脲醛呋喃树脂中氮含量的测定

脲醛呋喃树脂中的含氮量,一般采用克氏定氮法,方法繁琐,费时较长,不利于快速分析的要求,本文利用气相色谱法对脲醛呋喃树脂中的氮含量进行分析测定,并建立了测定方法.方法简捷、快速、重现性好,加标回收率在100.8～109.0之间,准确度较高,可很好的满足工业生产中快速分析的要求.     

高温熔融-电感耦合等离子体原子发射光谱法测定含铁尘泥中5种有害元素

准确、快速地测定含铁尘泥中有害元素,对含铁尘泥节能降废项目研究及综合利用有着重要的指导意义。实验针对含铁尘泥试样因含碳量高,导致常规酸溶解方法如果不增加除碳步骤则很难完全分解试样的问题,采用高温熔融法将试样制成熔融液后倾倒于稀酸中溶解的方法,解决了碳含量高难溶解的问题。采用四硼酸锂-碳酸锂混合熔剂在高温下将试样熔融,熔融液高温倾倒于稀酸中制成澄清溶液,由于骤冷,试样炸裂成微小玻璃珠,无迸溅,操作简单,使得后续溶解过程快速完成,从而建立了电感耦合等离子体原子发射光谱(ICP-AES)测定P、Pb、K、Na、Zn共5种有害元素的方法。按照实验方法测定含铁尘泥中P、Pb、K、Na、Zn,测定值的相对标准偏差(RSD,n=9)在1.4%～5.7%之间,加标回收率在96%～110%之间。研究结果表明方法能够满足含铁尘泥样品中5种元素的定量分析要求。     

预分离色谱法直接测定微量组份无限稀释活度系数

预分离色谱法可直接测定混合物中微量组份的无限稀释活度系数(γ~∞),而不必把此组份从混合物中分离出来。主要由四步组成:被测组份的预浓缩,被测组份的定性,选择预分离柱和γ~∞的测定。预浓缩样品经过预分离柱分出被测组份,然后进入测量柱测定γ~∞。此方法简捷、可靠与常规以纯溶质进样的色谱测y~∞的方法具有相同的测定精度,可广泛用于缺少纯样的场合。用此法测定了戊烯-1-炔-4、丁炔-2在若干酸醇中的γ~∞,分别求得了修正和未修正的UNlFAC参数,对kikic修正模型其值为ac=c,CooH=694.9(K)acooH,c=c=-99.08(K),ac=c,oH=812.99(K),aoH,c=c=143.36(K)     

Determination of the solubility parameter of poly(ethylene oxide) at 25°C by gas-liquid chromatography

The solubility parameter of poly(ethylene oxide) at 25°C has been determined using the method developed by DiPaola-Baranyi and Guillet, by the extrapolation of the values of the interaction parameter χ, at high temperatures, ranging from 70°–90°, 90°–110° and 110°–130°C down to 25°C. The values of the solubility parameter obtained, depending on the temperature ranges employed, are 9.8, 9.9 and 10.1, respectively.     

INVESTIGATION OF THE USE OF LASER-DOPPLER VELOCIMETRY IN TWO-PHASE BUBBLY FLOWS

Understanding the dynamic phenomena of viability loss of shear sensitive cells and bubble breakage and coalescence within airlift reactors requires knowledge of local, liquid-phase hydrodynamics. The laser-Doppler velocimeter (LDV) is a non-invasive instrument which may be used to obtain this information. Experimental procedures and software were developed to detect and measure Doppler bursts in two-phase flow in a split-cylinder airlift reactor. Off-line analysis of the data indicated a detection rate approximately one order of magnitude greater than that observed using an available commercial frequency tracker. Approximately 400 to 500 observations are needed for the ensemble mean to characterize the local mean velocity to within ±5% for a superficial gas velocity of 10.4 cm/s, the highest superficial gas velocity used in these studies. The limitations, prospects, and signal-processing options for LDV in this application are also discussed     

Zinc Coated Steel/Epoxy Adhesive Systems: Investigation of the Interfacial Zone by FTIR Spectroscopy

The present study takes advantage of the ability of Fourier Transform Infrared Spectroscopy (FTIR) for the analysis of ultrathin organic films on metals. FTIR in the reflection mode (IRRAS) is used in order to study the interaction of ultrathin films of dicyandiamide (hardener of most one-pack epoxy resins) with various substrates, model ones such as gold or zinc and industrial ones such as steel and zinc-coated steels.

Pure zinc surfaces and, to a lesser extent, zinc-coated steels are shown to react with dicyandiamide after heating at 180°C, as evidenced by the frequency shift of the absorption band (at about 2200 cm^-1) characteristic for nitrile groups. As real systems consist of thick layers of a fully formulated adhesive cured onto a metallic substrate, the direct investigation of such a buried interphase is no longer possible by FTIR and by most of the known spectroscopies. Some mechanically tested specimens are then analysed, after failure, by FTIR microspectrometry. The spectra obtained, corresponding to the fracture initiation zone which is about 100 μm in diameter, advocate for the presence of an ultrathin layer of modified polymer still covering the substrate.     

环己烷液相无催化剂的氧化动力学研究

采用搅拌釜反应器,在确认已排除传质因素对反应速率影响的情况下,研究了环己烷液相无催化剂的氧化反应动力学。应用自由基理论及最优化计算技术,从导出的8个候选动力学模型中,确定了最佳的动力学模型,它能满意地描述环已烷氧化过程。该动力学可为环己烷氧化工业生产操作条件的优化、反应器的选型及工业设计提供依据。     

人胎盘泌乳素的提纯及裂解片断免疫学特性的研究

采用人胎盘泌乳素（hPL）-亲和层析和抗人血清抗体-亲和层析技术，从胎盘匀浆中提取hPL纯品，经圆盘电泳、免疫电泳及交叉试验证实为单一成分。溴化氰水解后的产物，以高效液相色谱分析。分离出7个肽链片断峰，分别用hPL和人生长激素（hGH）放免法检测其活性，其中第6肽链片断无hGH免疫活性，若用此片断制备特异抗体，可避免与hGH出现交叉反应。     

Analysis of solvent extracts of bituminous coal macerals by chromatography, 1H n.m.r. and field-desorption mass spectrometry

Analysis of the carbon disulphide extracts of nine samples of UK coal-maceral concentrates by ¹H highresolution n.m.r. spectroscopy, gas-liquid chromatography and field-desorption mass spectrometry indicates the presence of components with a wide molecular weight range extending up to 1200 amu; these are attributed to n-alkanes up to ≈C₅₀ and highly condensed polynuclear aromatic compounds.     

Response of the seated human body to whole-body vertical vibration: biodynamic responses to sinusoidal and random vibration

The dependence of biodynamic responses of the seated human body on the frequency, magnitude and waveform of vertical vibration has been studied in 20 males and 20 females. With sinusoidal vibration (13 frequencies from 1 to 16 Hz) at five magnitudes (0.1–1.6 ms^? 2 r.m.s.) and with random vibration (1–16 Hz) at the same magnitudes, the apparent mass of the body was similar with random and sinusoidal vibration of the same overall magnitude. With increasing magnitude of vibration, the stiffness and damping of a model fitted to the apparent mass reduced and the resonance frequency decreased (from 6.5 to 4.5 Hz). Male and female subjects had similar apparent mass (after adjusting for subject weight) and a similar principal resonance frequency with both random and sinusoidal vibration. The change in biodynamic response with increasing vibration magnitude depends on the frequency of the vibration excitation, but is similar with sinusoidal and random excitation.