization is chemical analysis of originally applied materials, since this enables understanding the nature of chemical and physical degradation and determines the cleaning methods. Methods applied should be non-destructive and sensitive enough to detect trace elements in small sample amounts. The goal of this research was to describe the most useful procedures for fast and simple determination of specific metals of interest. Therefore we propose application of scanning electron microscopy equipped with EDS detector (SEM-EDS) for sample surface analysis and inductively coupled plasma-optical emission spectroscopy (ICP-OES) for chemical analysis of metals threads. For quality insurance reasons, a comparative method applied for chemical analysis was atomic absorption spectrometry (AAS). This combination of methods has proven to be very useful in analysis of historical samples, since SEM-EDS was a simple and non-destructive method which provided information on chemical composition of sample surfaces, while ICP-OES and AAS enabled the full insight into the average chemical composition of samples. Nevertheless, both ICP-OES and AAS were destructive methods which demanded dissolving of samples prior to the analysis. In this work nine different metal fibers collected from historical textile materials were characterized. Proposed methods enabled obtaining information on sample constitution, morphology, topology and chemical composition.     

Atomic absorption spectroscopic, conductometric and colorimetric methods for determination of some fluoroquinolone antibacterials using ammonium reineckate

Three accurate, rapid and simple atomic absorption spectrometric (AAS), conductometric and colorimetric methods were developed for the determination of gatifloxacin (GTF), moxifloxacin (MXF) and sparfloxacin (SPF). The proposed methods depend upon the reaction of ammonium reineckate with the studied drugs to form stable precipitate of ion-pair complexes, which was dissolved in acetone. The pink coloured complexes were determined either by AAS or colorimetrically at lambda(max) 525 nm directly using the dissolved complex. Using conductometric titration, the studied drugs could be evaluated in 50% (v/v) acetone. The optimizations of various experimental conditions were described. Optimum concentration ranges for the determination of GTF, MXF and SPF were 5.0-150, 40-440 microg mL(-1) and 0.10-1.5 mg mL(-1) using atomic absorption (AAS), conductometric and colorimetric methods, respectively. Detection and quantification limits are ranges from 1.5 to 2.3 microg mL(-1) using AAS method or 30-45 microg mL(-1) using colorimetric method. The proposed procedures have been applied successfully to the analysis of these drugs in pharmaceutical formulations and the results are favourably comparable to the reference methods.     

Matrix sensitivity of solid sampling AAS. Determination of zinc in geological samples

Direct solid sampling techniques in AAS have several advantages over wet digestion methods such as small sample size requirements and simple calibration procedures. But some disadvantages also exist such as the sample in homogeneity and the matrix sensitivity of calibration. The calibration is commonly carried out by varying the sample mass and evaluating the peak intensity versus absolute analyte amount. It is shown here that this procedure must be considered doubtful when matrix effects are expected. In the case of zinc determination in geological samples it has been shown that calibration functions obtained by different reference materials differ significantly from each other. As an alternative a three-dimensional calibration technique can be applied that evaluates the peak intensity versus both analyte content and sample weight. The resulting calibration planes are expected to be hyperbolically curved. This three-dimensional calibration has been applied to the determination of Zn in geological samples and compared with classical solid sampling AAS calibration procedures.     

Atomic absorption spectrometric determination of mercury in soil standard reference material following microwave sample pretreatment

Several decomposition procedures and their influence on the determination of mercury by electrothermal (ET) and cold vapour (CV) atomic absorption spectrometry (AAS) have been studied. Soil samples were decomposed by microwave digestion in closed and open vessels as well as by digestion under reflux according to German standard. The use of different acids (HNO₃, HCl or aqua regia) was evaluated and compared in respect to their influence on the determination of mercury by ET AAS and CV AAS. The digestion solutions were analyzed by ET AAS with a palladium modifier and by CV AAS using SnCl₂ or NaBH₄, as reducing agents. The detection limits obtained with different procedures were also evaluated. For the soil containing 6.25 g/g of Hg the ET AAS measurements were possible. In the case of lower concentration of mercury the CV AAS determination following the microwave digestion procedure with HCl or aqua regia is recommended. The accuracy of the proposed procedure was confirmed by the determination of total mercury in SRM 2711 Montana Soil.On leave from: Institut für Analytische Chemie, Technische Universitat Wien, Getreidemarkt 9, A-1060 Wien, Austria     

一种水溶性涂料的化学成分分析

采用傅里叶变换红外光谱、电镜/X射线能谱和原子吸收光谱等现代仪器测试方法对一种水溶性涂料的化学成分进行检测分析,对材料的红外光谱特征进行解析,综合定性和定量分析结果,确定出该涂料的各种组份及其配比.     

