125 resultados para Solid-phase Synthesis


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The low-temperature heat capacities of trifluoroacetamide were precisely determined with a small sample precision automated adiabatic calorimeter over the temperature range from 78 to 404 K. A solid-to-solid phase transition, a fusion and a phase transition from a liquid crystalline phase to fully liquid phase have been observed at the temperatures of 336.911+/-0.102, 347.622+/-0.094 and 388.896+/-0.160 K, respectively. The molar enthalpies of these phase transitions as well as the chemical purity of the substance were determined to be 5.576+/-0.004, 11.496+/-0.007, 1.340+/-0.005 kJ mol(-1) and 99.30 mol%, respectively, on the basis of the heat capacity measurements. The molar entropies of the three phase transitions were calculated to be 16.550+/-0.012, 33.071+/-0.029 and 3.447+/-0.027 J mol(-1) K-1, respectively. Further researches of the thermochemical properties for this compound have been carried out by means of TG and DSC techniques. (C) 2000 Elsevier Science B.V. All rights reserved.

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A sensitive homogenous time-resolved fluoroimmunoassay (TR-FIA) method for bensulfuron-methyl (BSM) based on fluorescence resonance energy transfer (FRET) from a Tb3+ fluorescent chelate with N,N,N',N'-[2,6-bis(3'-aminomethyl-1'-pyrazoly)-4-phenylpyridine] tetrakis(acetic acid) (BPTA-Tb3+) to organic dye, Cy3 or Cy3.5 has been developed. New method combined the use of BPTA-Tb3+ labeled streptavidin, Cy3 or Cy3.5 labeled anti-BSM monoclonal antibody and biotinylated BSM-BSA conjugate (BSA is bovine serum albumin) for competitive-type immunoassay. After BPTA-Tb3+ labeled streptavidin was reacted with a competitive immune reaction solution containing biotinylated BSM-BSA, BSM sample and Cy3 or Cy3.5 labeled anti-BSM monoclonal antibody, the sensitized and long-lived emission of Cy3 or Cy3.5 derived from FRET was measured, and thus the concentration of BSM in sample was calculated. The present method has the advantages of rapidity, simplicity and high sensitivity since the B/F (bound reagent/free reagent) separation steps and the solid-phase carrier are not necessary. The method gives the detection limit of 2.10 ng ml(-1). The coefficient variations of the method are less than 1.5% and the recoveries are in the range of 95-105% for BSM water sample measurement. (C) 2001 Elsevier Science B.V. All rights reserved.

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The low temperature heat capacities of N-(2-cyanoethyl)aniline were measured with an automated adiabatic calorimeter over the temperature range from 83 to 353 K. The temperature corresponding to the maximum value of the apparent heat capacity in the fusion interval, molar enthalpy and entropy of fusion of this compound were determined to be 323.33 +/- 0.13 K, 19.4 +/- 0.1 kJ mol(-1) and 60.1 +/- 0.1 J K-1 mol(-1), respectively. Using the fractional melting technique, the purity of the sample was determined to be 99.0 mol% and the melting temperature for the tested sample and the absolutely pure compound were determined to be 323.50 and 323.99 K, respectively. A solid-to-solid phase transition occurred at 310.63 +/- 0.15 K. The molar enthalpy and molar entropy of the transition were determined to be 980 +/- 5 J mol(-1) and 3.16 +/- 0.02 J K-1 mol(-1), respectively. The thermodynamic functions of the compound [H-T - H-298.15] and [S-T - S-298.(15)] were calculated based on the heat capacity measurements in the temperature range of 83-353 K with an interval of 5 K. (c) 2004 Elsevier B.V. All rights reserved.

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Organophosphorus pesticides (OPPs) in vegetables were determined by stir bar sorptive extraction (SBSE) and capillary gas chromatography with thermionic specific detection (TSD). Hydroxy-terminated polydimethylsioxane (PDMS) prepared by sol-gel method was used as extraction phase. The effects of extraction temperature, salting out, extraction time on extraction efficiency were studied. The detection limits of OPPs in water were <= 1.2 ng/l. This method was also applied to the analysis of OPPs in vegetable samples and matrix effect was studied. Linear ranges of OPPs in vegetable samples were 0.05-50 ng/g with detection limits <= 0. 15 ng/g and the repeatability of the method was less than 20% relative standard deviation. (c) 2005 Elsevier B.V. All rights reserved.

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The heat capacities (C-p) of five types of gasohol (50 wt % ethanol and 50 wt % unleaded gasoline 93(#) (E50), 60 wt % ethanol and 40 wt % unleaded gasoline 93(#) (E60), 70 wt % ethanol and 30 wt % unleaded gasoline 93(#) (E70), 80 wt % ethanol and 20 wt % unleaded gasoline 93(#) (E80), and 90 wt % ethanol and 10 wt % unleaded gasoline 93(#) (E90), where the "93" denotes the octane number) were measured by adiabatic calorimetry in the temperature range of 78-320 K. A glass transition was observed at 95.61, 96.14, 96.56, 96.84, and 97.08 K for samples from the E50, E60, E70, E80, and E90 systems, respectively. A liquid-solid phase transition and a solid-liquid phase transition were observed in the respective temperature ranges of 118-153 and 155-163 K for E50, 117-150 and 151-164 K for E60, 115-154 and 154-166 K for E70, 113-152 and 152-167 K for E80, and 112-151 and 1581-167 K for E90. The polynomial equations of Cp and the excess heat capacities (C-p(E)), with respect to the thermodynamic temperature, were established through least-squares fitting. Based on the thermodynamic relationship and the equations obtained, the thermodynamic functions and the excess thermodynamic functions of the five gasohol samples were derived.