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991.
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993.
Yan J Kline AD Mo H Shapiro MJ Zartler ER 《Magnetic resonance in chemistry : MRC》2004,42(11):962-967
A novel methodology using the order matrix calculation to determine the absolute sign of spin-spin couplings based on the structure of organic compounds is presented. The sign of the residual dipolar coupling (RDC) depends on the sign of corresponding scalar spin-spin coupling constant and the sign of the RDC has a dramatic influence on the order matrix calculation. Therefore, the sign of the spin-spin coupling constant can be obtained by an order matrix calculation through the corresponding RDC. Six types of spin-spin coupling constants, including 2J(H,H), 1J(C,F), 2J(C,F), 3J(C,F), 2J(F,H) and 3J(F,H), were obtained simultaneously. Except for 3J(C,F) where the measured RDCs have very small magnitudes, the signs were determined unambiguously. 相似文献
994.
A two-dimensional liquid chromatography/capillary electrophoresis technique was developed for rapid and comprehensive mapping of cell extracts. The cell extracts were first separated by reversed-phase HPLC based on hydrophobicity. Fractions of the effluent from the HPLC system were collected into 96-well microtiter plates and dried under vacuum. The fractions were reconstituted with deionized water, separated by capillary array electrophoresis based on charge-to-size ratio, and detected by UV absorption at 214 nm. Prior to analysis by multiplexed capillary electrophoresis, the reconstituted fractions were concentrated on-column using large volume sample stacking with polarity switching. In this way, high-resolution analysis of even the minor components in the complicated mixture was possible. 相似文献
995.
动力学光度法测定痕量钴的研究 总被引:6,自引:0,他引:6
催化动力学法测定微量Co~(2+)已有报道,方法灵敏度一般在10~(-6)~10~(-10g)数量级,多数用于测定水、血液和高纯物质中的Co~(2+),而测定中药內的痕量CO~(2+)还未见报道。本文研究了氨水介质中Co~(2+)催化二苯偶氮酰肼氧化褪色的新指示反应及动力学条 相似文献
996.
997.
合成了β-芳氧基丙酸芳酯及β-芳氧基丙酰芳胺等17种化合物,经IR,UV,HNMR和元素分析确定了它们的结构,并对它们的生物活性进行了初步考察。 相似文献
998.
CTMAB胶束体系中反离子缔合度的测定 总被引:2,自引:0,他引:2
对十六烷基三甲基淡化按(CTMAB)水胶束体系,不同方法测得其反离子缔合度产值不同【‘-\且很高于由股团电化学理论所得q值0.67问.本文以离子选择性电极法测定CTMAB水胶束体系中反离子缩合度(仁0.65),并研究了外加盐和乙醇的影响·1实验部分1.工试剂和仪器十六烷基三甲基漠化技(CP)在无水乙醇中重结晶两次,纯化物经帕环法测其表面张力在CMC附近无最低声、·淡化钾(AR),水为。次蒸馏水,PXJIC型离子计,302型PB,电极(响应范围为PB,=1.6~3.3,响应时间为5分钟)222型甘汞电极·1.2实验方法在CMCV/de的稀… 相似文献
999.
1000.
The complexes PtRu(5)(CO)(15)(PMe(2)Ph)(mu(6)-C) (2), PtRu(5)(CO)(14)(PMe(2)Ph)(2)(mu(6)-C) (3), PtRu(5)(CO)(15)(PMe(3))(mu(6)-C) (4), PtRu(5)(CO)(14)(PMe(3))(2)(mu(6)-C) (5), and PtRu(5)(CO)(15)(Me(2)S)(mu(6)-C) (6) were obtained from the reactions of PtRu(5)(CO)(16)(mu(6)-C) (1) with the appropriate ligand. As determined by NMR spectroscopy, all the new complexes exist in solution as a mixture of isomers. Compounds 2, 3, and 6 were characterized crystallographically. In all three compounds, the six metal atoms are arranged in an octahedral geometry, with a carbido carbon atom in the center. The PMe(2)Ph and Me(2)S ligands are coordinated to the Pt atom in 2 and 6, respectively. In 3, the two PMe(2)Ph ligands are coordinated to Ru atoms. In solution, all the new compounds undergo dynamical intramolecular isomerization by shifting the PMe(2)Ph or Me(2)S ligand back and forth between the Pt and Ru atoms. For compound 2, DeltaH++ = 15.1(3) kcal/mol, DeltaS++ = -7.7(9) cal/(mol.K), and DeltaG(298) = 17.4(6) kcal/mol for the transformation of the major isomer to the minor isomer; for compound 4, DeltaH++ = 14.0(1) kcal/mol, DeltaS++ = -10.7(4) cal/(mol.K), and DeltaG(298) = 17.2(2) kcal/mol for the transformation of the major isomer to the minor isomer; for compound 6, DeltaH++ = 18(1) kcal/mol, DeltaS++ = 21(5) cal/(mol.K) and DeltaG(298) = 12(2) kcal/mol. The shifts of the Me(2)S ligand in 6 are significantly more facile than the shifts for the phosphine ligand in compounds 2-5. This is attributed to a more stable ligand-bridged intermediate for the isomerizations of 6 than that for compounds 2-5. The intermediate for the isomerization of 6 involves a bridging Me(2)S ligand that can use two lone pairs of electrons for coordination to the metal atoms, whereas a tertiary phosphine ligand can use only one lone pair of electrons for bridging coordination. 相似文献