寡糖—8—氨基芘—1,3,6—三磺酸衍生物的毛细管电泳—激光诱？…

利用自组装的毛细管电泳－激光诱导荧光装置,研究了多种寡糖－８－氨基芘－１,３,６－三磺酸（寡糖ＡＰＴＳ）衍生物的分离。考察了电泳介质、浓度及pＨ对寡糖－ＡＰＴＳ 衍生物分离的影响,在酸性和碱性条件下,分别实现了痕量寡糖标准品及葡聚糖水解产物的高效分离。     

锑(Ⅲ)-向红菲咯啉络合吸附波及其应用

在 ０．０２ ｍｏｌ／Ｌ酒石酸（Ｃ４Ｈ６Ｏ６）－０．００３％溴化十六烷基三甲基铵（ＣＴＭＡＢ）介质中，研究了锑（Ⅲ）－向红菲咯啉（ＢＰＴ）的极谱行为。Ｓｂ（Ⅲ）－ＢＰＴ络合物在滴汞电极上于－０．５８ ｖ（ｖｓ．ＳＣＥ）得到一良好的吸附还原波，其二阶导数值与锑（Ⅲ）浓度在１×１０－８～７×１０－６ｍｏｌ／Ｌ范围内呈线性关系，检测下限可达８Ｘ１０－９ｍｏｌ／Ｌ。应用该法测定纯锡及铜合金中微量锑，结果较好。对电极反应机理进行了探讨。     

Ln（ClO4）3—DAPTU—H2O三元体系30℃时的相平衡研究

测定了Ｌｎ（ＣｌＯ４）３－ＤＡＰＴＵ－Ｈ２Ｏ（Ｌｎ＝Ｌｎ，Ｓｍ，Ｙｂ）三元体系在３０℃时的溶解度及饱和溶液的折光率，绘制了相应的溶度图和折光率－组成图。各体系的溶度曲线和折光率曲线均由三支组成，分别与ＤＡＰＴＵ、Ｌｎ（ＤＡＰＴＵ）２（ＣｌＯ４）３·８Ｈ２Ｏ（Ｌｎ＝Ｌａ，Ｓｍ，Ｙｂ）和Ｌｎ（ＣｌＯ４）３·ｎＨ２Ｏ（Ｌｎ＝Ｌａ，ｎ＝８；Ｓｍ，ｎ＝９；Ｙｂ，ｎ＝８）相对应。从溶度图上发现了３个未见文献报     

1-(4-磺酸基苯基)-3-[4-(苯基偶氮)苯基]-三氮烯与季铵盐型阳离子表面活性剂的显色反应及应用

合成了１－（４－磺酸基苯基）－３－［４－（苯基偶氮）苯基］－三氮烯（ＳＰＡＰＴ）,研究了该试剂在强碱性介质中与季铵盐型阳离子表面活性剂溴化十六烷基吡啶（ＣＰＢ）和溴化十六烷基三甲铵（ＣＴＭＡＢ）的显色反应体系,试剂与表面活性剂形成１∶３的紫红色离子缔合物,其表观摩尔吸光系数分别为１．６７×１０４和１．０６×１０４Ｌ·ｍｏｌ－１·ｃｍ－１。测定了显色体系中ＣＰＢ和ＣＴＭＡＢ的临界胶束浓度（ＣＭＣ）,证明在比尔定律范围内,ＣＰＢ和ＣＴＭＡＢ均以单分子缔合显色。确定了显色体系最佳实验条件     

乙烯系自由基聚合阻聚效应（ⅩⅧ）：哌啶氮氧自由基氨基硫…

本文研究了３种１－（芳酰基）－４［４＇－（２，２，６，６－四甲基哌啶）－１－氧自由基］氨基硫脲化合物（ＡＴＳＣＰＯ）分别同通用阻聚剂（ＣＩＨ），如对苯二酚（ＨＱ），苯醌（ＢＱ），吩噻嗪（ＰＴ）及二乙羟胺（ＤＥＨＡ）组成的混合阻聚剂对ＡＩＢＮ引发的ＭＭＡ自由基聚合的影响，研究结果表明：当［ＡＴＳＣＰＰ］／ＣＩＨ＝５：１时，除ＡＴＳＣＰＯ－ＢＱ外，其余阻聚效果均较ＡＴＳＣＰＯ和ＣＩＨ单独用作阻聚剂时高     

