Glass capillary columns for separation of free organic acids

Glass capillary columns have been prepared without acidic additive in the stationary phase, from which free organic acids elute as sharp and symmetrical peaks. The required surface in the borosilicate glass capillary was generated by a combination of leaching with aqueous HCl and deposition of colloidal silica particles; it can be coated with stationary phases have a broad range of polarity. Aqueous samples containing free organic acids can also be analyzed in such columns in an isothermal mode.     

Recent development in HPLC enantioseparation — a selected review

Summary Recent developments in the field of separating optical isomers by HPLC are discussed in this brief review. In particular it is focussed on various techniques for direct enantioseparation, the interpretation of possible enantioselective separation mechanisms, and the advantages and limitations of the diverse methods. This goal is supported by representative and selected examples of chiral separations.     

Aligning Text and Phonemes for Speech Technology Applications Using an EM-Like Algorithm

A common requirement in speech technology is to align two different symbolic representations of the same linguistic ‘message’. For instance, we often need to align letters of words listed in a dictionary with the corresponding phonemes specifying their pronunciation. As dictionaries become ever bigger, manual alignment becomes less and less tenable yet automatic alignment is a hard problem for a language like English. In this paper, we describe the use of a form of the expectation-maximization (EM) algorithm to learn alignments of English text and phonemes, starting from a variety of initializations. We use the British English Example Pronunciation (BEEP) dictionary of almost 200,000 words in this work. The quality of alignment is difficult to determine quantitatively since no ‘gold standard’ correct alignment exists. We evaluate the success of our algorithm indirectly from the performance of a pronunciation by analogy system using the aligned dictionary data as a knowledge base for inferring pronunciations. We find excellent performance—the best so far reported in the literature. There is very little dependence on the start point for alignment, indicating that the EM search space is strongly convex. Since the aligned BEEP dictionary is a potentially valuable resource, it is made freely available for research use.     

电解沉积压电频移分析的理论与验证

提出了控制电位电解和恒电流电解两类电解沉积的压电频移分析法测定的理论公式,用实验结果验证了它的正确性.     

The effect of ionizing radiation on microbiological decontamination of medical herbs and biologically active compounds

Several thousand tons of medical herbs are produced annually by pharmaceutical industry in Poland. This product should be of highest quality and microbial purity. Recently, chemical methods of decontamination are recognized as less safe, thus irradiation technique was chosen to replace them in use. In the Institute of Nuclear Chemistry and Technology the national program on the application of irradiation to the decontamination of medical herbs is in progress now. The purpose of the program is to elaborate, on the basis of research work, the facility standards and technological instructions indispensable for the practice of radiation technology.     

Determination of residual levels of unsaturation in partially hydrogenated poly(2,3-diphenyl-1,3-butadiene) using TG

The thermal degradation characteristics of head-to-head poly(styrene) [HHPS] should provide insight with respect to the impact of head-to-head placement on the thermal stability of traditional atactic head-to-tail polymer [HTPS]. The synthesis of head-to-head poly(styrene) must be accomplished indirectly. The head-to-head polymer is most satisfactorily obtained by dissolving metal reduction of poly(2,3-diphenyl-1,3-butadiene) [PDBD] generated by radical polymerization of the corresponding diene monomer. Full saturation of the polymer mainchain requires several iterations of the reduction procedure. Since the decomposition of poly(2,3-diphenyl-1,3-butadiene) is prominent at 374°C and that for head-to-head poly(styrene) is similarly facile at 406°C, it seemed feasible that TG of partially hydrogenated PDBD might be utilized as a convenient means of monitoring the extent of hydrogenation. This has been demonstrated for various levels of unsaturation remaining - from approximately 90 to less than 10%. Within this range the peak areas from the DTG plots of the partially hydrogenated polymer provide a good reflection of the ratio of unsaturated to saturated units in the polymer. Even low levels of unsaturation in the polymer may be detected by the asymmetry of the decomposition peak for the polymer. This revised version was published online in August 2006 with corrections to the Cover Date.     

