Short communication Catalytic synthesis of butyric esters with TiSiW_(12)O_(40)/TiO_2

The catalytic activities of TiSiW_(12)O_(40)/TiO_2 in synthesizing ethylester; propyl ester, n-butyl ester; and amyl ester were reported. It was demonstrated thatTiSiW_(12)O_(40)/TiO_2 is an excellent catalyst. Various factors concerned with esterification wereinvestigated. The optimum conditions were found: the mole ratio of alcohol to acid is 1.3:1, themass ratio of catalyst to reactants is 1.5 percent, and the reaction time is 1.0 h. Under theoptimum conditions, the yields are 88.0 percent for ethyl ester, 94.5 percent for propyl ester, 98.6percent for n-butyl ester, 99.1 percent for n-amyl ester, and 96.7 percent for iso-amyl ester,respectively.

Catalytic synthesis of cyclohexanone 1,2-propanediol ketal with H_4SiW_(12)O_(40)/PAn

A new environmental friendly catalyst, H_4SiW_(12)O_(40)/PAn was prepared andidentified by means of FT-IR, XRD and TG/DTA. Cyclohexanone 1,2-propanediol ketal was synthesizedfrom cyclohexanone and 1,2-propanediol in the presence of H_4SiW_(12)O_(40)/PAn The factorsinfluencing tlie synthesis were discussed and the best conditions were found out. The optimumconditions are: molar ratio of cyclohexanone to 1,2-propanediol is 1:1.4, the quantity of catalystis equal to 1.0 percent of feed stocks, and the reaction time is 40 min. H_4SiW_(12)O_(40)/PAn is anexcellent catalyst for synthesizing cyclohexanone 1,2-propanediol ketal and its yield can reachover 96.5 percent.

Preparation of SO_4^(2-)/TiO_2-WO_3 solid superacid and its catalytic activity in acetalation and ketaltion

SO_4^(2-)/TiO_2-WO_3 was prepared and its catalytic activity under differentsynthetic conditions was discussed with esterification of n-butanoic acid and n-butyl alcohol asprobing reaction. The optimum conditions are found that the mass fraction of H_2WO_4 used in thecompound is 12.5 percent, the calcination temperature is 580 deg C, the calcination time is 3 h, andthe soaked consistency of H_2SO_4 is 1.0 mol centre dot L^(-1). Then SO_4^(2-)/TiO_2-WO_3 wasapplied as the catalyst in the catalytic synthesis of eight similar important ketals and acetalsunder the optimum conditions and revealed high catalytic activity. On condition that the molar ratioof aldehyde/ketone to glycol is 1:1.5, the mass fraction of the catalyst used in the reactants is0.5 percent, and the reaction time is 1.0 h, the yields of ketals and acetals can reach 64.2percent-95.1 percent. Moreover, it can be easily recovered and reused.

Study on Non-Isothermal Decomposition Kinetics of Ephedrini Hydrochloridum

The thermal decomposition processes of ephedrini hydrochloridum and its kinetics are studied by TG-DTG techniques. A combined method, which includes Achar method, Coats-Redfera method, and Ozawa method, is put forward for determining kinetic model under non-isothermal conditions. By applying the combined method, it is determined that the thermal decomposition of ephedrini hydrochloridum is subjected to cylindrical symmetric diffusion. And the reaction function isƒ(α)=2(1-α)?, apparent activation energy (115.26±3.55) kJ·mol−1, pre-exponential factor 4.62×108 s−1. Results show that the combined method is feasible and simple.

Photodegradation of 17α-Ethynylestradiol in Aqueous Solution with Nitzschiahantzschiana or Chlorella vulgaris and Fe^(3+)

