高效液相色谱-电感耦合等离子体发射光谱联用的瞬时信号采集和处理软件及实际应用

本文对高效液相色谱-电感耦合等离子体原子发射光谱联用技术进行了研究.对所用ICAP-9000型等离子体原子发射光谱仪的控制采样程序进行了部分修改,采集的数据通过异步串行通讯方式由AppleⅡ微机传送至IBM PC286机进行处理。发展的瞬时信号采集程序能满足HPLC的检测要求,并将这一联用技术成功的用于砷的形态分析.     

Laser-Induced Fluorescence (LIF) Probe for <Emphasis Type="Italic">In-situ</Emphasis> Nitric Oxide Concentration Measurement in a Non-thermal Pulsed Corona Discharge Plasma Reactor

Laser-induced fluorescence (LIF) is an effective in-situ probe for NO concentrations below 300 ppm in a non-thermal plasma reactor. A new method has been developed to measure in-situ NO concentration in the reactor discharge region using a long-time—on the order of seconds—averaged fluorescence detection. This method, for quantifying NO concentration in a nonthermal plasma reactor, is simpler than a short-time—on the order of nanoseconds—fluorescence detection. For accurate measurement based on the new method, the LIF intensity must be close to the corona-induced fluorescence (CIF) intensity; the CIF intensity serves as a guide in selecting the LIF intensity. We find that a kinetic model proposed earlier works for two-tube reactors and represents the NO concentration in the middle of the reactor, which verifies the assumption of gas plug flow.     

Simultaneous multichannel mass-specific detection for high-performance liquid chromatography using an array detector sector-field mass spectrometer

The use of a separation step, such as liquid chromatography, prior to inductively coupled plasma mass spectrometry (ICP–MS) has become a common tool for highly selective and sensitive analyses. This type of coupling has several benefits including the ability to perform speciation analysis or to remove isobaric interferences. Several limitations of conventional instruments result from the necessity to scan or pulse the mass spectrometer to obtain a complete mass spectrum. When the instrument is operated in such a non-continuous manner, duty cycle is reduced, resulting in poorer absolute limits of detection. Additionally, with scanning instruments, spectral skew can be introduced into the measurement, limiting quantitation accuracy. To address these shortcomings, a high-performance liquid chromatograph has been coupled to an ICP–MS capable of continuous sample introduction and simultaneous multimass detection. These features have been realized with a novel detector array, the focal plane camera. Instrument performance has been tested for both speciation analysis and for the elimination of isobaric interferences. Absolute limits of detection in the sub picogram to tens of picograms regime are obtainable, while the added mass dimension introduced by simultaneous detection dramatically increases chromatographic peak capacity.     

Fundamental aspect and behavior of saturated fluorocarbons in glow discharge in absence of potential source of hydrogen

The glow discharge of a series of saturated fluorocarbons, C_nF_2n+2 (n = 1, 2, 4, 6, and 8), was studied with glass substrates which do not contain any hydrogen. It was found that the deposition rate was a function of the F/C ratio of the starting fluorocarbons. That is, fluorocarbons with higher F/C ratio, such as CF₄ and C₂F₆, hardly polymerized, while fluorocarbons with lower F/C ratio, such as C₈F₁₈, polymerized as well as C₂F₄. After plasma exposure, the surface of glass substrate was characterized by measurements of water contact angle, water droplet rolling-off angle, and ESCA. Although all saturated fluorocarbon plasmas could alter the surface more hydrophobic than before, the deposited materials from fluorocarbons with higher F/C were not stable. Also, in plasmas with high F/C fluorocarbons, i.e., CF₄ and C₂F₆, sputtering of the electrode material was observed. © 1992 John Wiley & Sons, Inc.     

电感耦合等离子发射光谱法测定渣油中铁、镍、钙、镁、钠、钒金属元素

用电感耦合等离子发射光谱法（ICP-AES）测定渣油中金属元素铁、镍、钙、镁、钠、钒，考察了不同的酸浓度对分析结果的影响和共存元素间的相互干扰，进行了加标回收率和精密度试验。     

Molecular Beam Mass Spectrometry System for Characterization of Thermal Plasma Chemical Vapor Deposition

A molecular beam mass spectrometry system for in situ measurement of the concentration of gas phase species including radicals impinging on a substrate during thermal plasma chemical vapor deposition (TPCVD) has been designed and constructed. Dynamically controlled substrate temperature was achieved using a variable thermal contact resistance method via a backside flow of an argon/helium mixture. A high quality molecular beam with beamtobackground signal greater than 20 was obtained under film growth conditions by sampling through a small nozzle (75 m) in the center of the substrate. Mass discrimination effects were accounted for in order to quantify the species measurements. We demonstrate that this system has a minimum detection limit of under 100 ppb. Quantitative measurements of hydrocarbon species (H, H₂, C, CH₃, CH₄, C₂H₂, C₂H₄) using Ar/H₂/CH₄ mixtures and silicon species (Si, SiH, SiH₂, SiCl, SiCl₂, Cl, HCl) using Ar/H₂/SiCl₄ mixtures were obtained under thermal plasma chemical vapor deposition conditions.     

