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61.
Summary A reversed phase liquid chromatographic method is proposed for the analysis of basic hair dyes (raw materials and colourant formulations). The performance of the method was enhanced by introducing post-column on-line photochemical derivatisation in combination with a Diode Array Detector. On-line photoderivatisation provided an effective way of selectively transforming the analytes to compounds with different spectral properties. For each analyte two characteristic UV-Visible spectra (photoreactor on and off) were obtained with the same mobile phase and this information in combination with the chromatographic data (k' at pH 3.0 and 4.5) enabled the unambiguous identification of both commonly used, approved, and banned basic hair dyes. Additionally, this approach was found useful to improve the method sensitivity, allowing the determination of analytes present in low concentration (0.03%) in complex commercial formulations.This work constitutes part of the thesis for the Dottorato di Ricerche of Roberto Gotti. 相似文献
62.
Hartmut Hibst 《Angewandte Chemie (International ed. in English)》1982,21(4):270-282
Owing to their particular crystallographic properties, ferrimagnetic hexagonal ferrites exhibit a far greater coercive force than the conventional magnetic pigments. They therefore appear to be suitable for use in magnetic information storage procedures, some of which are novel and are at the development stage. Thus, magnetic tapes of high coercive force containing barium ferrite could be used as master tapes for copying magnetic information or for producing forgery-proof magnetic cards, if magnetic heads having high-order write fields were successfully developed. Moreover, platelet-like ferrite pigments in which the preferred direction of magnetic orientation is perpendicular to the plane of the platelet are of great interest for perpendicular magnetic recording. In this progress report, the crystal structures, magnetic characteristics of hexagonal ferrites, and chemical processes for their production are discussed. In particular, reactions in salt melts or under hydrothermal conditions produce finely divided pigments whose particles have a pronounced hexagonal, plate-like habit, a narrow particle size distribution, and advantageous magnetic properties. The magnetic properties of the pigments crystallized from salt melts may be adjusted by cation exchange. 相似文献
63.
Kizek R Masarik M Kramer KJ Potesil D Bailey M Howard JA Klejdus B Mikelova R Adam V Trnkova L Jelen F 《Analytical and bioanalytical chemistry》2005,381(6):1167-1178
The electroanalytical determination of avidin in solution, in a carbon paste, and in a transgenic maize extract was performed in acidic medium at a carbon paste electrode (CPE). The oxidative voltammetric signal resulting from the presence of tyrosine and tryptophan in avidin was observed using square-wave voltammetry. The process could be used to determine avidin concentrations up to 3 fM (100 amol in 3 l drop) in solution, 700 fM (174 fmol in 250 l solution) in an avidin-modified electrode, and 174 nM in a maize seed extract. In the case of the avidin-modified CPE, several parameters were studied in order to optimize the measurements, such as electrode accumulation time, composition of the avidin-modified CPE, and the elution time of avidin. In addition, the avidin-modified electrode was used to detect biotin in solution (the detection limit was 7.6 pmol in a 6 l drop) and to detect biotin in a pharmaceutical drug after various solvent extraction procedures. Comparable studies for the detection of biotin were developed using HPLC with diode array detection (HPLC-DAD) and flow injection analysis with electrochemical detection, which allowed biotin to be detected at levels as low as 614 pM and 6.6 nM, respectively. The effects of applied potential, acetonitrile content, and flow rate of the mobile phase on the FIA-ED signal were also studied. 相似文献
64.
组合电化学是一种新的电化学研究策略,通过设计和构建大量多样性的电极阵列,并对其进行高通量筛选和表征,快速、高效地实现了体系的电化学研究。本文综述了近年来进行的组合电化学研究,重点介绍了组合光学筛选方法、组合电化学合成方法以及电化学平行筛选方法,并探讨了各种方法的优势和存在的问题。 相似文献
65.
Stefan G Ebbinghaus 《Journal of solid state chemistry》2004,177(3):817-823
Single crystals of the new compound La1.2Sr2.4RuO7, an oxide related to the hexagonal perovskites, were grown from a BaCl2 flux. The structure was solved by single crystal X-ray diffraction. La1.2Sr2.4RuO7 crystallizes in the space group with a=5.760(1) Å and c=18.273(3) Å. It is one of the rare examples of oxides with isolated RuO6-octahedra. The structure consists of alternating layers of RuO6-octahedra and trigonal (La,Sr)O6-prisms. These prisms are capped by one additional oxygen ion, which occupies a distorted position within the (La,Sr)O6-layers. La1.2Sr2.4RuO7 is the second member of the general [A2O][AnBn−1O3n] family of hexagonal perovskites with n=2 and the first ruthenate possessing this structure. XANES investigations, bond valence sum calculations and magnetic measurements show that ruthenium takes the oxidation state +5. Although the ruthenium ions have quite long distances, a medium strong antiferromagnetic interaction between these paramagnetic centers was observed. 相似文献
66.
