Fe-Al-α,α′-联吡啶催化体系催化马来酸酐与环氧丙烷开环共聚

马来酸酐与环氧丙烷开环共聚,所得聚酯具有功能团（C＝C）,可以通过接技、交联待方法改变其性能,马来酸杆与环氧化物开环共聚合成聚酯,所用催化剂通用有有机金属化合物和稀土 事物等,我们在铁系催化丁二聚合和马来酸酐与苯乙烯共聚的基础上,首次将Fe(acac)3-Al(i-Bu)3-α,α′－联吡啶催化剂用于马来酸酐与环氧化物开环共聚,发现该催化剂催化共聚反应具有时间短、收率高、共聚物交替度高等优点,并测定了共聚合反应动力学的参数。     

Development and validation of a gas chromatography/mass spectrometry procedure for confirmation of para-toluenesulfonamide in edible fish fillet tissue

Chloramine-T is a disinfectant being developed as a treatment for bacterial gill disease in cultured fish. As part of the drug approval process, a method is required for the confirmation of chloramine-T residues in edible fish tissue. The marker residue that will be used to determine the depletion of chloramine-T residues from the edible tissue of treated fish is para-toluenesulfonamide (p-TSA), a metabolite of chloramine-T. The development and validation of a procedure for the confirmation of p-TSA is described. Homogenized fish tissue is dried by mixing with anhydrous sodium sulfate, and the mixture is extracted with methylene chloride. The extract is passed through a silica gel solid-phase extraction column, from which p-TSA is subsequently eluted with acetonitrile. The acetonitrile extract is evaporated, and the oily residue is dissolved in hexane. The hexane solution is shaken with fresh acetonitrile. The acetonitrile solution is evaporated and the residue is redissolved in dilute potassium hydroxide solution. The aqueous solution is extracted with methylene chloride to further remove more of the fat co-extractive. The aqueous solution is reacted with pentafluorobenzyl bromide in presence of tetrabutylammonium hydrogensulfate. The resulting di-(pentafluorobenzyl) derivative of p-TSA is analyzed by gas chromatography/mass spectrometry. This method permits the confirmation of p-TSA in edible fish tissue at 20 ppb.     

冶金炉料中二氧化硅和碳化硅的联合测定

提出冶金炉料中二氧化硅及碳化硅的联合测定方法，硝酸－氢氟酸－盐酸溶解二氧化硅，用硅氟酸钾容量法测定，残渣经焦硫酸钾溶解杂质，不溶碳化硅以重量法测定，经试样全分析及精密度考证，方法简便、可靠．     

诺氟沙星的交流示波极谱滴定法研究

本文报道了示波极谱滴定法测定诺氟沙星的含量。用ＰＨ４．４的ＨＡｃ－ＮａＡｃ缓冲溶液溶解药样，并与过量的四苯硼钠作用生成沉淀。过滤后，用硫酸亚铊回滴过量的Ｎａ－ＴＰＢ，由示波极谱图［ｄＥ／ｄｔ＝ｆ（Ｅ）］上ＴＰＢ切口的消失指示滴定络点，进而在该溶液中进行空白实验。     

Numerical simulation of phase separation of immiscible polymer blends on a heterogeneously functionalized substrate

The spinodal phase decomposition of an immiscible binary polymer blend system is investigated with numerical models in two-dimensional and three-dimensional (3D). The effect of the elastic energy is included. The mechanism of the evolution of the phase separation is studied and the characteristic length R(t) is shown to be proportional to t(13). In the case when the phase separation is directed by a heterogeneously functionalized substrate, the increase in the characteristic length is divided into two stages by a critical time. The R(t) approximately t(13) diagram can be fitted with a straight line in both the first and second stages. The slope of the fitting line significantly decreases after the critical time. The compatibility of the resulting pattern to the substrate pattern is also measured by a factor C(S). It is observed that there is also a critical time in the evolution of the compatibility for the cases with and without elastic energy. The critical time of C(S) is identical with the respective critical time of R(t). The lateral and vertical composition profiles functionalized substrate is observed with the 3D model. The difference mechanism of the cases with and without elastic energy is discussed.     

