无焰燃烧烟密度标准物质的研制

介绍无焰燃烧烟密度标准物质的研制方法。选用合适的α-纤维素作为原材料,经打浆造纸后,作为标准物质候选物,经均匀性检验和稳定性考察合格后,对标准物质进行定值。在无焰燃烧条件下烟密度标准物质的标准值为175,扩展不确定度为8;校正烟密度标准物质的标准值为166,扩展不确定度为8。     

Lignanoids and Diterpenoids from Callicarpa furfuraceae

The three new lignanoids 1 – 3 and the five new phyllocladane diterpenoids 7 – 11 were isolated from the leaves of Callicarpa furfuraceae, together with two known lignanoids, lariciresinol ( 4 ) and (+)‐sesamin ( 5 ), and five known diterpenoids, 17‐norphyllocladane‐3,16‐dion ( 6 ), calliterpenone ( 12 ), calliterpenone 17‐acetate ( 13 ), (3β,16α)‐phyllocladane‐3,16,17‐triol ( 14 ), and (3β,16α)‐phyllocladane‐3,16,17‐triol 17‐acetate ( 15 ). Their structures were established by spectral‐data interpretation.     

Poly(choloyl)-based amphiphiles as pore-forming agents: transport-active monomers by design

This paper describes the design and synthesis of a family of pore-forming amphiphiles. Two of these amphiphiles, which are derived from cholic acid, lysine, and p-phenylenediamine, can produce pores in lipid bilayers as individual molecules. In sharp contrast, analogous amphiphiles that do not contain a rigid 1,4-phenylenediamide moiety favor the formation of dimer-based pores. Kinetic evidence in support of monomer- and dimer-based pores has been obtained from Na+ transport measurements across bilayers made from 1-palmitoyl-2-oleoyl-2-sn-glycero-3-phosphocholine (POPC). Structure-activity studies that have been carried out with pore-forming, dimer-based amphiphiles have also revealed a significant activity dependence on their overall compactness. The practical potential of pore-forming amphiphiles with controllable supramolecular properties is briefly discussed.     

First total synthesis of a GPI-anchored peptide

A GPI-anchored dipeptide of sperm CD52 antigen was prepared through a convergent synthesis. First, the dipeptide with its C-terminus free and the GPI with its nonreducing end phosphoethanolamine bearing a free amino group were synthesized separately. Then, the two building blocks were coupled with use of EDC/HOBt as the condensation reagent. Finally, the GPI-anchored peptide was deprotected to give the target molecule 1.     

Two Novel Sub-skeleton Types of ent-Kauranoids from Isodon gesneroides

Two novel ent-kauranoids with new sub-skeleton types, gesneroidins G and H were isolated as white powder from the ether extract of the leaves of Isodon gesneroides through normal phase column chromatography. Their structures were elucidated as 3β,6α,7β-triacetoxyl-15-hydroxyl-14-oxo-ent- 15,16-seco-kaur-11,17-olide and Iα-hydroxyl-3β,6α,7β,11 β-tetraacetoxyl-ent-nor-15,17-kaur-8,16-olide on the basis of the spectral evidences including ID and 2D NMR spectra.     

Identification of Different Cobalt Nucleation on Glassy Carbon

The nucleation mechanisms of cobalt from sulfate solutions were studied by utilizing the electrochemical technique, chronoamperometry. It was found that the recorded current-time transients introduced from 1.0mol/L CoSO4 solution were complexes with unusual shapes. All characteristic features were identified as separate process. The instantaneous or progressive nucleation with 2D or 3D growth exists during the cobalt deposition, depending on the applied potentials.     

Alkyl- and aryl-substituted corroles. 4. Solvent effects on the electrochemical and spectral properties of cobalt corroles

Solvent effects on the electrochemistry and spectroscopic properties of alkyl- and aryl-substituted corroles in nonaqueous media are reported. The oxidation and reduction of six compounds containing zero to seven phenyl or substituted phenyl groups on the macrocycle were studied in four different nonaqueous solvents (CH(2)Cl(2), PhCN, THF, and pyridine) containing 0.1 M tetra-n-butylammonium perchlorate. Dimers were formed upon oxidation of all corroles in CH(2)Cl(2), but this was not the case in the other three solvents, where either monomers or dimers were formed upon oxidation depending upon the solvent Gutmann donor number and the number or location of aryl substituents on the macrocycle. The half-wave potentials were analyzed as a function of the number of aryl substituents on the macrocycle as well as the concentration of added pyridine to PhCN solutions of the compound, and these data were combined with data from the spectroelectrochemistry experiments to determine the stoichiometry of the species actually in solution after the first oxidation or first reduction of each compound. The results of these experiments indicate that reduction of the bispyridine adduct (Cor)Co(III)(py)(2) proceeds via the monopyridine complex (Cor)Co(III)(py) to give in each case the unligated cobalt(II) corrole [(Cor)Co(II)](-). In contrast, pyridine remains coordinated after electrooxidation, and the final product was characterized as [(Cor)Co(III)(py)(2)](+).     

流通池光度滴定法应用—络合反应中的质子释放数测定

用具有流通池的分光光度计作测定装置,建立了由平衡移动法测定络合反应中质子释放数的新方法。方法简单、快速,仅用一个标准溶液,适于在变更pH值范围内金属离子不发生水解和没有其他副反应的体系。     

Bahadur efficiency and robustness of studentized score tests

We derive the exact Bahadur slopes of studentized score tests for a simple null hypothesis in a one-parameter family of distributions. The Student's t-test is included as a special case for which a recent result of Rukhin (1993, Sankhy Ser. A, 55, 159–163) was improved upon. It is shown that locally optimal Bahadur efficiency for one-sample location models with a known or estimated scale parameter is attained within the class of studentized score tests. The studentized test has an asymptotic null distribution free of the scale parameter, and the optimality of likelihood scores does not depend on the existence of a moment generating function. We also consider the influence function and breakdown point of such tests as part of our robustness investigation. The influence of any studentized score test is bounded from above, indicating certain degree of robustness of validity, but a bounded score function is needed to cap the influence from below and to ensure a high power breakdown point. We find that the standard Huber-type score tests are not only locally minimax in Bahadur efficiency, but also very competitive in global efficiency at a variety of location models.