空气中^131I的取样和测量方法的研究

本文介绍一种气态和气载~(131)I 取样器。着重介绍了一种指数分布源的效率刻度方法,讨论了与取样有关的一些问题。     

Dynamics of novel hydrogen-bonded acidic fluorinated poly(amide-imide-silica) hybrids studied by solid-state NMR

Novel hydrogen-bonded acidic fluorinated poly(amide-imide-silica) hybrid materials, FPAI-SiO₂ (6E and 6F) series, were synthesized by a sol-gel process. The structures and spin relaxation of the hybrids were characterized by infrared (IR), and ²⁹Si and ¹³C nuclear magnetic resonance (NMR) spectroscopy. The abundant Q⁴ structures implied that in free catalyst the degree of condensation of tetramethoxysilane was enhanced by hydrogen-bonded acidic fluorinated poly(amide-imide). The dynamics on the local mobility of the hybrids was investigated by the time constant for energy exchange between ¹H and ²⁹Si spin system (T_SiH) and spin-diffusion path length (L) measurements. It was found that the faster T_SiH of 6E and 6F hybrids compared with the previous study of similar 6C and 6D hybrids implied that 6E and 6F hybrids had more aggregated structures even though the organic terminal segment changed from rigid imide to more flexible amide. The interactions of the charge transfer between donor and acceptor molecules or π-π aromatic stacking may be the dominant factors to affect the structures of 6E and 6F hybrids. Moreover, M¹ and D² segments of 6F hybrids had the same level mobility and the mobility of the 6F hybrids was little improved as the soft and flexible 1,3-bis(3-aminopropyl)-tetramethyl-disiloxane segment was incorporated in the dense structures of 6F hybrids. All of the L values of 6E and 6F hybrids were on the scale of 3.5-4.0 nm. The result also suggested that 6E and 6F hybrids had similar denser structures as 6D hybrids.     

低密度MTC固井液在低渗透气井的试验研究

针对陕甘宁盆地低渗透气田天然气井地层漏失等问题，通过室内试验，设计了密度为１．４１～１．６０ｇ／ｃｍ３的二级固井高炉矿渣——ＭＴＣ水泥浆和ＡＰＩＧ级水泥——ＭＴＣ水泥浆。目的提高固井质量、降低固井成本。结果通过对高炉矿渣的水化机理和两种ＭＴＣ水泥浆对比分析，认为高炉矿渣——ＭＴＣ转化法较ＡＰＩＧ级水泥——ＭＴＣ转化法，具有外加剂用量少、抗压强度高、体系简单、固井成本低等特点。结论两种低密度ＭＴＣ水泥浆配方设计合理，性能优良，能满足现场施工的要求。     

Facile optical resolution of amino acid esters via hydrolysis by an industrial enzyme in organic solvents

Racemic amino acid esters were optically resolved via hydrolysis in organic solvents by the catalysis of an industrial alkaline protease, “Alcalase”. The products which were composed mainly of L-amino acids were insoluble and easily separated by filtration. The activity of the enzyme and enantiomeric excess of the products were significantly dependent on the nature of solvent and the water content in the reaction media. Generally, high values of enantiomeric excess were obtained at low water contents. Many natural and unnatural amino acids were resolved by this method.     

Preparation of fatty acid methyl esters for gas-chromatographic analysis of lipids in biological materials

Theoretically, preparation of fatty acid methyl esters (FAMEs) deals with reversible chemical reactions in a complex system. Methodologically, there are numerous ways, generally characterized by the type of catalysts used and steps involved. Although there are more than a half dozen common catalysts, the majority fall into either acidic (HCl, H₂SO₄ and BF₃) or alkaline types (NaOCH₃, KOH and NaOH), with each having its own catalytic capability and application limitations. In terms of steps, many conventional methods, including those officially recognized, consist of drying, digestion, extraction, purification, alkaline hydrolysis, transmethylation/methylation and postreaction work-up. Although these methods are capable of providing reliable estimates if some precautions are taken, they are cumbersome, time-consuming and cost-inefficient. A new approach has been to transmethylate lipidsin situ. Due to its simplicity, high sensitivity, comparable reliability and capability to determine total fatty acids, the method of direct transmethylation is finding a unique place in lipid determination. Regardless of which method is used, quantitative methylation requires chemists to take precautions at every step involved, particularly during FAME formation and subsequent recovery steps. Evidently, there is an urgent need for more systematic studies, guided by the chemical principle of reactions involved and physicochemical properties of regents and end products, into factors affecting these steps. Hopefully, this will lead to an improved method, which measures lipid composition in biological materials not only with high accuracy but also with high efficiency and minimum costs.     