原子吸收光谱法间接测定萤石中的全硫

基于SO42-和BaCrO4溶液反应生成BaSO4沉淀, 置换出定量的CrO42-, 通过原子吸收法测定Cr, 建立了间接测定萤石中硫的原子吸收光谱法. 方法的工作曲线范围0.05～20 μg/mL SO42-, 检出限为0.017 μg/mL S, 适用于硫质量分数在0.01%～3%范围内萤石样品的测定.     

Experimental investigation of contact angle, curvature, and contact line motion in dropwise condensation and evaporation

Image-analyzing interferometry is used to measure the apparent contact angle and the curvature of a drop and a meniscus during condensation and evaporation processes in a constrained vapor bubble (CVB) cell. The apparent contact angle is found to be a function of the interfacial mass flux. The interfacial velocity for the drop during condensation and evaporation is a function of the apparent contact angle and the rate of change of radius of curvature. The dependence of velocity on the apparent contact angle is consistent with Tanner's scaling equation. The results support the hypothesis that evaporation/condensation is an important factor in contact line motion. The main purpose of this article is to present the experimental technique and the data. The equilibrium contact angle for the drop is found experimentally to be higher than that for the corner meniscus. The contact angle is a function of the stress field in the fluid. The equilibrium contact angle is related to the thickness of the thin adsorbed film in the microscopic region and depends on the characteristics of the microscopic region. The excess interfacial free energy and temperature jump were used to calculate the equilibrium thickness of the thin adsorbed film in the microscopic region.     

Intrinsic characteristic times in the drift-diffusion problem

The redistribution of impurities in a sample in the shape of a slab filled with an isotropic liquid submitted to an external field is considered. The case in which the impurities are ions dissolved in the liquid, and the external field is an electric field is also investigated. It is shown that the intrinsic time connected with the presence of the electric field is proportional to the drift time. The constant of proportionality is of the order of the ratio between the thermal agitation energy and the electrostatic energy. A closed solution for the time evolution of the density of particles is obtained. The importance of the effect on real situations is investigated. The possible application of these results to nematic samples submitted to an external electric field is discussed.     

Intrinsic characteristic times in the drift-diffusion problem

The redistribution of impurities in a sample in the shape of a slab filled with an isotropic liquid submitted to an external field is considered. The case in which the impurities are ions dissolved in the liquid, and the external field is an electric field is also investigated. It is shown that the intrinsic time connected with the presence of the electric field is proportional to the drift time. The constant of proportionality is of the order of the ratio between the thermal agitation energy and the electrostatic energy. A closed solution for the time evolution of the density of particles is obtained. The importance of the effect on real situations is investigated. The possible application of these results to nematic samples submitted to an external electric field is discussed.     

Chiral recognition in gas-phase cyclodextrin: Amino acid complexes—Is the three point interaction still valid in the gas phase?

The validity of the "three-point interaction" model is examined in the guest exchange reaction involving complexes of cyclodextrins and amino acids. The amino acid guest is exchanged in the gas phase in the presence of a gaseous alkyl amine. The net reaction is proton transfer between the protonated amino acid and the alkyl amine. The amino acid is lost as a neutral species. This reaction is sensitive to the chirality of the amino acid. Several amino acids are examined as well as the respective methyl esters to determine the role of the three interacting groups (ammonium, carboxylic acid, and side chain) in enantioselectivity. We find that the three-point interaction model is indeed valid in the gas phase. Enantioselectivity is optimal when two points of attraction and one repulsion is present in the gas-phase complex. The results are supported by molecular modeling calculations. A mechanism for the exchange is proposed.     

惰气熔融-红外法测定镍钛合金中的氧含量

针对镍钛(NiTi)合金中的氧含量进行研究,建立了惰气熔融-红外吸收法测定NiTi合金中氧含量的新方法。研究了不同助熔剂、称样量、分析功率、分析时间及比较器水平对测定结果的影响。确定采用镍做助熔剂,分析功率为4.0至5.5kW,分析时间为30s,比较水平为2的条件对NiTi合金中氧含量进行测定。惰气熔融-红外法测定NiTi合金氧含量相对标准偏差为1.8%,对标准样品的测定结果与标准值基本相符。方法操作简单,分析速度快,能满足生产要求,对工艺研究和产品质量控制具有积极意义。     

铝土矿有效铝含量测定影响因素研究

研究了影响铝土矿中有效铝含量测定的主要影响因素.主要探讨了样品粒度、均匀性对有效铝溶出效果的影响及样品组成对有效铝含量大小的影响.利用电感耦合等离子体原子发射光谱(IC P-A ES)法测定铝土矿中有效铝含量、X射线荧光光谱(XRF)法测定铝土矿中总氧化铝含量和其它杂质成分含量,借助X射线衍射光谱(XRD)法对样品进行...     