Summary The paper describes tests for liquid chromatographs to assess the autosampler and pump flow rate precision; suitability of
the instrument for normal phase chromatography; UV detector performance; and external band broadening characteristics. Tests
for mixing and proportioning characteristics of solvent pumps and performance of diode array detectors are also considered.
These tests are designed to evaluate the performance of both newly released liquid chromatography equipment and equipment
already in operation. Data from evaluations carried out by instrument manufacturer’s and suppliers is reported and discussed.
This data offers specifications to a common format for initial selection of instruments prior to purchase. 相似文献
67.
Sylvie Malo Antoine Maignan Sylvain Marinel Maryvonne Hervieu Kenneth R. Poeppelmeier Bernard Raveau 《Solid State Sciences》2005,7(12):1492
Recently, the ferroelectromagnet YMnO3 has been the focus of interest because it exhibits both antiferromagnetism (Néel temperature 80 K) and ferroelectricity (Curie temperature 914 K). There have been no reports of complete YMn1−xMxO3 solid solutions in which substitution of the foreign M cation preserves the hexagonal P63cm structure. In contrast there exist several homeotypic phases with the general formula, Ln1+nCunMO3+3n (n=1 (M=Ti), 2 (M=V) and 3 (M=Mo); Ln: lanthanide). Several YMn1−x(Cu3/4Mo1/4)xO3 compounds have been synthesized. The solid solution, from YMnO3 (x=0) to YCu3/4Mo1/4O3 (x=1) has been characterized by X-ray diffraction and transmission electron microscopy study. For 0<x<0.9, the compounds are found to crystallize in the non-centrosymmetric structure, space group P63cm, of YMnO3. The Mn-free end member, x=1, crystallizes in a complex multiple cell, the superstructure being associated to Cu3+/Mo6+ cationic ordering. Dilution of the Mn3+ magnetic array by the paramagnetic (Cu2+) and diamagnetic (Mo6+) cations is found to decrease the antiferromagnetic ordering temperature and it becomes undetectable for x0.5 compositions. 相似文献
68.
以氨水和硝酸锌为前躯体,采用低温水溶液法在涂敷ZnO晶种层的玻璃衬底上外延生长了ZnO纳米棒晶阵列。应用SEM、TEM、SAED和XRD表征了ZnO纳米晶的形貌和结构。讨论了该组成体系水溶液法纳米棒外延生长的机理及其对棒晶形貌的影响。通过对水溶液pH值的原位二次调整,制备出了ZnO纳米管和表面绒毛状的棒晶阵列,基于生长机理探讨了它们的形成原因,为实现不同形貌ZnO纳米晶阵列的优化控制提供了可能的技术途径。结果表明,不同形貌的ZnO均属沿c轴择优取向的六方纤锌矿结构。 相似文献
69.
《Electroanalysis》2006,18(6):573-578
The electroanalytical detection of trace mercury(II) at gold ultra‐microelectrode arrays is reported. The arrays consist of 256 gold microelectrodes of 5 μm in diameter in cubic arrangements which are separated from their nearest neighbor by 100 μm. The array was utilized in nitric acid using linear sweep voltammetry where a linear response from mercury additions over the range 10 μg L?1?200 μg L?1 (10?8?10?6 M) was observed with a sensitivity and detection limit of 0.11 nC/μg L?1 and 3.2 μg L?1 (16 nM) respectively from using a deposition time of 30 s at ?0.2 V (vs. SCE). This methodology was explored in 0.1 and 1 M chloride media over the mercury range 10 μg L?1?200 μg L?1 (5×10?8?10?6 M) where similar sensitivities of 0.087 nC/μg L?1 and 0.078 nC/μg L?1 were observed with an identical detection limit. The protocol is demonstrated to be useful for the determination of mercury for analysis of environmental water samples. 相似文献
70.
Simplified Solid-Phase Extraction Procedure and Liquid Chromatographic Determination of Celecoxib in Rat Serum 总被引:1,自引:0,他引:1
A simplified solid phase extraction method, eliminating a preliminary protein precipitation has been developed for the determination of celecoxib in rat plasma. The technique included a solid phase extraction of the serum samples on a [poly (divinylbenzene-co-N-vinylpyrrolidone)] sorbent. After conditioning, the cartridge was loaded with 0.5 mL of acidified serum containing internal standard. Elution was made with 1 mL of a mixture of acetonitrile and methanol (1/1, v/v). After evaporation of the eluate to dryness and reconstitution with methanol, the samples were analyzed on an octadecyl bonded phase with several mobile phases containing acetonitrile and a phosphate buffer. Detection was carried out using a Photodiode Array Detector. Full validation of the proposed method was provided (linearity range: 0.01–2 mg. L–1, average extraction efficiency: 92.4%; average intra-day variability: 4.6% with an accuracy of 94.8%; average interday variability: 5% with an accuracy of 95.3%, limit of detection: 0.005 mg. L–1, limit of quantification: 0.002 mg. L–1). The proposed method was successfully utilised to quantify celecoxib in rat plasma for a pharmacokinetic study.Revised: 26 January and 23 April 2004 相似文献