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.     

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。     

电位滴定法快速测定磷肥中的水溶性磷

建立了电位滴定法快速测定磷肥中水溶性磷含量的方法。用蒸饮水溶解磷肥中的水溶性磷,通过硝酸钡和阳离子交换树脂除去干扰离子,用六次甲基四胺-硝酸缓冲溶液制试液的酸度（pH=5.4),在乙醇体系中,用一定浓度的硝酸铅标准溶液进行电位滴定,用二阶微分法确定硝酸铅标准溶液的滴定终点体积。方法的RSD为0.66%-0.97%,回收率为100.00%-100.10%。     

Mo2C膜表面粗糙化规律的计算机模拟

引入晶粒边界修正,改进了Mo2C膜表面粗糙化物理模型,将DT2模型推广到包括有温度的情况,对Mo2C膜表面形态进行计算机模拟并统计模拟图的高度分布,确定表面粗糙度随沉积时间和基底温度的变化规律。结果表明：引入晶粒边界修正大大促进了理论与实验结果的一致,Mo2C膜表面粗糙化属快速粗造化,粗造度随基底温度升高而非线性地增大。     

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。     

Measuring the electrophoretic mobility of concentrated suspensions in nonaqueous media

We present a new method of measuring the electrophoretic mobility of a particle in a concentrated suspension. The method is used to measure the electrophoretic mobility of PMMA particles (diameter 10 microm) suspended in a mixture of liquid hydrocarbons. The particle volume fraction of the suspension is varied from 0 up to 0.30 and the resulting variation of the electrophoretic mobility is discussed. The suspending liquid is such that its refractive index is very close to that of the particles. Thus the suspension is almost transparent and it is possible to follow through a microscope the motion of one particle. The suspension is subjected to a low-frequency electric field (0.5 Hz). The cell containing the suspension is mounted on a piezoelectric crystal. The displacement that compensates for the particle motion (when the particle image is steady) is determined.     

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.     

The method of moments for multiplet deconvolution in gamma-ray spectrometry

The method of moments is described for deconvolution of a mixture of identical distributions; it is not necessary to know the type of the individual peak distribution. The algorithm for computing the positions and contributions of the peaks forming the multiplet is presented. The real shape of the peak is used. The computational stability of the method of moments for the deconvolution of various types of convolved triple peaks is shown to be satisfactory. The algorithm is used for deconvolution of some double peaks obtained in neutron activation analysis of rock standards. The program is fast and suitable for microcomputers.     

非标记铕配合物荧光免疫分析法研究: 测定血清中的金属硫蛋白

本文报告一种新型非同位素免疫分析法, 非标记稀土铕配合物荧光免疫分析。它仍以免疫反应为基础, 所不同的是无须制备标记物。较标记免疫分析法简便、快速、在所建立的方法中, 金属硫蛋白(MT)的量与Eu-β-二酮配合物的荧光强度成负相关。测定范围为0-1.3μg/mL, 测定血清中MT的回收率为95%-100%, 相对标准偏差<10%。     

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.     

氟吗啉合成工艺热危险性及动力学研究

氟吗啉是一种新型杀菌剂, 合成工艺热危险性和动力学研究将解决工程问题, 并保障安全生产. 采用差示扫描量热-热重分析仪(DSC-TG)测试主要原料、中间体和产品的热稳定性, 采用反应量热仪(RC1)研究反应热行为, 同时开展反应动力学研究. 研究结果显示, 主要中间体(3,4-二甲氧基苯基)(4-氟苯基)甲酮吸热分解温度为559.3 K, 乙酰吗啉吸热分解温度为478.2 K, 氟吗啉吸热分解温度为638.6 K. 氟吗啉合成反应摩尔放热量为15.44 kJ/mol, 绝热温升ΔT_ad为9.1 K, 本研究合成工艺的热危险性较小. 氟吗啉合成反应动力学方程为：r_A=kc_A^a=8.34×10^-3C_A^0.57, 对主要中间体(3,4-二甲氧基苯基)(4-氟苯基)甲酮的反应级数为0.57 级.     

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.     

由乳酸合成乳酸乙酯反应动力学的研究

研究了用强酸性阳离子交换树脂催化乳酸和乙醇酯化反应的动力学,通过对实验结果的分析,发现该反应正反应为二级反应,逆反应为零级反应,并由此推导出了反应动力学方程。同时还发现在温度较低时这一反应存在诱导期现象,并对这一现象进行了分析。     

Characteristics of an amperometric flow-through detector with a renewable stationary mercury electrode

The construction of the detector is described and its performance is assessed for 1,4-benzoquinone by flow-injection analysis. The detection limit is 0.5 ng and the relative standard deviation of the peak current is 0.4% for a 102-ng sample. The peak current is highly sensitive to temperature changes of the mercury electrode system. The relative temperature coefficient is 15% K^-1, whereas the corresponding value with respect to the mobile phase is 0.6% K^-1. The dependence of the peak current on the volume flow rate is described and explained by appropriate models.     

间苯二酚光度法测定环氧丙烷中丙醛的研究

在聚氨酯生产中,环氧丙烷中醛类物质含量直接影响聚醚质量,需要严格检查、控制。醛类物质的测定,目前国内外一般采用色谱法或比色法。也有用Hg~(2+)盐安培滴定法测定芳香醛。用2,4-二硝基苯肼直流极谱法测定醛,用原子吸收法测定低分子量醛和酮。我们根据间苯二酚与丙醛在果糖和浓盐酸作用下生成红色醌式产物的特性,较详细地研究了间苯二酚光度法测定环氧丙烷中微量丙醛的最佳条件和干扰因素。结果表明,本法灵敏度高、稳定性好,应用范围广。     

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.     

The electro-oxidative activity of cysteine on the Au electrode as evidenced by surface enhanced Raman scattering

It is demonstrated from the surface-enhanced Raman scattering that cysteine is adsorbed on the Au electrode via its carboxylate moiety. The mechanism is mainly via the charge transfer involving the pi electron-rich carboxylate moiety. The adsorption of cysteine is weak that its diffusion on the Au surface is possible. The collision of two cysteine molecules may lead to the electro-oxidative formation of cystine in an irreversible way due to that the disulfide bond is not in the close vicinity of the electrode and its rupture is hampered. The physical difference as compared to its adsorption on the Ag electrode is stressed.     

植物甾醇女士访谈录

通过采访植物甾醇女士,了解植物甾醇家族的成员、基本性质、生理功能等。揭示了其降低胆固醇、减肥、美容功能的基本原理,了解了抗癌机理,介绍了植物甾醇在食物中的分布、人体吸收困难的原因及对策,为人类健康生活提出膳食建议。     

Studies on the polarographic behaviour of estazolam

In 0.1M NH(3)-NH(4)Cl buffer (pH 9.2) a sensitive 2-electron reduction wave of estazolam is obtained by single-sweep oscillopolarography. The peak potential is -1.08 V (vs. SCE). The peak height is proportional to the concentration of estazolam over the range 1.0 x 10(-7)-9.0 x 10( partial differential)M. The detection limit is 5.0 x 10(-8)M. The behaviour of the reduction wave has been studied and applied to the determination of estazolam. The reduction process is irreversible and the wave shows adsorptive characteristics, the behaviour obeying the Frumkin adsorption isotherm. The adsorption coefficient beta is 1.16 x 10(6) 1./mole and the interaction factor alpha is -1.06. The mechanism of the electrode reaction is discussed.