Stress studies on acyclovir

Acyclovir is an antiviral drug of choice in the treatment of many types of herpes virus infections, including genital herpes simplex infections, herpetic conjunctivitis, herpes simplex encephalitis, etc. The present study describes the degradation behavior of acyclovir under different International Conference on Harmonization recommended stress conditions (hydrolysis, oxidation, photolysis, and thermal decomposition) in order to establish a validated stability-indicating high-performance liquid chromatography method. Acyclovir is found to degrade extensively in acidic conditions and oxidative stress. Mild degradation of the drug occurs in alkaline and neutral conditions. The drug is stable to dry heat. The drug is found to be sufficiently stable after light exposure in a solid state; however, photolytic degradation is observed when the drug is exposed as a solution in water. The major degradation product in acidic hydrolysis and photolysis is identified as guanine through comparison with the standard. Separation of drug and the degradation products under various conditions is successfully achieved on a C-18 column utilizing water-methanol in the ratio of 90:10. The flow rate is 1 mL/min, and the detection wavelength is 252 nm. The method is validated with respect to linearity, precision, accuracy, selectivity, specificity, and robustness. The mean values of slope and correlation coefficient are 39.307 and 0.9998 with relative standard deviation values less than 2%. The recovery of the drug is found to be in the range of 97.34% to 102.35%. From the previous study it is concluded that the stability-indicating method developed for acyclovir can be used for analysis of the drug in various stability samples.     

Oxidative kinetics of aminoacids by N-bromoacetamide : A study of solvent effect and general base catalysis

The kinetic results of the oxidation of aminoacids by N-bromoacetamide in acid and alkaline media are presented. It is noticed that the order with respect to substrate is dependent on the nature of the medium, 0.30 – 0.80 in perchloric acid (except phenylalanine in which case the order is 1.0) and alkaline media and zero order in aqueous acetic acid. Irrespective of the medium, the reaction is first order in [oxidant]. The rate of oxidation increases with [OH^-] and decreases with [H⁺]. The changes observed in the direction of the pH-rate profile correspond to the ionization constants of the aminoacids. The reaction is inhibited by the addition of acetamide in perchloric acid medium but, is independent of it in alkaline medium. The rate of oxidation is susceptible to changes in the composition of acetic acid and is maximum at 25% aqueous acetic acid. The oxidation of aminoacids by N-bromoacetamide is also catalysed by carboxylate anions. The catalytic constants of propionate, butyrate, acetate, chloropropionate and chloroacetate are measured and Brønsted coefficients (β) so evaluated are in the range 0.38 – 0.46. The proposed mechanism and the derived rate laws are consistent with the observed kinetics.     

The effect of nanographites dispersed in Undec-10-enic acid on optical property and morphology of PDLC films

The electric conductivity is an important factor for reducing the switching voltage of polymer-dispersed liquid crystals (PDLC) films. The electric conductivity of polymer matrix is changed by doped nanographite which is uniform dispersed in polymer matrix in acid condition. The influence of doped nanographite to switching electric field is studied. With increasing of doped nanographite, the switching voltage is dramatically reduced. The effect of nanographite on the polymerization and electro-optic are discussed. The kinetic polymerization of the PDLCs is monitored in lights scattering by UV/VIS spectrometer. The polymerization speed is compared by the max scattering point in different samples which doped by nanographite. The electro-optic of PDLCs films is measured by Polarimeter (PerkinElmer Model 341) to determine the threshold voltage. Information gained from polarizing optical microscope and Fourier transform infrared image depict the morphology of the liquid crystal droplets dispersed in polymer matrix.     

