Stainless steel capillary columns for high temperature gas chromatography

A layer of elemental silicon has been deposited on the surface of stainless steel tubing by means of chemical vapor deposition (CVD). Two kinds of capillary column were prepared from the deactivated tubing: cross-linked, silanol-terminated polydime-thylsiloxane wall coated open tubular (WCOT) columns and molecular sieve 13X porous layer open tubular (PLOT) columns. Unlike fused silica capillary columns, stainless steel WCOT and PLOT columns can be operated at temperatures in excess of 400°C. High temperature simulated distillation has been performed successfully with a macro bore WCOT column and rapid PNA (paraffin, naphthene, and aromatic) analysis with a multidimensional gas solid chromatographic (GSC) system using PLOT columns.     

Mass spectrometric diagnosis of the surface nitriding mechanism in a d.c. glow discharge

Reactive constituents have been investigated in a molecular beam generated in the cathode surface glow area and surface boundary layer. Mixtures of nitrogen and hydrogen form NH_x(x=0–4) compounds, which are of relevance in heterogeneous, plasma vs. metal nitriding reactions. Ammonia decomposition leads to NH_x(x=2–4). Strong cataphoretic enrichment of hydrogen has been observed in the cathode glow area. Heterogeneous reactions of NH_x with iron lead to the formation of iron nitrides via intermediates such as FeNH_2–3. In a pulsed d.c. glow discharge, increased sputtering and decreased hydrogen enrichment have been observed.     

Preparation of Fe/B powders by mechanical alloying

Steels with a high boron content are valuable as a neutron shield in waste containers and as control absorbers in nuclear reactors. The purpose of this study was to obtain by mechanical alloying an iron powder with 50% boron (by weight) and then powder-metallurgy materials. The elementary powders were mixed in a high-energy mill for 36 h in an inert atmosphere. Samples were withdrawn at intervals, and the powder was characterized by differential thermal analysis, X-ray diffraction and electron microscopy. The Fe/B powders withdrawn at different intervals of milling were diluted with further additions of iron up to a final content of 10% boron. The mixtures were uniaxially compacted at 500 MPa; their green density was verified, and they were sintered in argon at 1150°C. Their physical properties (density and dimensional change) and bending strength were evaluated and microstructural studies and fracture tests were performed.     

Electrocatalytic properties of surface oxides on gold,platinum, and stainless steel electrodes in electrooxidation of malic acid

Electrocatalytic properties of oxides formed at gold, platinum, and stainless steel electrodes in the malic acid electrooxidation in 0.1 M Na₂SO₄ are studied. Gas chromatographic analysis of the electrolyte after holding the potential at 1.0 V for 8 h shows that on platinum and gold electrodes 2 mmol of acetaldehyde are produced and on stainless steel, 45 mmol. The acetaldehyde yield is the highest on stainless steel.From Elektrokhimiya, Vol. 41, No. 3, 2005, pp. 304–309.Original English Text Copyright © 2005 by Avramov Ivi, Popi, Antonovi.This article was submitted by the authors in English.     

A stream tube model for miscible flow

A simple theoretical model is described for deriving a 1-dimensional equation for the spreading of a tracer in a steady flow at the field scale. The originality of the model is to use a stochastic appoach not in the 3-dimensional space but in the 1-D space of the stream tubes. The simplicity of calculation comes from the local relationship between permeability and velocity in a 1-D flow. The spreading of a tracer front is due to local variations in the cross-sectional area of the stream tubes, which induces randomness in travel time. The derived transport equation is averaged in the main flow direction. It differs from the standard dispersion equation. The roles of time and space variables are exchanged. This result can be explained by using the statistical theory of Continuous Time Random Walk instead of a standard Random Walk. However, the two equations are very close, since their solutions have the same first and second moments. Dispersivity is found to be equal to the product of the correlation length by the variance of the logarithm of permeability, a result similar to Gelhar's macrodispersion.Nomenclature A total cross-section area of the sample - C (resident) concentration of tracer - D,D ^* dispersion coefficient - F flux of tracer - G probability distribution function for permeability in the stream-tube segments - I tracer intensity (mass crossing a surface per unit time) - K permeability - L length of the medium - M number of stream tubes in the medium - N number of segments along a stream tube - P pressure - Q total flow rate in the sample - a length of an elementary stream-tube segment - g probability distribution function for permeability in the space - i, j indices, tube numbers - q flow rate in each stream tube - s variable cross-section area of a stream tube - t, t time - u front velocity - x space variable in the flow direction - small local variation in time - , _t longitudinal, transverse dispersivity - porosity of the porous medium - correlation length in the permeability field - viscosity of the fluid - time for filling an elementary stream tube segment - standard deviation of a stochastic variable - probability distribution of arrival times (Gaussian)     