The photodegradation of 17α-ethynylestradiol (EE2) induced by highpressure mercury lamp (λ≥313 nm, 250 W) in aqueous solution with algae (e. g.Nitzschia hantzschiana andChlorella vulgaris) and Fe3+ was ineestigated initially. The affecting factors on the photodegradation were studied and described in details, such as algae concentration, Fe3+, exposure time, and so on. The concentration of EE2 in distilled water was determined using fluorescence spectrophotometer. The photodegradation of EE2 in aqueous solution exposed to 250 W high-pressure mercury lamp was evident in the presence of algae and Fe3+. With the algae concentration increasing, photodegradation rate increased. Fe3+ could accelerate the photocatalytic degradation of EE2 in aqueous solution with algae. The colloidal ferric hydroxide particles that might have absorbed on the algae cells could enhance the photocatalytic degradation of EE2 by algae. The catalysis in photocatalytic degradation reaction mainly resulted from the active oxygen (H2O2,1O2 and ·OH) that was caused by algae and Fe3+ under 250 W HPML. In this paper, the mechanism of photocatalytic degradation of EE2 by algae and Fe3+ is discussed theoretically in details. Key words 17α-ethynylestradiol - photodegradation - high-pressure mercury lamp - Nitzschia hantzschiana - Chlorella vulgaris - Fe3+ CLC number X 131. 2 Foundation item: Supported by the Scientific Research Foundation of Wuhan Environmental Protection Bureau and the National Natural Science Foundation of China (20177017)Biography: Liu Xian-li (1965-), male, Ph. D candidate, Associate professor, research direction: environmental chemistry

Synthesis and Crystal Structure of New Supramolecular Adducts of[PtCl_6]^(2-) with Cucurbit [7] uril:[(H_3O)_2 [PtCl_6]_3 [C_(42)H_(42)N_(28)O_ (14)_2·H_2O

A novel supramolecular adduct 3(C 42H 42N 28O 14) 2·H 2O (1) was synthesized by mixing 2- and cucurbit uril in solution of hydrochloric acid. The crystal structure was determined by single crystal X-ray diffraction analysis. The crystal belongs to orthorhombic system and space group F dd2 with cell dimensions: a=4.705 33 (5) nm, b=7.153 80 (6) nm, c= 1.894 61 (2) nm, Z=16, V=63.7744 (11) nm3, D c= 1.534 g/cm3, μ=3.007 mm -1, F(000)=29 120, R 1= 0.070 7, wR 2=0.169 2. In crystal, the cucurb uril molecules form two zig-zag chains.

Photocatalytic Oxidation of NO_ x with Porous TiO_2 Nanometer Thin Film

A new kind of porous nano-'IiO_2 composite films was prepared on the glasssubstrate with the water glass as binders and the sodium fluorosilicate as solidifying reagent. Themorphologies of the films were studied by scanning electron microscope(SEM).The UV-Visspcctiophotometer was also used to investigate the absorption of the films. The gas-phasephotocatalytic oxidation of nitrogen oxides on the composite film was carried out in Ti0_2/UVsystem, and some important factors affecting the photocatalytic oxidation were also studied such asthe catalyst concentration, vapor pressure and the presence of oxygen. The results showed theconversion of NO_x reached 97.5% alter 2 h UV-irradiation. The final product of photo-oxidation wasdetected to be HNO_3 by FT-IR. The way of photocatalytic oxidation of NO_x was possibly useful inthe practical application.

Spectrofluorimetric Method for the Determination of Triamcinolone Acetonide

A simple and highly sensitive method for the determination of triamcinolone acetonide in pharmaceutical formulations is presented. The approach is based on the fluorescence of production of triamcinolone acetonide oxidized by concentrated sulfuric acid. The effect of H2SO4, β-cyclodextrin (β-CD), solvent and cetyltrimethylammonium bromide (CTMAB) were discussed. And two analytical systems were established. One is CTMAB system, the linear range is 0–4.6×10?6 mol/L, and the detection limit is 3.59×10?8 mol/L. The other is β-CD and ethanol system, the linear range is 0–2.3×10?6 mol/L and the detection limit is 1.91×10?8 mol/L. The selectivity of analysis, the analytical figures of optimization, and the accuracy of the method are demonstrated with the determination of triamcinolone acetonide in pharmaceutical preparations. Key words triamcinolone acetonide - fluorimetry - CTMAB - β-cyclodextrin - pharmaceutical analysis CLC number O 657.39 Foundation item: Supported by the National Natural Science Foundation of China (20275028)Biography: Pan Zu-ting (1945-), male, Professor, research direction: analytical chemistry.

