电热蒸发进样微波等离子体炬原子发射光谱法中共存元素的影响

本文考察了以微波等离子体炬（MPT）为光源，电热钽丝环进样时，溶液中共存元素对发射信号的影响。     

Thermal analysis study on vaporization of some analgesics. Acetanilide and derivatives

The thermal behaviour of acetanilide (Ac) and two of its analogues, namely the para-ethoxyacetanilide (p-Eto Ac) and the para-bromoacetanilide (p-Br Ac), which are used as analgesics in the pharmaceutical industry was studied with a simultaneous TG/DSC unit. The examined analgesics showed two endothermic DSC peaks due to melting and vaporization. By combining the experimental TG data with the corresponding reference vapour pressure data obtained with the Antoine equation the plot of P versus v was derived. From the slope of this equation the constant k-value was determined for Ac. Then, using the same k-value the vapour pressures of p-Eto Ac and p-Br Ac were determined in the same temperature range. The vaporization enthalpies for all the studied compounds were obtained from different methods and a very good agreement was found. Vaporization follows a zero-order kinetics. The activation energy of vaporization (E_vap) was calculated from the dynamic TG experiments, using the Arrhenius equation.     

电热蒸发进样—等离子体原子发射光谱中钒和钛的蒸发机理研究

自1974年Nixon报道钽丝电热蒸发作为ICP-AES进样技术以来,这一技术已引起了人们的极大兴趣,受到越来越广泛的重视。电热蒸发(ETV)-ICP-AES是一种将蒸发和激发分步进行的联用技术。石墨是目前普遍使用的蒸发器材料。然而,在高温下某些元素和石墨材料可以发生碳化反应,形成热稳定的碳化物,使分析物蒸发不完全或根本不蒸发,从而影响分析结果的灵敏度和准确性。为了解决这一问题,我们曾提出了以聚四氟乙烯(PTFE)悬浮体为氟化剂,氟化辅助ETV-ICP-AES直接测定粉煤标样中钒和钛的新方法,其检出限     

Application of correlation-gas chromatography to evaluate the vaporization enthalpy of a component in an equilibrium mixture

The vaporization enthalpies and vapor pressures of acetoin, ethyl 3-hydroxybutyrate and ethyl 3-hydroxyhexanoate, found in a variety of foods and flavors, are evaluated at T = 298.15 K using correlation-gas chromatography; values of (48.7 ± 0.4), (55.9 ± 0.6) and (61.9 ± 0.6) kJ mol⁻¹, respectively, were obtained. These values are in good agreement with estimated values. Vapor pressures of the standards as a function of temperature were also used to calculate vapor pressures of the target compounds and all resulting data were fit to second order polynomials. These polynomials were then used to predict boiling temperatures of both standards and target substances. Agreement with experimental boiling temperatures was generally within 10 K suggesting that vapor pressures are accurate to within a factor of two. Acetoin exists as an equilibrium mixture of monomer and dimer. This report provides an example of the utility of using correlation-gas chromatography to obtain thermochemical data on an impure material.     

Experimental vapor pressures of 1,2-bis(dimethylamino)ethane, 1-methylmorpholine, 1,2-bis(2-aminoethoxy)ethane and N-benzylethanolamine between 273.18 and 364.97 K

In this work, the experimental vapor pressures of four amines 1,2-bis(dimethylamino)ethane, 1-methylmorpholine, 1,2-bis(2-aminoethoxy)ethane and N-benzylethanolamine using a static apparatus are reported. The temperature range is comprised between 273.18 and 364.97 K and the pressure range between 0.782 Pa and 333 kPa. The molar enthalpies of vaporization at 298.15 K were calculated from Clausius–Clapeyron equation fitted on the experimental results.     

Computerized simulation of solute–particle vaporization in an inductively coupled plasma

Recent experiments involving aerosol introduction into the inductively coupled plasma have shown that intact droplets and solute particles cause enormous fluctuations in analyte emission and mass-spectral signals. Here, particle-vaporization kinetics are simulated as a detailed function of the operating conditions, fundamental properties and spatial location in the inductively coupled plasma, and as a function of several of the properties of the particles themselves: diameter, chemical composition and size distribution. These simulations portray the particle vaporization as proceeding nominally linearly with respect to the particle radius when the particles are small, but roughly quadratically with radius when the particles are very large. Further, the heat- and mass-transfer-limited rates of vaporization are roughly equal for the typical gas-temperature range in the plasma tail flame, so that at any height either process might limit the rate of vaporization. This similarity gives rise to a dynamic, competitive picture of plasma vaporization kinetics.     

Mass Transport of β-Diketonate Precursors for MOCVD of YBa_2Cu_3O_(7-δ) High T_c Superconducting Thin Films

IntroductionSoonafterthediscoveryofhighT.supercoducting(HTSC)oxides,metalor-ganicchemicalvapourdeposition(MOCVD)wasproposedforpreparingtheirthinfilms[1j.Asgenerallyacceptedtoday['J,thistechniquehasdemonstrateditssuperioradvantagesinmakinglargeareahighqualityHTSCthinfilmsandwillplayamajorroleintheadvanceofdeviceapplicationofHTSCthinfilmsoverthenextfewyears.TheprecursorsusedinMOCVDforpreparinghighT.superconductingthinfilmsaremostlymetalbeta-diketonates.Theyaresolidsatroomtemperatureand…     

提高光纤F-P应变传感器输出信号质量的方法研究

光纤F-P应变传感器输出信号质量的好坏直接影响解调精度.从光纤F-P应变传感器的基本原理出发,针对光纤F-P腔内损耗的问题,提出了用增加端面反射率的办法来弥补耦合损耗的影响;并通过理论分析、计算机仿真和实验对该问题进行了研究.实验表明,选用与F-P腔固有的最佳反射率匹配的端面镀膜,对增加干涉图样的对比度,提高信号输出幅值有很好的效果.     

新贮氢材料——含微量锰的微晶镁粉

以气雾化冷凝法制备了含有微量Mn的微晶镁粉(Mg(Mn)). XRD表明，其主物相仍然是六方晶系的微晶镁，其粒径在100～500 nm之间.这种微晶镁粉(Mg(Mn))具有较高的储氢量(6.2％)，在280 ℃具有较快的放氢速度.     

电热蒸发进样电感耦合等离子体原子发射光谱（ETV－ICP－AES）联用技术研究

本文采用国产部件组装了一套ＥＴＶ－ＩＣＰ－ＡＥＳ仪器体系，对装置的连接及操作参数进行优化。深入系统地考察了分析物的蒸发过程和传输过程，提出了难熔元素的蒸发和传输机理。研究了ＥＴＶ－ＩＣＰ－ＡＥＳ中基体效应，提出了以聚四氟乙烯为氟化剂，氟化辅助ＥＴＶ－ＩＣＰ－ＡＥＳ测定难熔元素的新方法，应用于环境和生物标样中痕量元素分析，获得满意结果。