Complete assignments of 1H and 13C NMR data for 10 phenylethanoid glycosides

Ten phenylethanoid glycosides, including two new ones, isolated from the aerial parts of the mangrove plant Acanthus ilicifolius were identified. The first complete assignments of the 1H and 13C NMR chemical shifts for these glycosides were achieved by means of 2D NMR techniques, including 1H-1H COSY, TOCSY, HSQC and HMBC spectra.     

SYNTHESIS, STRUCTURE AND ELECTROCHEMICAL STUDIES ON SINGLE MoFe_3S_4 AND WFe_3S_4 CUBANE-TYPE CLUSTER COMPOUNDS*

Single cubane-like clusters, MFe_3S_4(R_2dtc)_5 (M=Mo, R_2=—(CH_2)_4—, Bz_2; M=W, R_2=Me_2, —(CH_2)4—; dtc=dialkyldithiocarbamate) were synthesized by assembly reaction of (NH_4)_2MS_4 (M=Mo, W), FeCl_2 with R_2dtcNa (or NH_4) in DMF. The structure, IR, EPR and cyclic voltammogram are described and discussed. MoFe_3S_4(C_4H_8dtc)_5 was also obtained from the conversion of linear cluster Fe(DMF)_6[(FeCl_2)_2MoS_4] in the presence of C_4H_8dtc NH_4. Both clusters MoFe_3S_4(C_4H_8dtc)_4·2C_2H_5CN and WFe_3S_4(C_4H_8dtc)_5·2DMF crystallize in the monoclinic space group C2/c with a=12.544(2), (Mo-cluster), 12.533(4) (W-cluster); b=20.478(4), 20.121(6); c=19.582(7), 19.659(2);β=102.82(2), 102.96(3)°; and Z=4, 4. Their structures were refined to R=0.057 and 0.064 with use of 2690 and 2179 reflections (ι>3Q(I)), respectively. Many similarities in structure for Mo and W clusters indicate that both Mo and W play a very similar role in the clusters.     

MgFe2O4-Fe2O3纳米粉体的软化学合成及电磁学特性

Nano-MgFe₂O₄-Fe₂O₃ magnetic powders were synthesized by citrate gel under microwave irradiation. The structure，particle size distribution，electromagnetic characteristics of nano-MgFe₂O₄-Fe₂O₃ were characterized by using TG-DTA, X-ray, electronic microscope, nano-size measurement and electromagnetism measurement apparatus。The results show that the product is a mixture of MgFe₂O₄ and Fe₂O₃ with average size of 44 nm, tanδ for the product is 0.265 and 0.610 at frequency of 1.0 GHz and 1.8 GHz respectively.     

CuO/Al2O3催化剂高温固相反应的原位XRD和Raman研究

采用原位XRD和激光Raman光谱等技术对CuO/Al2O3系列催化剂高温下的表面组成和体相结构的变化进行研究.结果表明,随着焙烧温度升高,CuO首先与载体Al2O3发生固相反应生成CuAl2O4.CuAl2O4层能阻止外层CuO进一步向载体Al2O3扩散,从而使部分CuO稳定在CuO/Al2O3催化剂的表层.     

新显色剂1－（对－偶氮苯）－3－（2－噻唑）－三氮烯与锌显色反应的研究及应用

本文研究了新显色剂１－（对－偶氮苯）－３－（２－噻唑）－三氮烯在非离子表面活性剂ＴｒｉｔｏｎＸ－１００存在下，与锌（Ⅱ）显色反应的适宜条件。结果表明，在ｐＨ１３．０～１４．０范围内，锌（Ⅱ）与题示试剂形成１：３的稳定粉红色配合物，其最大吸收波长为５４５ｎｍ，试剂的最大吸收波长为４６３ｎｍ。配合物表现摩尔吸光系数在５４５ｎｍ处为９．６×１０￣４Ｌ·ｍｏｌ￣（－１）＊ｃｍ￣（－１）；０～２４μｇ／２５ｍＬＺｎ符合比耳定律。该试剂对锌的选择性良好。方法用于铝合金中锌的直接测定，结果令人满意。     

Importance of the Debye interaction in organic solutions: Henry's law constants for polar liquids in nonpolar solvents and vice versa

Henry's law constants have been determined for -butyrolactone (BL), ethyl acetate (EA), and 2-methyl-3-pentanol (MEP) in mixtures of iso-octane (ISO) and toluene (TOL), for BL, EA, TOL, and ISO in cinnamaldehyde (CIN) and for TOL and ISO in each other and in BL. From these data and published vapor pressures, the activity coefficients at infinite dilution and the standard molar Gibbs free energy of transfer, G ₂ ⁰ of the solutes from dilute solution in ISO to dilute solution in each solvent medium have been calculated. The different behavior patterns of BL and EA are attributed to differences in their abilities to exist in different conformations possessing different dipole moments. For polar solutes, G ₂ ⁰ decreases with increasing polarizability of the solvent and with increasing dipole moment of the solute, suggesting increased contributions from dipole-induced dipole (Debye) interactions. The sigmoidal plot of G ₂ ⁰ against the change in pair potential energy calculated from the classical expressions suggests that G ₂ ⁰ seriously underestimates the strength of the Debye interactions in comparison with the London interactions.     

Liquid chromatography of the s-triazines

Summary A series of thirty s-triazine compounds have been separated using reversed-phase high-pressure liquid chromatography. A relationship between substituent activity and retention time was developed to predict molecular structure.Work partially completed at the CIBA-GEIGY Corp., McIntosh, Ala., USA.     

A Polarographic Study of ϵ-Caprolactam Complexes of Uranium and Tellurium

The polarographic behaviour of uranium and tellurium has been studied in the presence of increasing concentration of complex forming agent viz. ?-caprolactam at pH 4.4 for U(VI) and at pH 10.0 for Te(IV) at μ=0.1 M KNO₃. In both cases the waves have been found to be diffusion controlled and irreversible. The values of kinetic parameters (σπ_a and K°_f,h) have been calculated as a function of the ligand concentration. Method is suitable for the quantitative determination of these metals individually and simultaneously with the effect of diverse ions.     

铽(Ⅲ)-1,4-双(1′-苯基-3′-甲基-5′-氧代吡唑-4′-基)丁二酮-[1,4]体系荧光性质的研究及应用

本文研究了Tb(Ⅲ)-1,4-双(′-苯基-3′-甲基-5′-氧代吡唑-4′-基)丁二酮-[1,4](BPMPBD)-溴化十六烷基三甲胺(CTMAB)体系的荧光性质,探讨了响影体系荧光性质的诸因素,确定了最佳实验条件。该体系中Tb(Ⅲ)浓度以2.0×10~(-5)～1.0×10~(-10)mol/L范围内与其荧光强度呈线性关系,检测限可达到5.0×10~(-11)mol/L。应用于合成样品中微量Tb(Ⅲ)的分析,结果令人满意。     

缩杂环酮系化合物合成研究的新进展

本文以3-乙酰基酚酮化学为中心,综述了与具有两个以上的亲核基团的试剂进行成环反应来合成缩杂环(艹卓)酮系化合物的研究新进展。