A targeted mass spectrometry-based approach for the identification and characterization of proteins containing α-aminoadipic and γ-glutamic semialdehyde residues

The site-specific identification of α-aminoadipic semialdehyde (AAS) and γ-glutamic semialdehyde (GGS) residues in proteins is reported. Semialdehydic protein modifications result from the metal-catalyzed oxidation of Lys or Arg and Pro residues, respectively. Most of the analytical methods for the analysis of protein carbonylation measure change to the global level of carbonylation and fail to provide details regarding protein identity, site, and chemical nature of the carbonylation. In this work, we used a targeted approach, which combines chemical labeling, enrichment, and tandem mass spectrometric analysis, for the site-specific identification of AAS and GGS sites in proteins. The approach is applied to in vitro oxidized glyceraldehyde-3-phosphate dehydrogenase (GAPDH) and an untreated biological sample, namely cardiac mitochondrial proteins. The analysis of GAPDH resulted in the site-specific identification of two AAA and four GGS residues. Computational evaluation of the identified AAS and GGS sites in GAPDH indicated that these sites are located in flexible regions, show high solvent accessibility values, and are in proximity with possible metal ion binding sites. The targeted proteomic analysis of semialdehydic modifications in cardiac mitochondria yielded nine AAS modification sites which were unambiguously assigned to distinct lysine residues in the following proteins: ATP/ATP translocase isoforms 1 and 2, ubiquinol cytochrome-c reductase core protein 2, and ATP synthase α-subunit.     

Untersuchungen zur atomspektroskopischen spurenanalyse in AIIIBV-halbleiter-mikroproben—III: Untersuchungen zur schichtabtrennung und zur spurenanalyse in dünnen GaAs schichten

Three methods for stripping thin layers of GaAs have been compared with regard to depth of layer and reproducibility. They are (1) chemical etching with methanolic bromine solution, (2) mechanical separation with a microtome, (3) chemical etching after a preliminary amperostatic anodic oxidation. Conditions were optimized. The depth of strip was 0.4 μm for chemical etching, 1 μm for the mechanical separation and 0.02 μm for the anodic oxidation method. Thus the anodic oxidation is specially suitable for profile analysis, and the mechanical method for investigation of thicker layers; chemical etching lies between them. The trace elements in the micro samples thus obtained were determined by d.c. are atomic-emission spectrography (AES) and atomic-absorption spectrometry with electrothermal atomization in a graphite tube (AAS). The absolute and relative detection limits of AAS for the 0.1–0.2 mg micro samples were on average better by an order of magnitude than those of AES. The advantage of AES lies in the possibility of simultaneous determination of several elements. in der Möglichkeit der Simultanbestimmung mehrerer Elemente.     

Systematic investigations of the multi-element preconcentration from copper by precipitation of the matrix as copper(I) oxide and copper(I) thiocyanate

Two methods for multi-element preconcentration from copper by reductive matrix precipitation are presented. In systematic investigations on the coprecipitation behaviour of Ag, Al, Au, Bi, Cd, Co, Cr, Fe, Ga, In, Mn, Mo, NJ, Pb, Sb, Se, Sn, Te and Zn during precipitation of the copper matrix as Cu₂O or CuSCN, the separation parameters were optimized. By combination with a hexamethyleneammonium hexamethylenedithiocarbamate collector precipitation, a concentration of 8 elements (Cu₂O precipitation) or 13 elements (CuSCN precipitation) in a small volume was achieved. The limits of detection of the procedures are, depending on the element, 0.1–5 μg g^?1 for flame atomic absorption spectrometry (AAS) and 0.01–0.1 μg g^?1 for graphite furnace AAS. The relative standard deviations are about 3%. The analytical performance of the procedures is compared with that of an electrolytic copper separation.     

Feasibility study for the preparation of a tuna fish candidate reference material for total As determination

This work describes the evaluation of several parameters for the preparation of a tuna fish candidate as a reference material (RM) in order to measure the total As mass fraction by slurry sampling graphite furnace atomic absorption spectrometry (SLS-GF AAS) and slurry sampling hydride generation atomic absorption spectrometry (SLS-HG AAS). The main parameters investigated were the homogeneity, analyte segregation and composition during material production. For candidate RM preparation, tuna fish was collected at a local market, cleaned, freeze-dried and treated using different procedures as follows: (1) ground in a cutting mill and separated in different particle sizes (2) ground in cryogenic mill. The mass fraction of As in the cryogenically ground sample was (4.77?±?0.19)?μg?g^?? for SLS-GF AAS and (4.61?±?0.34)?μg?g^?? for SLS-HG AAS. The accuracy of the procedures was checked with tuna fish certified reference material (BCR 627) with recoveries of 102 and 94% for SLS-GF AAS and SLS-HG AAS, respectively. The homogeneity factor was calculated for different pretreatment procedures and for particle sizes in the range of 500??50?μg, indicating good homogeneity, except for raw fish. There was no observed analyte segregation and no losses, no contamination and no changes in the microdistribution of material during preparation.     

Analysis of eco-relevant elements and noble metals in printed wiring boards using AAS,ICP–AES and EDXRF

Different analytical procedures were developed to investigate the chemical composition of printed wiring boards. A set of 11 samples from different electronic devices were ground and prepared for ICP-AES and AAS analyses by extraction with aqua regia and microwave digestion. Several sample preparation techniques were used for the analyses by EDXRF; the best results were obtained by embedding the samples in Vaseline. Since no standard reference material is available for printed wiring boards, a model reference material was created to compare the applicability and limitations of the employed analytical techniques.