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161.
A comparison is made between dichlorosilanes and cyclic siloxanes as starting materials in the synthesis of stationary phases for capillary gas chromatography (CGC) and supercritical fluid chromatography (SFC). Siloxanes containing one or more of the side groups methyl, vinyl, phenyl, and cyanoethyl in various ratios were synthesized and compared. These phases were characterized by chromatographic (gel permeation, GPC), spectroscopic (IR, 1H NMR, 29Si NMR), and thermal (DSC) methods. Coated fused silica columns were evaluated with respect to polarity, crosslinkability with several free-radical initiators, and thermal stability. A new liquid phase, 7% cyanoethyl, 7% phenyl, 1% vinyl methyl polysiloxane is shown to be more polar than OV-1701, more temperature stable, easily crosslinked and suitable for use in supercritical fluid chromatography. 相似文献
162.
《Arabian Journal of Chemistry》2020,13(5):5326-5331
The electrochemical behavior of PbO2/PbSO4 electrode is investigated in 4.5 M H2SO4 in presence of three surfactants, Sodium Dodecyl Sulfate (SDS), Cetyltrimethylammonium bromide (CTAB) and Sodium tripolyphosphate (STPP), using cyclic voltametry, electrochemical spectroscopy impedance and galvanostatic discharge as techniques. The micro morphology of the surface of the modified PbO2 electrodes is examined by scanning electron microscopy. The results show that SDS and CTAB when added in the electrolyte could refine the coating particles and change the roughness of the surface of the electrode leading to a thin film of PbO2 with amorphous character. In addition, SDS and CTAB shift the hydrogen evolution potential towards more negative values, improve the discharge capacity of the anodic layer and accelerate the charge transfer. Under cathodic polarization, CTAB presents the lowest value of the charge transfer resistance Rct. In the contrary, STPP shifts the oxygen evolution potential towards more positive values, passivates the surface of the electrode and inhibits completely the reaction of PbO2 formation. 相似文献
163.
聚(对苯二甲酸-1,3-丙二酯)环状低聚物的合成、表征和开环聚合反应 总被引:1,自引:0,他引:1
探索了由对苯二甲酰氯和1,3-丙二醇在“假高稀”条件下合成聚(对苯二甲酸-1,3-丙二酯)(PTT)环状低聚物的可行性.通过柱色谱分离了环状低聚物和线形低聚物;用核磁共振、质谱和元素分析表征了产物的化学结构;用GPC和HPLC研究了不同大小环的分布,发现在本文实验条件下合成的PTT环状低聚物主要由二、三、四、五和七聚体构成,其中环状三聚体含量最多,没有发现环状六聚体的存在.PTT环状低聚物的熔程为92.3~222.6℃,熔融后是无色、透明的低粘度液体.于250℃将PTT环状低聚物分别在辛酸亚锡、1-乙基-3-氯四丁基锡氧烷、钛酸四丁酯和三氧化二锑催化下进行开环聚合反应,制备了特性粘数为0.18~0.49dL/g的聚合物. 相似文献
164.
Two new marine sediment standard reference materials (SRMs) for the determination of organic contaminants 总被引:3,自引:0,他引:3
Wise SA Poster DL Schantz MM Kucklick JR Sander LC Lopez de Alda M Schubert P Parris RM Porter BJ 《Analytical and bioanalytical chemistry》2004,378(5):1251-1264
Two new marine sediment standard reference materials (SRMs), SRM 1941b Organics in Marine Sediment and SRM 1944 New York/New Jersey Waterway Sediment, have been recently issued by the National Institute of Standards and Technology (NIST) for the determination of organic contaminants including polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyl (PCB) congeners, and chlorinated pesticides. Both sediment SRMs were analyzed using multiple analytical methods including gas chromatography/mass spectrometry (GC/MS) on columns with different selectivity, reversed-phase liquid chromatography with fluorescence detection (for PAHs only), and GC with electron capture detection (for PCBs and pesticides only). SRM 1941b has certified concentrations for 24 PAHs, 29 PCB congeners, and 7 pesticides, and SRM 1944 has certified concentrations for 24 PAHs, 29 PCB congeners, and 4 pesticides. Reference concentrations are also provided for an additional 58 (SRM 1941b) and 39 (SRM 1944) PAHs, PCB congeners, and pesticides. SRM 1944, which was collected from multiple sites within New York/New Jersey coastal waterways, has contaminant concentrations that are generally a factor of 10–20 greater than SRM 1941b, which was collected in the Baltimore (Maryland) harbor. These two SRMs represent the most extensively characterized marine sediment certified reference materials available for the determination of organic contaminants.Electronic Supplementary Material Supplementary material is available in the online version of this article at . A link in the frame on the left on that page takes you directly to the supplementary material. 相似文献
165.
