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91.
Mercury Compounds with Cyancarbanions. II Synthesis and Crystal Structure of Dimercury(I)-bis(1,1,3,3-tetracyanpropenide) The structure of dimercury(I)-bis(1,1,3,3-tetracyanpropenide), Hg2(tcp)2, has been determined by single-crystal X-ray diffraction methods. The crystals are monoclinic, space group P 21/n. The unit cell dimensions are: a = 9.9193(3) Å, b = 5.6912(6) Å, c = 13.3806(4), β = 92.544(4)° and Z = 2. The mercury atoms in the centrosymmetric cation are three-coordinate with Hg? Hg 2.503, Hg? N 2.207, 2.207, 2.560 Å. tcp behaves as a bidentate ligand forming infinite chains running parallel to the a-axis. 相似文献
92.
一种基于流动注射梯度技术识别异常峰及校正的方法 总被引:1,自引:0,他引:1
基于流动注射梯度信息提出了一种利用梯度比均值进行定量的校正方法。方法具有在线自动判别和修复异常峰并自行校正的功能,和通用的标准系列定量方法相比,两者测定精度相当。但本文提出的方法抗干扰能力明显优于后者,可适用于在线过程监测。 相似文献
93.
94.
在芳烃溶剂中用氯化二乙基铝和叠氮化钠反应合成了叠氮化二乙基铝(DEAA),其产率高达87%,比文献值高出17%。在正己烷中没有合成出DEAA,在含30%四氢呋喃(THF)的正己烷中合成出DEAA·THF配合物。在芳烃溶剂中,随着苯环上甲基数目的增加,DEAA的收率增加。测定了氯化二乙基铝、氯化二乙基铝的正己烷溶液、氯化二乙基铝的甲苯溶液的 27Al NMR谱。由 27Al NMR谱数 据确定了氯化二乙基铝在甲苯中解离平衡式,计算了氯化二乙基铝在甲苯中解离平衡的热力学数据。用DEAA与苯甲酸甲酯直接合成了苯甲酰叠氮,并表征了其结构。这是一个新反应,至今无文献报导。用实验证明了在正己烷溶液中,用氯化二乙基铝、叠氮化钠与苯甲酸甲酯合成苯甲酰叠氮,没有经过氯化二乙基铝和叠氮化钠反应生成中间体DEAA的这一步。依据实验事实建立了上述三种反应的反应机理。 相似文献
95.
Pinotti Laura M. Silva Rosineide G. Giordano Roberto C. Giordano Raquel L. C. 《Applied biochemistry and biotechnology》2002,98(1-9):679-686
This article reports studies concerning the production of penicillin G acylase (PGA) by Bacillus megaterium. This enzyme has industrial use in the hydrolysis of penicillin G to obtain 6-aminopenicillanic acid, an essential intermediate
for the production of semisynthetic β-lactam antibiotics. Although most microorganisms produce the enzyme intracellularly,
B. megaterium provides extracellular PGA. The enzyme production by microorganisms involves several steps, resulting in a many operational
variables to be studied. The study of the inoculum is an important step to be accomplished, before addressing other issues
such as culture optimization and downstream processing. In this study, using a standard inoculum as reference, several runs
were performed aiming at the definition of operational conditions in the PGA production. Cell concentration and PGA activity
in the production medium were measured after 24, 48, and 72 h of the beginning of the production phase. This study encompasses
the duration of the inoculum germination phase and the concentration of cells used to startup the germination. Based on these
results, PGA productivity during the production phase was maximized. The selected values for these variables were 1.5 × 107 spores/mL of germination medium, germination during 24 h, and 72 h for the production phase. 相似文献
96.
Andreas Manz Elisabeth Verpoorte Carlo S. Effenhauser Norbert Burggraf Daniel E. Raymond D. Jed Harrison H. Michael Widmer 《Journal of separation science》1993,16(7):433-436
Miniaturization of separation columns implies equally reduced vol- umes of injectors, detectors, and the connecting channels. Planar chip technology provides a powerful means for the fabrication of micron-sized structures such as channels. This is demonstrated by two examples. An optical absorbance detector chip exhibits the expected behavior of a 1 mm optical path length cell despite its volume of 1 nL. A capillary electrophoresis device allows integrated injections of 100 pL samples, efficiencies of 70,000 to 160,000 theoretical plates in 10 to 20 seconds, and external laser-induced fluorescence detection at any capillary length of choice between 5 and 50 mm. 相似文献
97.
