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21.
Zusammenfassung Leitfähigkeitsmessungen an Et4NCl-Lösungen zeigen die Gültigkeit derBjerrumschen Theorie in PhPOCl2; die Dissoziationskonstante beträgt 1,5·10–2. FeCl3 verhält sich nicht wie eine Ionenverbindung, doch ähnlich wie in POCl3. Zur Verfolgung von Ionenreaktionen wurden konduktometrische Titrationen ausgeführt. ZnCl2 und AlCl3 geben 2 Chloridionen, BCl3, TiCl4, SnCl4 und PCl5 je 1 Chloridion an die Akzeptoren FeCl3 oder SbCl5, ab. In Gegenwart von polaren Chloriden nehmen BCl3, AlCl3, FeCl3, PCl5 und SbCl5 je 1 Chloridion, ZnCl2, TiCl4 und SnCl4 je nach Angebot 1 oder 2 Chloridionen auf. Sowohl die Chlorometallate, als auch die Chloroniumverbindungen sind im gleichen Ausmaß wie Et4NCl ionisiert.Mit 4 Abbildungen2. Mitt.:M. Baaz, V. Gutmann, M. Y. A. Talaat undT. S. West, Mh. Chem.92, 150 (1961).Herrn Prof. Dr.L. F. Audrieth zum 60. Geburtstag gewidmet. 相似文献
22.
The high frequency oscillator provides an excellent means of detecting the end-points of titrations performed with ethylenediaminetetraacetic acid or its salts. The determination of various divalent metals is reported, based on both direct and indirect titrations. Because of the great sensitivity of the method it is possible to determine cobalt, nickel, copper (II), zinc, cadmium, lead and manganese (II) in concentration ranges of 1/1000 to 1/6000M. 相似文献
23.
An absorptiometric method is described for sulphide ion, based on the green colour which is formed when sulphide ions are treated in ammoniacal solution with iron(III) and an excess of nitrilotriacetic acid. The recommended procedure can be applied from 1200 down to 8 ppm of sulphide and is interfered with seriously only by selenite from amongst seventeen other anions examined. The colour system is stabilized by an excess of sulphite. Suggestions are made about the nature of the colour body and its mechanism of production. 相似文献
24.
J. Bates Q. Zhang L. Spiccia B. O. West 《Journal of Sol-Gel Science and Technology》1994,2(1-3):29-34
Two lead titanium oxyalkoxides with composition Pb2Ti4O2(O2CCH3)2(OC2H5)14 and Pb2Ti2O2(O2CCH3)2(OCH(CH3)2)8 have been isolated and characterised by elemental analysis, IR, 207Pb NMR and molecular weight measurements. X-ray structural analysis of the 1:2 complex confirmed the presence of two Pb2Ti2O units which are linked by a common Pb···Pb edge and are held together by alkoxide and acetate bridges. The acetate groups have migrated from the Pb to the Ti centres during the reaction. Hydrolysis of the 1:1 Pb/Ti complex produced clear gels providing the H2O/complex ratio was less than 4. Heat treatment of the gel results in loss of residual organics below 400°C. The XRD pattern indicates the presence of the pyrochlore and perovskite phases after heating at 500°C but the sample is poorly crystalline. Complete conversion to the perovskite phase of lead titanate occurs on heating to 600°C for 1 hour. Thin films of lead titanate were deposited by dip-coating a solution of this complex in isopropanol. Analyses of the films, carried out using electron microprobe, Scanning Auger Spectroscopy and Rutherford Backscattering, indicated that they were of excellent quality, crystalline after heating at 600°C and with relatively sharp substrate-coating interface. 相似文献
25.
A new triterpenoid saponin with novel sugar moiety (1), a new trisaccharide derivative (2), as well as a known monosaccharide derivative (3), were isolated from the dried stem of Epigyhum aurilum. The structures of compounds 1 and 2 were determined by MS and NMR spectram analyses. 相似文献
26.
Douglas X. West Collin P. Galloway Catherine A. Paulson Roger K. Bunting Lewis K. Pannell 《Transition Metal Chemistry》1989,14(6):420-424
Summary CoII complexes of various stoichiometries have been isolated from reactions of the metal chlorides and bromides withN-2-(4-picolyl)-,N-2-(6-picolyl)- andN-2-(4,6-lutidyl)-N-phenylthioureas. 相似文献
27.
The effect of various organic solvents on the absorption characteristics of vanadium was studied in fuel-rich oxy-acetylene and nitrous oxide-acetylene flames. The absorption of the 3183.9 Å line of vanadium was greatly enhanced by the use of various mixed organic solvents when fed to oxy-acetylene flames. In the case of the nitrous oxide-acetylene flame, the addition of diethylene glycol (about 8% in the final solution) and similar compounds to the aqueous solution of vanadium increased the absorption by about 50%. The observations and the possible role of the mixed organic solvents are discussed. 相似文献
28.
An indirect spectrophotometric method is proposed for the determination of cyanide down to 0.2 ppm. It is based on the fact that cyanide prevents the formation of the strongly absorbing ternary complex between silver(I), 1,10-phenanthroline and Bromopyrogallol Red in nearly neutral aqueous solution. Among 17 cations examined, only mercury(II) could not be tolerated. Zinc, cadmium and cobalt interfered only when present in large amounts. A 1000-fold molar excess (over cyanide) of 14 anions can also be tolerated. Bromide, iodide and thiocyanate interference is overcome by addition of lead nitrate, ammonium sulphate and barium nitrate, followed by centrifugation. 相似文献
29.
Douglas X. West Robert M. Makeever Gozen Ertem John P. Scovill Lewis K. Pannell 《Transition Metal Chemistry》1986,11(4):131-137
Summary TheN-methyl-2-[1-(2-pyridinyl-1-oxide)ethylidene]hydrazinecarbothioamide, HLO4M, has been used to prepare a series of CoIII, NiII and CuII complexes. Species with two deprotonated LO4M ligands, one LO4M and one HLO4M ligand, two HLO4M ligands and one HLO4M ligand with two small anionic ligands have been isolated. The deprotonated LO4M bonds as a tridentate ligandvia theN-oxide oxygen, the imine nitrogen (N1 and the sulphur while the HLO4M ligand coordinates primarily as a bidentate ligandvia only the first two atoms listed above. I.r., electronic, mass and e.s.r. spectra have been used to determine the nature of these complexes. One of the more striking differences between these compounds and those prepared with other thiosemicarbazones of 2-acetylpyridine and 2-acetylpyridineN-oxide is that tetrahedral yellow [Ni(HL)X2] rather than planar brown [NiLX] (X=Cl or Br) solids have been isolated with this ligand. Other differences in the nature of the coordination spheres of the various metal ions occur with this particular ligand when compared to previously studied thiosemicarbazone complexes.NATO Fellow, on leave from Medical Faculty, Istanbul University. 相似文献
30.
[reaction: see text] The silyl group of 2-silylpyrrolidines such as 1 plays several critical roles: a stereochemical control element in a facially selective carbenoid addition to the ring nitrogen, a stereochemical "placeholder" during regioselective 1,2-migration with retention by the resulting spirocyclic ammonium ylide, and a hydroxyl surrogate for an eventual stereoselective Fleming-Tamao oxidation. This chemistry represents a novel use of the Stevens rearrangement and offers a short, enantioselective route to hydroxylated quinolizidines such as 3 from Boc-pyrrolidine. 相似文献