High-performance liquid chromatographic method for the quantitative analysis of a synthetic copolymer with antitumor activity (copovithane) and methylamine in human blood plasma and urine

A method for the determination of a synthetic polymeric compound with antitumor activity (copovithane) and methylamine in blood plasma and urine is described. Copovithane is prepared by radical polymerisation of a diurethane with N-vinylpyrrolidone. The method is based on high-performance liquid chromatography of the methylamine hydrochloride which arises during the hydrochloric acid hydrolysis of the parent substance. The methylamine hydrochloride is converted to the trinitrobenzenesulphonyl derivative for the purpose of chromatographic detection. The limit of determination for copovithane in blood plasma is 1.2 mg/l and in urine 1.5 mg/day. The determination limit for methylamine in blood plasma is 0.2 mg/l and in urine 0.3 mg/day. The imprecision is dependent on the sample, and amounts to +/- 6.8% for blood plasma and +/- 6.4% for urine.     

Solar Light Active Graphitic Carbon Nitride/Biochar Nanocomposite for RhB Dye Degradation

In this work, nanocomposite graphitic carbon nitride/biochar is successfully prepared by physical mixing method to achieve efficient charge separation and photodegradation of RhB dye under sunlight. The biochar is synthesized by heating biomass in muffle furnace in an inert atmosphere. The graphitic carbon nitride is prepared using melamine as a precursor and heating it in a muffle furnace in air atmosphere. The structural characterizations FTIR and X-ray diffraction are done to confirm the functional groups and crystallography of prepared samples. The photodegradation of RhB dye by nanocomposite is analyzed using a UV–visible spectrophotometer under solar irradiation. It is found that the RhB dye is completely reduced by the nanocomposite in less than 6 min in the presence of sunlight. The kinetic study confirms the photodegradation of RhB dye is first order reaction and rate constant is found to be 0.31 min⁻¹.     

Computer simulation of ion chromatography separation: an algorithm enabling continuous monitoring of anion distribution on an ion-exchange chromatography column

A computer algorithm for the calculation of ion chromatography separation is presented. It is based on the calculation of equilibrium concentrations of present analyte in discrete column segments. The continuous column is treated as a number of discrete cells or segments where the equilibration process between the stationary phase and the eluent is simulated. The ion-exchange equilibration process is supposed to be instantaneous and quantitative. The continuous flow of the eluent is rendered by discrete transfers. The size of each transfer of the eluent corresponds to a portion of the volume contained in one column segment. The equilibrium calculations in all column segments are repeated for each transfer of the eluent, through all the stages of the chromatographic process. The distribution of the analytes between the stationary phase and the eluent can be monitored at any step and in any column segment which means that the described algorithm provides the spatial and time concentration profiles. The simulated chromatogram is acquired as a time-concentration profile in the last column segment. The obtained chromatograms are in good agreement with the experimental ones. The distribution of ions between the stationary phase and the eluent in the early stages of the ion chromatographic process can thus be studied with confidence.     

用于煤制天然气的气化-热解耦合系统模拟研究及能量分析

大规模煤制天然气系统中气流床气化是一种重要且富吸引力的技术。对一种气流床气化-热解耦合系统进行了研究。该系统中气化炉分为两段:主要进行煤焦气化的气化段以及主要发生煤热解的热解段。采用流程模拟方法建立了耦合系统模型并与煤气化废锅系统进行了比较。同时,考察了操作条件对耦合系统气化性能的影响,提出了优化的操作条件。结果显示,气化温度1400 ℃时,耦合系统优化的蒸汽煤比为250~300 kg(steam)·t^-1(dry coal)。耦合系统的冷煤气效率为88.18%,高于气化废锅系统(84.14%),且其消耗指标均有所降低。但耦合系统的气化性能受到热解段焦油和CH₄产率很大的影响。耦合系统总体能量利用效率为92.26%,略低于气化废锅系统(93.39%),但其火用效率比气化废锅系统高2.2%。这说明通过热解-气化的耦合方式能够有效回收气化高温合成气中的显热并提高其能量品位。     

荧光光度法测定大气、水和土壤中痕量汞

本文研究了汞离子与硫化荧光素汞反应定量地释放出荧光素汞的条件,提出了一种间接测定痕量汞的荧光光度法。应用于大气、水和土壤中痕量汞的测定,方法简便、快速。