Preparation and crystal structure of the La2Ni12P5 and isotypic ternary lanthanoid—Nickel phosphides
Yu. B. Kuz'ma V. S. Babizhet'sky S. I. Chykhrij S. V. Oryshchyn V. K. Pecharsky 《无机化学与普通化学杂志》1993,619(3):587-592
The new ternary phosphide La2Ni12P5 has been prepared by direct arc melting of the components as pure metals and red phosphorus. The crystal structure has been determined using X-ray single crystal diffraction data. The compound exhibits a new type of crystal structure, P21/m with lattice parameters a = 10.911(3), b = 3.696(2), c = 13.174(4) Å, β = 108.02(2)°, V = 505,2(6) Å3, Z = 2. Atomic parameters least squares refinement of 116 independent variables (anisotropic approximation for thermal vibrations) employed 1 284 independent Io(hkl); RF = 0.0278 and RW = 0.0287. The crystal structure is characterized by trigonal prismatic arrangement of phosphorus atoms stacking variant of infinite (with phosphorus centered) columns built by metal trigonal prisms ‖ [010]. Two or three such columns are connected through common edges (lanthanum atoms). The compounds RE2Ni12P5 (where RE = Ce, Pr, Nd and Eu) display the same with La2Ni12P5 crystal structure. Lattice parameters of these compounds have been refined using powder diffraction data. 相似文献
98.
Nb6.74Ta5.26S4 has been prepared by high temperature techniques. The crystal structure has been determined from single crystal X-ray diffraction data (R/Rw = 0.0588/0.0655). The compound crystallizes in the orthorhombic space group Pnma with unit cell dimensions a = 959.11 (26) pm, b = 336.37 (10) pm, and c = 3282.51 (74) pm. The orthorhombic cell contains four formula units. Its structure is similar to that of Nb-rich sulfides, rather than to that of Ta-rich sulfides. The metal coordinations are capped distorted cubic prisms and pentagonal prisms while the coordinations of sulfur are capped trigonal prisms. 相似文献
99.
Delenclos S. Kolinsky C. Longuemart S. Hadj Sahraoui A. Buisine J. M. 《Journal of Thermal Analysis and Calorimetry》2002,70(2):549-558
The photopyroelectric (PPE) method is proposed as a sensitive technique to study a binary mixture of liquid crystals in a
contact preparation. The photothermal signal is generated while scanning the contact preparation. The crystal-smectic A, smectic
A-nematic, and nematic-isotropic interphase boundaries are detected. The displacement of these boundaries due to the variation
of the temperature is monitored. The study of these displacements allows us to draw the complete temperature-concentration
phase diagram of a binary mixtures.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
100.
Hiroshi Iwase 《Analytica chimica acta》2002,463(1):21-29
Determination of small amounts of the fat-soluble species Vitamin A (VA) (2.5 μg/g) and β-carotene (9 μg/g) from emulsified nutritional supplements containing 50 kinds of co-existing compounds and a fat content between 2000 and 8000 times higher was performed by solid-phase extraction (SPE) and high-performance liquid chromatography (HPLC) with fluorescence detection set at ex. 350 nm and em. 480 nm, and visible detection at 450 nm using an Inertsil ODS 80A (5 μm) analytical column. Mobile phases of methanol-ethanol (50:50) and acetonitrile-ethanol (70:30) were used for the both vitamins. A Bond Elut C18 cartridge was chosen for SPE after comparison with eight other types of SPE cartridge. Retention time of VA and β-carotene was 7 and 8 min, respectively, giving a limit of detection of ca. 0.1 ng per injection at a signal-to-noise ratio 3:1. Recoveries of VA and β-carotene were over 90% by the standard addition method. Relative standard deviation of VA and β-carotene were ca. 2.9 (n=5) and 2.3% (n=5), respectively. 相似文献