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51.
A rapid method is presented for the gravimetric determination of molybdenum (as the oxinate) in ferromolybdenum and molybdenum additives. The sample is fused with a mixed flux of sodium peroxide and sodium carbonate in a zirconium crucible for complete decomposition. Leaching the cooled fusion cake with water provides instantaneous separation of molybdenum as sodium molybdate from iron(III) and other hydrous oxides. After filtration, the molybdenum is precipitated with oxine after addition of EDTA and oxalate to obviate interference from other metal oxinates, and determined gravimetrically. The precision and accuracy are comparable to those of referee methods. 相似文献
52.
P. M. Henrichs J. M. Hewitt L. J. Schwartz D. B. Bailey 《Journal of polymer science. Part A, Polymer chemistry》1982,20(3):775-782
Spin-lattice relaxation times and nuclear Overhauser enhancements (NOE) for 13C nuclei in copolymers of acrylonitrile and vinylidene chloride were measured at 20.1 and 67.9 MHz. In the ? CCl2? region of the spectrum T1 and NOE values of the various resonances are equal within experimental error and are invariant to changes in composition. The T1 and NOE values of the ? CCl2? region, however, are not equal to those of the ? CH? or ? CN region. As a result compositions cannot be calculated by direct comparison of the areas in the ? CCl2? region and either the ? CH? or the ? CN region. Discrepancies can be corrected for the ? CH? resonances by multiplication of the area by an empirical constant. A similar constant for the ? CN region is composition-dependent at 20.1 and 67.9 MHz. A chemical shift anisotropy mechanism is postulated as important for relaxation of the ? CN resonances. The overall influence of variable T1 and NOE values on quantitative determination of polymer composition is considered. 相似文献
53.
Mason Gene Bailey Billy E. Gillett 《The Journal of the Operational Research Society》1980,31(3):257-262
An algorithm is presented for solving families of integer linear programming problems in which the problems are "related" by having identical objective coefficients and constraint matrix coefficients. The righthand-side constants have the form b + θd where b and d are conformable vectors and θ varies from zero to one.The approach consists primarily of solving the most relaxed problem (θ = 1) using cutting planes and then contracting the region of feasible integer solutions in such a manner that the current optimal integer solution is eliminated.The algorithm was applied to 1800 integer linear programming problems with reasonable success. Integer programming problems which have proved to be unsolvable using cutting planes have been solved by expanding the region of feasible integer solutions (θ = 1) and then contracting to the original region. 相似文献
54.
Measuring the metabolome: current analytical technologies 总被引:44,自引:0,他引:44
The post-genomics era has brought with it ever increasing demands to observe and characterise variation within biological systems. This variation has been studied at the genomic (gene function), proteomic (protein regulation) and the metabolomic (small molecular weight metabolite) levels. Whilst genomics and proteomics are generally studied using microarrays (genomics) and 2D-gels or mass spectrometry (proteomics), the technique of choice is less obvious in the area of metabolomics. Much work has been published employing mass spectrometry, NMR spectroscopy and vibrational spectroscopic techniques, amongst others, for the study of variations within the metabolome in many animal, plant and microbial systems. This review discusses the advantages and disadvantages of each technique, putting the current status of the field of metabolomics in context, and providing examples of applications for each technique employed. 相似文献
55.
Petrie RJ Bailey T Gorman CB Genzer J 《Langmuir : the ACS journal of surfaces and colloids》2004,20(23):9893-9896
In this Letter, we report on the motion of water droplets on surfaces decorated with molecular gradients comprising semifluorinated (SF) organosilanes. SF molecular gradients deposited on flat silica substrates facilitate faster motion of water droplets relative to the specimens covered with an analogous hydrocarbon gradient. Further increase in the drop speed is achieved by advancing it along porous substrates coated with the SF wettability gradients. The results of our experiments are in quantitative agreement with a simple scaling theory that describes the faster liquid motion in terms of reduced friction at the liquid/substrate interface. 相似文献
56.
Wenzel TJ Freeman BE Sek DC Zopf JJ Nakamura T Yongzhu J Hirose K Tobe Y 《Analytical and bioanalytical chemistry》2004,378(6):1536-1547
Chiral crown ethers 1 and 5 are useful enantiomeric discriminating agents in 1H NMR spectroscopy for neutral and protonated primary amines, amino acids, and amino alcohols. The presence of the carboxylic acid groups in 1 and 5 provide sites at which ytterbium(III) can bind. Adding ytterbium(III) nitrate to crown–substrate mixtures in methanol-d4 causes shifts in the spectra of substrates and often enhances the chiral discrimination in the 1H NMR spectrum. The enhancement in enantiomeric discrimination that occurs in the presence of ytterbium(III) allows lower concentrations of the crown ether to be used in chiral recognition studies. Several amide derivatives of 1 were prepared and evaluated as chiral NMR discriminating agents, although except for 1e, these were less effective than 1. 相似文献
57.
[reaction: see text] The preparation of 1,3-dimethylindans from 4-(2-bromophenyl)-1-pentene (1) and 2-(2-iodo-1-methylethyl)styrene (2) substrates via radical-mediated cyclization and intramolecular carbolithiation has been investigated. Although cyclization of the radical derived from either substrate proceeds with modest selectivity for the cis-isomer, as does cycloisomerization of the aryllithium derived from substrate 1 (cis/trans approximately 2), intramolecular cyclization of the alkyllithium derived from substrate 2 is a highly cis-selective process (cis/trans = 12). 相似文献
58.
59.
Latent low-coordinate titanium imides supported by a sterically encumbering beta-diketiminate ligand
Basuli F Clark RL Bailey BC Brown D Huffman JC Mindiola DJ 《Chemical communications (Cambridge, England)》2005,(17):2250-2252
Addition of an equal molar quantity of R- (R = Me, SiMe3) to complex (Nacnac)Ti=NAr(OTf) (Nacnac- =[ArNC(tBu)]2CH, Ar = 2,6-iPr2C6H3) forms the imido alkyl (Nacnac)Ti=NAr(R), which can be readily protonated to afford [(Nacnac)Ti=NAr(L)]+ (L = THF, Et2O, eta1-C6H5NMe2), or treated with B(C6F5)3 to afford the zwitterion (Nacnac)Ti=NAr(micro-CH3)B(C6F5)3. 相似文献
60.
Stephen Pleasance Joseph F. Anacleto M. Ruth Bailey David H. North 《Journal of the American Society for Mass Spectrometry》1992,3(4):378-397
Atmospheric pressure ionization (API) techniques are evaluated for the mass spectral analysis of N-methyl carbamate pesticides. Atmospheric pressure chemical ionization (APCI) using a heated nebulizer interface provided both protonated molecules and abundant, characteristic fragment ions. With ion spray (ISP; pneumatically assisted electrospray ionization), which utilizes a milder “ion evaporation” process, primarily protonated molecules were obtained, although fragment ions similar to those observed in APCI could be induced by variation of the API orifice voltage. Product ion spectra of ISP-derived protonated molecules, generated by tandem mass spectrometry using collision-induced dissociation, are also presented. The APCI and ISP spectra of the carbamates are compared to those obtained with a thermospray interface and also to their electron ionization and methane CI spectra obtained with a particle beam interface. For all four interfaces, combined liquid chromatography mass spectrometry methods using conventional (4.6 mm i.d.) columns are described for the separation and detection of pesticide mixtures. These methods are applied to the confirmatory analysis of three representative carbamate pesticides, spiked at the 0.1-ppm level in green peppers. For those carbamates amenable to gas chromatography mass spectrometry, comparative results are presented. 相似文献