水性聚氨酯的制备及其性能的研究

本文以琥珀酸酐与三羟甲基丙烷反应,制得了含有羟基和羧基的酯类亲水性单体,并以此单体与ＴＤＩ和ＰＰＧ－１０００反应,制得了含有羧基的聚氨酯预聚体,在三乙醇胺水溶液中分散得到了水性聚氨酯（简称ＷＰＵ）。本文对预聚体的溶剂种类和用量,对乳胶粒的大小及形状的影响进行了研究,确认溶剂的用量越大,乳胶的粒径就越小;以丙酮作溶剂,乳胶粒为棒状或橄榄球状,而以丁酮为溶剂,得到的乳胶粒为圆球状。通过改变亲水单体的用     

N,O-羧甲基壳聚糖的合成和性质研究

采用多段升温法将壳聚糖改性,合成了取代度为1.84、平均分子量为3.08×105、等电点为7.28的N,O-羧甲基壳聚糖(CMC),分别用紫外光谱、红外光谱、荧光光谱对其结构进行了表征,并对其水溶液的Zeta电位、电导率、表面张力以及水分散体系中羧甲基壳聚糖微粒的粒径分布进行了研究.结果表明, N,O-羧甲基壳聚糖具有表面活性;介质的pH值和浓度对羧甲基壳聚糖溶液的稳定性有很大的影响.     

聚苯胺薄膜电极上示差脉冲伏安法可逆波理论研究

本文提出了聚苯胺(PANI)薄膜电极上示差脉冲伏安法可逆波理论,经验证理论和实验结果相符合.     

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.     

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。     

Vibrational-translational energy transfer n atom-polyatomic molecule collisions in thermal reaction systems

Vibrational-translational energy transfer probabilities and collisional efficiencies are calculated for atom-polyatomic molecule collisions. It is assumed that a collision complex is formed and that the total internal vibrational energy is statistically distributed among all the modes of the complex. An attractive potential is assumed and account is taken of the centrifugal barrier. Conservation of system angular momentum is imposed. Convolution of the several thermal distribution functions is carried out and completeness and detailed balance are observed. Comparison of calculated quantum statistical quantities with experiment is made for the thermal isomerization of methyl and ethyl isocyanide in the presence of heavy atomic bath gases, such as Xe or Ar, and semiquantitative agreement is found.     

用计算全息法检测卡塞格林系统主镜

为实现对卡塞格林光学系统中的非球面主镜表面面形的高精度检测,设计了一种二元位相型计算全息图(CGH)。介绍了工作原理,对CGH的相位模型参数的优化设计、衍射次级分离以及台阶位置与深度计算等关键问题进行了讨论。通过引入虚拟玻璃的概念快速建立非球面检测模型,针对卡塞格林系统主镜中心开孔的特点,通过加入同轴载波实现了衍射次级的完全分离,相比目前常用的倾斜载波方法简化了相位量化复杂度,数值仿真计算出了最优的台阶深度,降低了加工难度。给出了相应的设计方法及实例,研制投产了CGH。测试得到主镜面形的均方根误差为0.018λ,并与传统补偿器结果(RMS=0.019λ)进行对比,两者测试结果吻合,验证了该设计与检测方法的正确性,该设计方法简单快捷,适用于卡塞格林光学系统主镜面形检测。     

Determination of free, total, and esterified cholesterol by high-performance liquid chromatography

A method is described for measuring free, total, and esterified cholesterol in blood serum in which reversed-phase liquid chromatography is used and the eluate is monitored at 200 nm. The sample for total cholesterol is prepared according to the Abell-Kendall procedure, and for free cholesterol an extract of serum--isopropanol (1:5, v/v) is used. The column is a muBondapak C18, 10 micrometers, and the mobile phase for total cholesterol is isopropanol--acetonitrile (50:50, v/v); for free cholesterol, it is isopropanol--acetonitrile--water (60:30:10). An approximation of the free cholesterol, triglycerides, and individual cholesteryl esters is obtained from single chromatograms of isopropanol extracts of serum if the first mobile phase is used. In a comparison study with the Abell-Kendall method for total cholesterol, the correlation is excellent and the precision is acceptable.     

渣油悬浮床加氢水溶性催化剂预硫化研究 Ⅱ 钼酸盐硫化产物的XPS分析

通过XPS分析法对钼酸盐的硫化行为进行了考察,分别考察了四价钼物种质量分数和硫钼元素的质量分数比，发现硫化产物的表面化学组成中四价钼质量分数和硫钼元素质量分数比不成正比，证实了该产物表面钼的硫化物不完全以MoS2形式存在。未经过临氢加热的硫化产物表面的四价钼物种的质量分数显著低于经过临氢加热的样品的质量分数，说明临氢加热在钼酸盐的硫化过程中起了重要作用。氯化铵是钼酸盐硫化过程中有效的助硫化剂，当它的用量增大时，硫化产物表面四价钼的质量分数也增大。以蒽为探针，使用化学探针法测定了硫化产物在渣油加氢过程中的催化活性，发现随着氯化铵用量的增加，产物的催化活性也相应提高，印证了XPS测定结果。     

Precolumn,Capillary Column,Electron Capture G-AS Chromatography For High Efficiency Trace Determination

Abstract

A method for gas chromatographic trace determination is described in which the sample solution is injected into a packed precolumn which is connected to an EC-detector. When solvent and low boiling compounds have been eluted, the precolumn is connected to the cold entry of a capillary column with another EC-detector and the trace compound is collected as a narrow band at the entry of this column. The precolumn is then reconnected to its own detector, the capillary column is heated and the trace compound is eluted and measured. Meanwhile high boiling compounds are swept out of the precolumn. When the base line of the precolumn is stable the next sample is injected and the capillary column is cooled again, and so on. In order to avoid background plateaus and ghost peaks the carrier gas must be purified, which is easily achieved with cooling traps with dry-ice and acetone.     