The synthesis of unsymmetrically substituted metallophthalocyanines (M = Zn, Ni, Co) bearing two phenylethyl moieties and six alkythio substituents was achieved by co-cyclotetramerization of two different phthalonitrile derivatives, namely 4,5-di(hexylthio)phthalonitrile and 4,5-di(phenylethynyl)phthalonitrile in the presence of zinc, cobalt or nickel salts. In contrast to the totally alkyne substituted phthalocyanines, these partially alkyne-containing derivatives are more soluble and their Q band absorptions are red-shifted when compared with all alkylthio phthalocyanines. Electrochemical properties of the phthalocyanines were studied by cyclic voltammetry. 相似文献
166.
J. Stephen Clark Rebecca P. Freeman Andrew W. Thomas Claire Wilson 《Tetrahedron letters》2004,45(47):8639-8642
A concise enantioselective synthesis of the cyclic ether core of the marine natural product (+)-laurenyne has been accomplished using ring-closing metathesis for medium-ring construction. 相似文献
167.
Toshiharu Arai 《Tetrahedron letters》2004,45(30):5921-5924
A stereoselective total synthesis of (+)-cylindricine C has been achieved starting with (S)-N-Boc-2-pyrrolidinone. The key elements of this synthesis involve the sequence of reactions including BF3-mediated addition of the allyl Grignard reagent to the cyclic imine, spirocyclization via enamine formation, and intramolecular Michael addition to form the tricyclic core. 相似文献
168.
《Electroanalysis》2004,16(17):1439-1443
A film of poly‐L ‐lysine (PLL) adheres better to the surface of a glassy carbon electrode when the PLL is partially cross‐linked by means of glutaraldehyde. A film composition of 97.5% PLL/2.5% glutaraldehyde gives good adhesion and retains the anionic exchange capability of the PLL. The performance of the film was tested with hexacyanoferrate(III) using electrochemical and nonelectrochemical accumulation. 相似文献
169.
Masahiro YoshimuraKazuomi Tsuda Hiroshi NakatsukaTomoya Yamamura Masato Kitamura 《Tetrahedron》2011,67(51):10006-10010
Catalytic reactivity in the hydrogenation of a cyclic anhydride to a biotin synthetic intermediate has been investigated on the basis of Lyons’ original method using Wilkinson Ru complex, revealing the high performance of DPPF and XANTPHOS diphosphines possessing wide bite angles. The results have shown a new trail for design of the corresponding asymmetric catalysts, and the potential utility of (S,S)-Et-FerroTANE and (S,S)-(R,R)-Ph-TRAP has been demonstrated. 相似文献
170.
Juan Á. BiscegliaJimena E. Díaz Romina A. TorresLiliana R. Orelli 《Tetrahedron letters》2011,52(41):5238-5240
In this Letter we present a method for the synthesis of N-acyl-N′-arylhexahydropyrimidines 1, by ring closure of N-acyl-N′-aryl-1,3-propanediamines 3 with formaldehyde. Cyclodehydrations were performed in aqueous medium under microwave irradiation, and led to high yields of the desired compounds in remarkably short reaction times. The method also allowed for the synthesis of hitherto unreported N-acyl-N′-arylhexahydro-1,3-diazepines 2. The acyclic tetramethylenic precursors 4 were synthesized by selective functionalization of N-arylputrescines. 相似文献