Synthesis of Novel Covalent-linked Linear Porphyrin-Thiophene Copolymers

Linear porphyrin-thiophene copolymers were synthesized by linking 5, 15-positions of porphyrin with tetrathiophene or bithiophene moieties for preparing conducting polymer. 2,8,12,18-tetraethyl-3,7,13,17-tetramethyl-5, 15-dithienylporphyrin4a (45.1%), 5, 15-di-bithienyl- 2,8,12,18-tetraethyl-3, 7, 13, 17-tetramethylporphyrin4b (61. 2%) and their metal complexes were also reported in high yields (>90%) as the monomers. 5, 15-di-bithienylporphyrin and its metal complexes could be polymerized by oxidation using FeCl3 as oxidant. However, 5,15-dithienylporphyrin and its metal complexes can not be polymerized by same reaction. Their polymers were synthesized by electrochemical oxidation on the gold-plate electrode. The structures of copolymers were identified by elemental analysis and IR spectra. And the conductivity of poly 5,15-di-bithienylporphyrin was measured to reach over 1.0× 10?6S/cm. Key words organic conductor - thienylporphyrin - porphyrin-thiophene copolymer - electropolymerization CLC number O 62 Foundation item: Supported by the National Natural Science Foundation of China (29872033, 20272046)Biography: CHEN Zhang-ping (1946-), male, Professor, research direction: porphyrin chemistry.

Synthesis of a Photolabeling Probe for the Study of Antiviral Mechanism of Ribavirin

Ribavirin has been used in urgency to treat SARS patients recently. In order to study its antiviral mechanism by photolabeling approach, we have synthesized and characterized 5-azido-1-β-D-ribofuranosyl-1,2,4-triazole-3-carboxiamide 1 as a photolabeling probe of ribavirin. The azidotriazole nucleoside showed rapid and clean photochemical reaction, suggesting that l is a promising probe to study the antiviral mechanism of ribarivin by photolabeling.

Fast Dating of Yongzheng Copper Coins in Tsing Empire by SEM-EDS

Twenty Yongzheng copper coins were fast dating by X-ray energy dispersive spectrometer with scanning electron microscope (SEM-EDS) according to official ingredient. The 20 coins were classified in two groups according to the results. Group 1 represents the coins minted before AD 1 728 and group 2 represents the coins minted after AD 1 728. At concentration range (0.00%–5.13%), the distribution of lead is not homogeneous in the coins, and the largest diameter of lead inclusion is less than 15 μm. The official fineness degrade is supported. Key words archaeometry - Yongzheng coins - dating - SEM-EDS CLC number O 69 - K 854.2 Foundation item: Supported by the Project of Instrument Upgraded of Ministry of Science and Technology of ChinaBiography: Lei Jun-feng (1975-), male, Ph. D, research direction: numismatic archaeology and instrument analysis.

Synthesis and Structure of Polypyrrole Derivatives/V_2O_5 Nanocomposites

Poly (N, N, N-trimethyl-(2-pyrrol-1-yl) ethyl ammonium iodide)/V2O5 (PTPAI/V2O5) nanocomposites were synthesized by sol-gel method. This method involved formation of vanadium pentoxide xerogel in the presence of polypyrrole derivatives solution. X-ray diffraction (XRD) indicated that the polypyrrole derivative particles encapsulated in the fibrous V2O5 network and the layered distance significantly increased from 1. 077 39 to 1. 354 56 nm. The interaction between polypyrrole and V2O5 in the ‘nanocomposites’ was characterized by IR spectroscopy. The Scanning Electron Microscope (SEM) micrographs reveal the structural contrasts between the hybrid materials and the pristine vanadium oxide xerogel. Key words polypyrrole/V2O5 - nanocomposites - XRD - SEM CLC number O 633. 5 Foundation item: Supported by the Natural Science Foundation of Hubei Province (2003ABA030)Biography: Shi Chuang (1978-), male, Master candidate, research direction: synthesis chemistry.

Microcalorimetric Study on Tyrosine Oxidation Catalyzed by Tyrosinase

Through the method of initial heat release rate, the kinetic property of tyrosine oxidation catalyzed by tyrosinase from Pseudomonas maltophilia was investigated using a LKB-2107 batch microcalorimeter. Tyrosine was catalyzed and oxidized into L-dopa, then into melanin catalyzed by tyrosinase. We found that the tyrosinase reaction obeyed the Michaelis-Menten kinetics, and at 298.15K and pH 7.0, the initial exothermic rate (W0 ) are in the range of 0.1567~0.5704 mJ·s-1, the maximum exothermic rate (Wmax) are in 0.4152 ~ 0.8143mol·L-1, and mean value of the Michaelis constant (Km) is 2.199±0.105104 mol·L-1.

Microwave-assisted Polymerization of ε-Caprolactone with Maleic Acid as Initiator and Drug Release Behavior of Ibuprofen-Poly(ε-caprolactone) System

Poly(e-caprolactone) (PCL) with weight-average molar mass over 10000 g/mol was synthesized by microwave-assisted ring-opening polymerization of e-caprolactone (e-CL) with maleic acid (MA) as initiator (2.45 GHz, 360 W, 85 min). Ibuprofen-PCL controlled release system was prepared directly by the ROP of e-CL in its mixture with ibuprofen. The release of ibuprofen from the system was sustained and steady.