Micro construction of poly(epsilon-caprolactone)/poly(L-lactic acid) blend film by solution casting under microwave irradiation

The micro construction of poly(epsilon-caprolactone) (PCL) and poly(L-lactic acid) (PLLA) blend films fabricated by solution casting under microwave irradiation was investigated by selective enzymatic degradation and scanning electron microscopy (SEM). The results were totally different from the blends obtained by conventional methods. The blend was more homogeneous and the PCL continuous phase more compact as no spherulites and tiny zone separation were observed from the film surface and no PCL network was observed inside the film, and the degradation of a PCL plank by Pseudomonas lipase was significantly retarded. The distributed PLLA micro spheres were enlarged and amorphous. The thermal behavior of the blend by microwave heating revealed that PCL and PLLA underwent a melting process, which induced the variations of the PCL phase and PLLA spheres. The weight loss caused by degradation of the PCL/PLLA blend obtained by conventional methods (B50c) is greater than that of the blend obtained by microwave methods (B50m), which reflects the change in morphology from a loose PCL network (B50c) to a dense PCL plank (B50m).     

Measurements of HO2 uptake coefficient on aqueous (NH4)2SO4 aerosol using aerosol flow tube with LIF system

The γ(HO₂) was elevated with increase of Cu(II) concentrations in aqueous (NH₄)₂SO₄ aerosol. The threshold of Cu(II) concentration was 10^-3 mol/L for the dramatic increase of γ(HO₂) to 0.1, suggesting sensitive γ(HO₂) value to concentration of transition metal ions in aerosol.     

石墨炉原子吸收法中热解涂层石墨管在无标准分析法测定环境样品中铬的应用

本文探讨了热解涂层石墨管测定铬的最佳实验条件,研究了各种酸和干扰物质的基体效应,提出用浓氨水为基体改进剂克服高氯酸的干扰。比较了各原子化温度时的理论和实验特征量。使热解涂层石墨管有可能用于无标准分析法测定各种环境样品中的铬。     

石墨炉原子吸收法测定钒的研究

本文比较了在标准石墨管,热解涂层和全热解石墨管中钒的吸收信号形状。用全热解石墨管和EDTA铵盐作基体改进剂,直接测定水系沉积物中痕量钒。方法的特征量为61pg/0.0044A。     

原子吸收光谱法测定拉伸断口铬镍钼钛钢样品中主成分

研究了毫克级铬镍钼风样品中主成分镍的火焰原子吸收光谱法（FAAS法）和铬、钼、钒、钛、铝的塞曼恒温平台石墨炉原子吸收光谱法（ZSTPF－AAS法）。采用了微波溶样技术作为防污染样品预处理技术，采用石墨管硅涂层改进技术提高了仪器的测试精度。其中铬、镍、钼、钒、钛、铝的相对标准偏差分别为2.7%,0.97%,8.6%,7.3%,1.7%,7.3%。其加标回收率分别为96.5%,97%,96.7%,93%,98%,91%。通过分析，发现在较低温度下铬镍钼钛钢断面上有轻微的钼偏析现象，可能是拉伸断裂的主要化学影响因素。