Ln（ClO_4）_3－DAPTU－H_2O三元体系30℃时的相平衡研究

测定了Ｌｎ（ＣｌＯ_４）_３－ＤＡＰＴＵ－Ｈ_２Ｏ（Ｌｎ＝Ｌａ，Ｓｍ，Ｙｂ）三元体系在３０℃时的溶解度及饱和溶液的折光率，绘制了相应的溶度图和折光率－组成图，各体系的溶度曲线和折光率曲线均由三支组成，分别与ＤＡＰＴＵ、Ｌｎ（ＤＡＰＴＵ）_２（ＣｌＯ_４）_３·８Ｈ_２Ｏ（Ｌｎ＝Ｌａ，Ｓｍ，Ｙｂ）和Ｌｎ（ＣｌＯ_４）_３·ｎＨ_２Ｏ（Ｌｎ＝Ｌａ，ｎ＝８；Ｓｍ，ｎ＝９；Ｙｂ，ｎ＝８）相对应。从溶度图上发现了３个未见文献报道的固液异组成溶解的化合物，通过化学分析及元素分析、ＴＧ－ＤＴＧ、ＩＲ对其进行了表征。     

1—（2—羟基—3,5—二硝基苯基）—3—[4—（苯基偶氮）苯基]—三氮烯—阴离子表面活性

在三乙醇胺介质中,新试剂１－（２－羟基－３,５－二硝基苯基）－３－「４－（苯基偶氮）苯基」－三氮烯（ＨＤＮＰＡＰＴ）与季铵盐型阳离子表面活性剂及阴离子表面活性剂（ＡＳ）反应显色,形成三元（ＤＢＯＳＯ３Ｎａ）,十二烷基磺酸钠（ＤＯＳＯ３Ｎａ）和十二烷基硫酸钠（ＤＳＯ４Ｎａ）的方法,表观摩尔吸光系数均达１０＾４以上。方法已应用于环境水样中阴离子表面活性剂的测定。     

C60／TiO2杂化材料的合成与表征

本论文采用３－氨内基三氧基硅烷（ＡＰＴＥＳ）作偶联剂，通过单电子转移过程使用ＡＰＴＥＳ的氨基与Ｃ６０反应，再通过ＡＰＴＥＳ的三乙氧基硅基团与钛酸正丁酯一起水解缩合，成功地将Ｃ６０引入ＴｉＯ２网络，制得均匀透明的棕黄色直径为２０ｍｍ的整志固体。证明了Ｃ６０同ＴｉＯ２网络间是以共价键结合的；并用紫外－可见光光谱研究了杂化材料的透明度。     

OPTICALLY ACTIVE AMINO ACIDS WITH HIGHLY BRANCHED SIDE CHAIN（Ⅱ）：SYNTHESIS AND RESOLUTION OF RACEMIC 2－ACETAMIDO－7，7－DIMETHYLOCTANOIC ACID AND 2－ACETAMIDO－8，8－DIMETHYLNONANOIC ACID ETHYL ESTERS

ＯＰＴＩＣＡＬＬＹＡＣＴＩＶＥＡＭＩＮＯＡＣＩＤＳＷＩＴＨＨＩＧＨＬＹＢＲＡＮＣＨＥＤＳＩＤＥＣＨＡＩＮ（Ⅱ）：ＳＹＮＴＨＥＳＩＳＡＮＤＲＥＳＯＬＵＴＩＯＮＯＦＲＡＣＥＭＩＣ２－ＡＣＥＴＡＭＩＤＯ－７，７－ＤＩＭＥＴＨＹＬＯＣＴＡＮＯＩＣＡＣＩＤＡＮ...     