过一硫酸的合成及其在铀水冶中的应用

文章介绍了选择过一硫酸合成的最佳条件及进行生产的可行性。介绍了过一硫酸用于含铀煌斑岩、辉绿岩、花岗岩及炭板岩矿石提取铀时,与常规酸浸方法对比,有很好的经济效益和对环境的保护价值。     

Planning the GMAW process by constraint propagation

Although the gas metal arc welding (GMAW) process is widely used for joining metals, its planning is still a cumbersome task. The planning procedure involves many complex interrelationships among the process variables and depends heavily on empirical knowledge. Therefore, a solution method that allows a convenient way to represent the domain knowledge and evaluate the process variable relationships is needed. Further, the lack of a strong domain theory to quantify these interrelationships is a deficiency in the planning of the GMAW process. This paper presents a solution method that overcomes this deficiency and introduces a convenient knowledge representation scheme. The solution method considers the planning procedure to be a constraint satisfaction problem (CSP). The AC-4 algorithm is used to obtain arc consistency among nodes in the constraint network and the PC-4 algorithm is applied to obtain path consistency in the network. A modified version of the AC-4 algorithm is developed to reduce the search space and correspondingly reduce the computation time. An example is presented to demonstrate the capability of the method and its potential to reduce lead time.     

Effect of doping polyacrylic acid with some dopants as studied by different techniques

The molecular weight of polyacrylic acid (PAA) was determined by a viscometric method using NaNO₃ as solvent at 30°C. The specific electric conductivities (σ) of PAA as well as PAA doped with carbon black (CB), chromium oxide (Cr₂O₃), and cupferron with different concentrations (from 0.25 to 1 wt %) were measured at a temperature range 360–400 K. IR spectra of some polymers were determined and it was shown that when PAA was doped with 0.5 wt % CB, a C? O? C band appeared at 775–875 cm^?1. The positron annihilation lifetime (PAL) spectra in PAA doped with the above‐mentioned dopants were measured as a function of their concentrations. It was observed that the short lifetime intensity I₁ decreased, whereas the intermediate lifetime intensity I₂, which is related to the conductivity of the material, increased with increasing the wt % of Cr₂O₃ and cupferron as well as at low concentrations of CB. These results are discussed in terms of the conducting island model. It was found that there were distinct positive relationships between σ and I₂. © 2002 John Wiley & Sons, Inc. J Appl Polym Sci 84: 877–883, 2002; DOI 10.1002/app.10381     

Neutral poly(3,4-ethylenedioxythiophene-2,5-diyl)s: preparation by organometallic polycondensation and their unique p-doping behavior

Neutral and non-doped poly(3,4-ethylenedioxythiophene), PEDOTh(Ni), and its hexyl derivative, PEDOTh-C₆(Ni), have been prepared by organometallic dehalogenation polycondensation of 2,5-dichloro-3,4-ethylenedioxythiophene and its hexyl derivative with a zerovalent nickel complex. PEDOTh-C₆(Ni) was soluble in organic solvents and ¹H NMR data indicated that it had an M_n of 11,000. MALDI-TOF mass analysis of PEDOTh(Ni) gave M_n and M_w of about 1700 and 2400, respectively. PEDOTh-C₆(Ni) showed a UV-Vis absorption peak at 546 nm in CHCl₃. Electrochemical oxidation of PEDOTh-C₆(Ni) started at about −0.40 V vs Ag⁺/Ag and gave a peak at 0.20 V vs Ag⁺/Ag. Chemical and electrochemical oxidation (or p-doping) of PEDOTh-C₆(Ni), both in solutions and in a solid state, led to weakening of the original π-π^∗ peaks and rise of new peak(s) in a region of 800-1500 nm. The p-doping of PEDOTh-C₆(Ni) caused not only a decrease in the intensity of ¹H NMR signals of the bridging ethylene hydrogens but also a decrease in that of the hexyl side chain, suggesting a strong interaction of the p-dopant with the side chain. NMR data of poly(3-methoxythiophene-2,5-diyl) also supported an assumption that p-doping brings about a severe change in electronic state of the substituent attached to the polythiophene main chain. PEDOTh(Ni) had a density of 1.71 g cm⁻³; the molecular packing mode of PEDOTh(Ni) is discussed based on the density of the polymer and its XRD data.     

8-R-9苄基-9H-嘌呤衍生物的合成研究

采用 (Ph3 P) 2 PdCl2 为催化剂 ,DMF为溶剂 ,对 8 碘 9 苄基 9H 嘌呤与有机锡试剂RSnBu3 (R=乙烯基、2 噻吩基、2 呋喃基、苯乙炔基和苯基等 )之间的Stille偶合反应进行了研究 ,合成出了5种 8位取代的嘌呤衍生物。在反应温度为 80℃ ,n(8 碘 9 苄基 9H 嘌呤 )∶n (RSnBu3 )∶n〔(Ph3 P) 2 PdCl2 〕 =1 0∶1 2∶0 0 5的较佳工艺条件下 ,产品收率 4 1%～ 91%。用1H NMR、13 C NMR和MS对产物进行了表征