Separation of Dopamine and Epinephrine by a Novel Electrophoresis Technique with Nafion Membrane as Separation Column

A novel electrophoresis technique, in which a strip of perflurosulfonic-acid (nafion 117) membrane was used to replace the conventional separation column and liquid buffer solution within, was developed and employed to separate the mixture of dopamine and epinephrine under a low separation voltage of 100 V with quadruple pulses amperometry detection. It was showed that the so-called Nafion membrane electrophoresis could be one of very simple and easy method and has the potentiality to be used to separate and analyze some small organic biologic molecules. Key words nafion membrane - electrophoresis - electrochemical detector - dopamine - epinephrine CLC number O 657. 7 Foundation item: Support by the Foundation of Electroanalytical Chemistry Open Lab (203231510), Changchum, China.Biography: Fang Cheng (1971-), male, Lecture, Ph. D, research direction: Electroanalysis.

A Novel Degradation Pathway of Zn(dmid)(phen)_2 in Pyridine

The light-oxidation degradation processes of Zn(dmid)(phen)_2 ( dmid = 4,5-dimercapto-l, 3-dithiole-2-one, phen = 1,10-phenanthroaline) in pyridine solvent has beenmonitored. It has been found under the light, dmid^(2-) of Zn(dmid)-(phen)_2 in pyridine solutioncould generate NCS~ and NCS^-replaces dmid^(2-) to form Zn(NCS)_2 (phen)_2 simultaneously. Thecrystal structure of Zn(NCS)_2 (phen)_2 has been determined. In the crystal of Zn(NCS)_2 (phen)_2,two NCS~ ligands are arranged in syn-configuration, and there is strong pi-pi interaction betweenthe two adjacent parallel phen.

Electrochemical Determination of Trace Amounts of Lead (Ⅱ) and Cadmium (Ⅱ) at a Calix[6]arene Modified Carbon Paste Electrode

An electrochemical method for the simultaneous determination of lead(II) and Cadmium(II) with a calix[6]arene modified carbon paste electrode (CPE) has been developed. Pb2+ and Cd2+ were accumulated at the surface of the modified electrode via formation of chemical complexes with calix[6]arene, and reduced at 1.40 V. During the following anodic potential sweep, reduced lead and cadmium were oxidized, and two well-defined striping peaks appeared at about ?0.60 V and ?0.84 V. Compared with a bare carbon paste electrode, the calix[6]arene modified CPE greatly improves the sensitivity of determining lead and cadmium. The stripping peak currents change linearly with the concentration of Pb2+ 3.0×10?8–8.0×10?6 mol·L?1 and with that of Cd2+ 6.0×10?8–1.0×10?5 mol ·L?1. The detection limits of Pb2+ and Cd2+ are found to be 8.0×10?9 mol·L?1 and 2.0×10?8 mol·L?1, respectively. The modified carbon paste electrode was applied to determine trace levels of lead and cadmium in water samples. Comparing with that of atomic absorption spectrometry, the results suggests that the calix[6]arene modified CPE has great potential for the practical sample analysis. Key words lead(II) - cadmium(II) - calix[6]arene - differential pulse stripping voltammetry - chemically modified electrode CLC number O 657.15 Foundation item: Supported by the National Natural Science Foundation of China (60171023)Biography: JI Xiao-bo (1980-), male, Master, research direction: electroanalytical chemistry.

Synthesis and luminescent properties of Eu^(3+)-doped Na_(24)As_2W_(22)O_(83)

The Eu^(3+)-doped Na^(24)As_2W_(22)O_83 phosphor has been prepared by solidstare reaction from Na_3AsO_4.12H_2O, Na_2WO_4.2H_2O and WO_3, and characterized by elementalanalysis, infrared spectroscopy and powder X-ray diffractometry. According to the measurements withX-ray diffraction, this material belongs to orthorhombic system with its lattice constants: avelence 1.4750 nm, b velence 1.1944 nm, c velence 1.1062 nm, it is consistent with space groupD_2~4-P2_12_12_1 (No.19). The emission and excitation spectra were measured. The luminescentproperties of Eu^(3+)-doped Na^(24)As_2W_(22)O_83 and mechanism of energy transfer were discussed.