稀土离子氮化层的组织结构观察和分析

将纯稀土金属镧、铈、钕分别放入氮化炉中，对722M24钢进行离子氮化处理，用金相显微镜、扫描电子显微镜以及透射电镜观察和分析比较了稀土离子氮化和普通离子氮化氮化层的组织结构，发现在相同条件下，不同稀土元素对氮化影响是有区别的，其中铈、钕对离子氮化有一定的促进作用，可以抑制硬脆的Fe2-3N相形成，改善扩散层的脉状组织，但纯镧金属阻碍氮的扩散，抑制铁氮化物生成，降低扩散层深度，不利于加速氮化进程。     

Particle dynamics and particle heat and mass transfer in thermal plasmas. Part III. Thermal plasma jet reactors and multiparticle injection

Thermal plasma processing involves complex interactions of particulates with plasmas. In previous studies (see Parts I and II of this series), an assessment of different effects has been made considering the dynamics and heat and mass transfer of a single particle immersed into a thermal plasma. The last paper of this sequence is concerned with the simulation of thermal plasma jet reactors and the effects caused by multiparticle injection.A mathematical model is proposed for the simulation of thermal plasma jet reactors, including the mixing phenomena between the jet and the surrounding gases by generalizing the governing equations for simple mixing flows. Also included is the density fluctuation effect by extending the K- model to a four-equation turbulence model combined with a probability density function. This model is internally consistent covering additional physical phenomena which are not covered by existing models. Unfortunately, its expected higher accuracy cannot be proven because of the present uncertainties associated with the input.For multiparticle injection, the simulation repeats calculations for single-particle injection, but with different initial conditions correcting the solutions by considering the coupling effects between particles and the plasma.The results indicate that (i) thermal plasmas show different mixing behavior in different gases; (ii) the density fluctuation effect is important since it causes large differences between the mass-weighted and unweighted time-averaged temperatures of thermal plasma jets; (iii) coupling effects become important when the particle loading rate exceeds half of the plasma mass flow rate; (iv) there are 16 constraints imposed on the modeling work which have to be considered for establishing a base for comparison with future experimental studies.     

Voltammetric behaviour and determination of moxifloxacin in pharmaceutical products and human plasma

The oxidative behaviour of moxifloxacin was studied at a glassy carbon electrode in different buffer systems using cyclic, differential pulse, and Osteryoung square-wave voltammetry. The oxidation process was shown to be irreversible over the entire pH range studied (2.0–10.0) and was diffusion-controlled. The methods were performed in Britton–Robinson buffer and the corresponding calibration graphs were constructed and statistical data were evaluated. When the proposed methods were applied at pH 6.0 linearity was achieved from 4.4×10^–7 to 1.0×10^–5 mol L^–1. Applicability to tablets and human plasma analysis was illustrated. Furthermore, a high-performance liquid chromatographic method with diode-array detection was developed. A calibration graph was established from 4.0×10^–6 to 5.0×10^–5 mol L^–1 moxifloxacin. The described methods were successfully employed with high precision and accuracy for estimation of the total drug content of human plasma and for pharmaceutical dosage forms of moxifloxacin.     

Dense Sphene-type Solid Electrolyte Through Rapid Sintering for Solid-state Lithium Metal Battery

The sphene-type solid electrolyte with high ionic conductivity has been designed for solid-state lithium metal battery. However, the practical applications of solid electrolytes are still suffered by the low relative density and long sintering time of tens of hours with large energy consumption. Here, we introduced the spark plasma sintering technology for fabricating the sphene-type Li_1.125Ta_0.875Zr_0.125SiO₅ solid electrolyte. The dense electrolyte pellet with high relative density of ca. 97.4% and ionic conductivity of ca. 1.44×10^-5 S/cm at 30℃ can be obtained by spark plasma sintering process within the extremely short time of only ca. 0.1 h. Also the solid electrolyte provides stable electrochemical window of ca. 6.0 V(vs. Li⁺/Li) and high electrochemical interface stability toward Li metal anode. With the enhanced interfacial contacts between electrodes and electrolyte pellet by the in-situ formed polymer electrolyte, the solid-state lithium metal battery with LiFePO₄ cathode can deliver the initial discharge capacity of ca. 154 mA·h/g at 0.1 C and the reversible capacity of ca. 132 mA·h/g after 70 cycles with high Coulombic efficiency of 99.5% at 55℃. Therefore, this study demonstrates a rapid and energy efficient sintering strategy for fabricating the solid electrolyte with dense structure and high ionic conductivity that can be practically applied in solid-state lithium metal batteries with high energy densities and safeties.