TWO NEW C_(19)-DITERPENE ALKALOIDS FROM DELPHINIUM SWINANENSE VAR LEPTOPOGON

ＴＷＯ　ＮＥＷ　Ｃ＿（１９）－ＤＩＴＥＲＰＥＮＥ　ＡＬＫＡＬＯＩＤＳ　ＦＲＯＭ　ＤＥＬＰＨＩＮＩＵＭ　ＳＷＩＮＡＮＥＮＳＥ　ＶＡＲ　ＬＥＰＴＯＰＯＧＯＮＴＷＯＮＥＷＣ＿（１９）－ＤＩＴＥＲＰＥＮＥＡＬＫＡＬＯＩＤＳＦＲＯＭＤＥＬＰＨＩＮＩＵＭＳＷＩＮ...     

Laser-based refractive index detection for micro-channels

Laser-based refractive index detection, based upon refractive index changes in micro-channels, is a kind of laser-based optical determination for solutions. As it is capable of label-free determination, it has been regarded as a considerable growth prospect. The key aspect in related researches lay in the development of novel detection configurations, which would possibly result in better sensitivity. Over the past decade, micro-channel laser-based refractive index detection has been significantly improved, resulting in traversed, hologram-based, back-scattered, retro-reflected interference, optical ring resonant, etc., detection configurations. Moreover, laser-based refractive index detection has been combined with other laser-based detection strategies, in order to pursue a universal and sensitive detection. And last but not least, some utilizations of laser-based refractive index detection have been reported, while both advantages and drawbacks exist. In this paper, laser-based refractive index detection for micro-channels will be reviewed in proceeding sequence.     

Element-selective atomic emission detection for capillary GC of metal-containing compounds

Element-selective GC detection by microwave-induced plasma atomic emission spectroscopy has been used to examine a wide variety of compounds containing metals, non-metals, and metalloids. “Recipes”, or new selective detection schemes for use with the software of the computer-controlled system, have been developed for the selective detection of boron, aluminum, gallium, titanium, vanadium, chromium, manganese, rhenium, palladium, and platinum. Figures of merit including limits of detection, linear dynamic range, and spectral selectivity over carbon have been established for most of these elements. Gas chromatography – atomic emission detection (GC-AED) has been applied to the selective detection of vanadium, nickel, and iron in metalloporphyrins present in crude oil, manganese-selective detection of methylcyclopentadienylmanganese tricarbonyl (MMT) in gasoline, and titanium-selective detection of reaction mixtures containing titanium catalysts or titanium boride molecular precursors.     

实时直接分析质谱在农药检测中的应用

实时直接分析(Direct analysis in real time,DART)作为一种原位电离技术发展迅猛,其与质谱联用已成为热门的分析技术并广泛应用于法庭科学领域,如食品安全、爆炸物检测、毒物毒品分析和药物分析等方面。目前农药的常规检测方法已非常成熟,但引入原位电离-质谱联用技术可以拓宽检测范围,缩短检测时限。该文从实时直接分析质谱(DART-MS)技术的工作原理、检测条件优化及其在农药检测方面的应用进行综述,并对DART-MS的应用前景进行了展望。     

Simultaneous LIF and retro-reflected beam interference detection for CE

This Short Communication describes a novel optical detection method for CE, based on the combination of LIF detection and retro-reflected beam interference detection. By the use of a side-illuminated laser beam, an on-column multifunctional detection for CE has been developed, and some key elements in the scheme have been optimized. In addition, two miscellaneous samples including fluorescent dyes, carbohydrates and amino acids have been determined to evaluate its performance. Without any additional pretreatment, sufficient LOD and linear ranges have been achieved for most analytes. Its performance in retro-reflected beam interference detection is better than those mentioned in a former report, and its fluorescent sensitivity is comparable with the achievable sensitivity by conventional LIF systems, all of which together combine high sensitivity and universal analysis to a certain extent.     

A systematic scheme of qualitative analysis for anions.IV

A comprehensive investigation has been undertaken to ascertain how the basic radicals that pass into the sodium carbonate filtrate arc distributed among the various groups for the detection of anions. Methods for the detection of these basic radicals in the presence of the anions have been worked out in detail. It was found that the scheme for the detection of anions put forward previously remains unaffected by the presence of these basic radicals. It has been shown that the scheme for the detection of anions can be integrated with the comprehensive schemes for the detection of basic radicals and insoluble substances.     