A rapid solvent extraction method for the determination of caesium-137 in environmental materials

A solvent extraction method for the quantitative determination of caesium-137 in environmental samples is described. Caesium carrier is added to the ashed sample, which is dissolved with hydrochloric acid. The solution is filtered to remove any carbon and the pH is adjusted to 2.0. Sodium dodecylbenzene sulphonate is added and the extraction is done with phenol-nitrobenzene mixture. The organic phase is washed with EDTA solution and the caesium is stripped from the washed solvent with 6 M hydrochloric acid. The caesium is precipitated as caesium chlorostannate to ensure absolute decontamination from potassium-40. Recovery from standard solution is about 85% and from vegetation, rainwater and effluent samples about 80%. The method is applicable in the presence of large quantities of interfering ions, and decontamination factors for many nuclides are greater than 10³.     

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.     

Characterization of a urea optical sensor based on polypyrrole

A new optical sensor for urea determination is presented. It is based on the enzymatic reaction with urease, which is first photoimmobilized with polyacrylamide onto a chemically polymerized polypyrrole (PPy) film. The main advantage of this sensor is that no indicator dye or pH indicator is needed, because PPy itself acts as the support and the indicator. These PPy films show an absorbance spectrum in the near IR range which is pH dependent. The variation of absorbance is thus directly related to the change of pH caused during the enzymatic reaction, which is also dependent on the urea concentration. The linear range of the sensor is from 0.06 to 1 M of urea, which is the common level of urea concentration found in blood and urine samples.     

Effect of cationic monomer on properties of fluorinated acrylate latex

Cationic fluorinated acrylate latex was prepared via semi-continuous emulsion copolymerization of cationic monomer and other monomers.The resultant latex and its film were characterized with dynamic light scattering detector and contact anglc meter. Influences of amount of DMDAAC on the propcrtics of resultant latex and its film were investigated in detail.Results show that the particle size of the latex has the minimum value and the zeta potential of the latex is increased when the amount of DMDAAC is increased.In addition,the particle size of the latex is unimodal distribution when the amount of DMDAAC is not more than 2.5%. However,the particle size of the latex is bimodal distribution when the amount of DMDAAC is more than 2.5%.The contact angle is varied slightly with the increase of amount of DMDAAC when it is not more than 2.5%.Nevertheless,the contact angle is decreased with the increase of the amount of DMDAAC when it is more than 2.5%.     

Staircase voltammetry with finite diffusion space

A theory of the staircase voltammetry in a thin-layer cell is developed. The influence of the cell thickness and the redox reaction rate constant on the current and the peak potentials is analyzed. For moderately thick cells, the kinetic maximum is predicted. The relationship between peak currents and the square root of the scan rate is not linear and the response may entirely vanish if the redox reaction is fast, the cell is very thin and the scan rate is slow.     

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.     

Wastewater treatment using nanomaterial quaternary photocatalyst ZrCdPbO4 - Removal of colour pollutant by an eco friendly process

Pollution of environment is a major issue and has drawn attention of researchers throughout the globe. Water is polluted by various means like excretion of various industries and house releases, for example release of yarn, paper, and cloth industries etc. Present investigation consists of removal of such a pollutant. For this, synthesis of a novel quaternary nano particle sized photocatalyst ZrCdPbO₄ is carried and its characterization by different analytical techniques is also carried out. This is further used for removal of colour pollutants from the environment and Erythrosine-B is considered as a role model. Effect of various operational parameters like pH, concentration of dye, amount of photocatalyst, irradiation power etc. is studied, maximum degradation condition is extracted, and it is observed that reaction follows pseudo first order kinetics. Scavenger study suggests the participation of OH free radical in the reaction. Complete degradation of the dye in presence of light and photocatalyst is reported here by. Reusability of the photocatalyst is tested and is found to work up to five cycles efficiently.     

Spectrophotometric and gravimetric determination of sulfur in sebacate-base lubricants

Sulfur is determined in sebacate-base lubricants spectrophotometrically and gravimetrically. In the spectrophotometric method, a 0.2–0.3-g sample is treated with mixed acids, magnesium chloride is added, and the solution is evaporated to dryness. The sulfate is reduced to hydrogen sulfide by treatment with a mixture of hydriodic. hypophosphorous, and hydrochloric acids, and the hydrogen sulfide is distilled into ammonia solution. Lead citrate reagent is added and the brownish yellow color of lead sulfide sol is measured. An improved technique and apparatus for the distillation is described. In the gravimetric method, a 5-g sample is treated with mixed acids, antimony and tin are volatilized by treatment with hydrobromic acid, and sulfur is precipitated as barium sulfate. The recommended range of the spectrophotometric method is 0.005–0.15%,and that of the gravimetric method is 0.01–1% sulfur.     

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。