Conductivity detection for conventional and miniaturised capillary electrophoresis systems

Since the introduction of capillary electrophoresis (CE), conductivity detection has been an attractive means of detection. No additional chemical properties are required for detection, and no loss in sensitivity is expected when miniaturising the detector to scale with narrow-bore capillaries or even to the microchip format. Integration of conductivity and CE, however, involves a challenging combination of engineering issues. In conductivity detection the resistance of the solution is most frequently measured in an alternating current (AC) circuit. The influence of capacitors both in series and in parallel with the solution resistance should be minimised during conductivity measurements. For contact conductivity measurements, the positioning and alignment of the detection electrodes is crucial. A contact conductivity detector for CE has been commercially available, but was withdrawn from the market. Microfabrication technology enables integration and precise alignment of electrodes, resulting in the popularity of conductivity detection in microfluidic devices. In contactless conductivity detection, the alignment of the electrodes with respect to the capillary is less crucial. Contactless conductivity detection (CCD) was introduced in capillary CE, and similar electronics have been applied for CCD using planar electrodes in microfluidic devices. A contactless conductivity detector for capillaries has been commercialised recently. In this review, different approaches towards conductivity detection in capillaries and chip-based CE are discussed. In contrast to previous reviews, the focus of the present review is on the technological developments and challenges in conductivity detection in CE.     

Sensitive determination of aliphatic amines in water by high-performance liquid chromatography with chemiluminescence detection

A sensitive method has been developed for liquid chromatographic determination of short aliphatic amines in water samples. Analytes are preconcentrated and dansylated on solid sorbents (C18 solid-phase extraction cartridges). The dansyl derivatives are chromatographed and post-column mixed with peroxyoxalate (TCPO) and H2O2 in order to perform chemiluminescence detection. Optimal results have been obtained using a sample volume of 5 ml. The method has been applied to the quantification or screening of several aliphatic amines: methylamine, ethylamine, butylamine, diethylamine, pentylamine and hexylamine. The screening procedure has been developed including also polyamines (putrescine, cadaverine, spermidine and spermine). The results obtained by using chemiluminescence (CL) detection have been compared with other detection systems (fluorescence and UV). The sensitivity can increase from 3 to 75 times respect UV detection and from 2 to 10 times respect fluorescence detection depending on the amine. The detection limits achieved were between 0.15 and 0.9 microg/l.     

Sample preparation for evaluation of detection limits in X-ray fluorescence spectrometry.

The influence of analyte mass concentration on determination of detection limits in X-ray fluorescence spectrometry has been investigated experimentally. Both the total reflection X-ray fluorescence (TXRF) and the conventional energy-dispersive X-ray fluorescence techniques have been used to derive the dependence of analyte mass concentration on the values of detection limits. Results obtained indicate that values of detection limits are optimum, or in other words, they are closer to the true detection limit of the technique, when analyte concentrations are in the range of 10 times of the detection limit.     

Surface-enhanced Raman spectrometry for detection in liquid chromatography using a windowless flow cell

A windowless flow cell has been developed for surface-enhanced Raman (SER) detection in liquid chromatography. Using colloidal silver as an active substrate, SER spectrometry of banned drugs in sport is presented. The experimental factors of primary influence on the analytical performance of the cell have been studied. The results of SER detection with the proposed cell have been compared to UV detection.     

Separation of non-UV-absorbing synthetic polyelectrolytes by CE with contactless conductivity detection

A specific method for the separation and detection of non-UV-absorbing polyelectrolytes has been developed. The analysis of such polyelectrolytes by liquid chromatography is nearly impossible due to strong ionic interactions and charge density effects. CE makes use of these charge density effects and thus enables for proper separation. A capacitively coupled contactless conductivity detector has been applied for the detection in CE. A low molar mass poly(acrylic acid) sodium salt standard (PAA1.3k) was separated in free solution CE and detected with the contactless conductivity detector. Different amphoteric electrolytes have been tested for their applicability as BGE for the separation of polyelectrolytes with conductivity detection. It has been shown that the best detection results are obtained with an arginine-sorbate buffer.