CeO2和Pd在Ni/γ-Al2O3催化剂中的助剂作用

采用脉冲微反技术研究了添加n型半导体氧化物CeO2及贵金属Pd对Ni/γ Al2O3催化剂上CH4积炭/CO2消炭反应性能的影响,并运用BET、TPR、CO2 TPSR及氢吸附等技术对催化剂进行了表征.结果表明, n型半导体氧化物CeO2的添加可以降低Ni/γ Al2O3催化剂上CH4裂解积炭活性,提高CO2消炭活性,添加少量贵金属Pd可以进一步改变载体Al2O3、助剂CeO2和活性组分Ni之间的相互作用,从而改善Ni/γ Al2O3催化剂的抗积炭性能.通过Ni Ce Pd/γ Al2O3催化剂上CH4积炭/CO2消炭模型对上述作用机制作出了新的解释.     

Evidence of steric factors in the fungitoxic mechanisms of 8-quinolinol and its 2-, 3-, 4-, 5-, 6-and 7-chloro and bromo analogues

Summary A study was made of the fungitoxicity of 2-, 3-, 4-, 5-, 6- and 7-chloro and bromo-8-quinolinols againstAspergillus niger,A. oryzae,Myrothecium verrucaria,Trichoderma viride andTrichophyton mentagrophytes in Sabouraud dextrose broth and in Yeast Nitrogen Base supplemented with 1%D-glucose and 0.088%L-asparagine. Based on the presence or absence of synergism between pairs of substituted 8-quinolinols and reversal or nonreversal of toxicity byL-cysteine or N-acetyl-L-cysteine, the following conclusions were reached: (1) substituents on the quinoline ring change the site(s) of action of the toxicant; (2) the sites of action of the 5-, 6-, and 7-chloro-8-quinolinols are different from each other and from 8-quinolinol and its 2-, 3-, and 4-chloro analogues, and the same is true for the corresponding bromo compounds; (3) 8-quinolinol and its 3- and 4-chloro and bromo analogues appear to share common sites of action; (4) for good antifungal activity the 2 position of the ring must not be substituted by sterically bulky groups; (5) the geometry of the binding sites of action are not so constrained that they cannot accommodate the analogously substituted chloro- and bromo-8-quinolinols.

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Nachweis sterischer Faktoren bei der Fungitoxizität von 8-Chinolinol und seinen 2-, 3-, 4-, 5-, 6- und 7-Chlor- und -Brom-Analogen

Zusammenfassung Es wurde eine Studie der Fungitoxizität von 2-, 3-, 4-, 5-, 6- und 7-Chlor- und-Brom-8-chinolinol gegenüberAspergillus niger,A. oryzae,Myrothecium verrucaria,Trichoderma viride undTrichphyton mentagrophytes in Sabouraud Dextrose Nährmedium und in Hefe-N-Base mit 1%D-Glucose und 0.088%L-Asparagin unternommen. Auf der Basis des Zutreffens oder der Abwesenheit eines Synergismus zwischen Paaren von substituierten 8-Chinolinolen und der Umkehrung oder Nichtumkehrung der Toxizität durchL-Cystein oder N-Acetyl-L-cystein wurden folgende Schlußfolgerungen abgeleitet: (1) Substituenten am Chinolin-Ring ändern die Aktionsstelle(n) des Toxikans; (2) Die Angriffsstellen der 5-, 6- und 7-Chlor-8-chinolinole sind untereinander und von 8-Chinolinol und seinen 2-, 3- und 4-Chlor-Analogen verschieden, wobei das auch für die entsprechenden Brom-Verbindungen gilt; (3) 8-Chinolinol und seine 3- und 4-Chlor- und -Brom-Analogen scheinen gemeinsame Aktionsstellen zu teilen; (4) für eine gute antifungale Aktivität darf die 2-Position des Rings nicht mit sterisch anspruchsvollen Gruppen besetzt sein; (5) Die Geometrie des Bindungsstellen der Wirkung ist nicht so gespannt, daß nicht sowohl analoge Chlor- oder Brom-8-chinolinole Platz finden.

     

Investigation of the separation of scandium and rare earth elements from red mud by use of reversed-phase HPLC

A chromatographic method has been developed for separation and determination of scandium (Sc) and rare earth elements (REEs) in samples from a red mud (RM)-utilization process. Reversed-phase high-performance liquid chromatography (RP-HPLC) with post-column derivatization using 4-(2-pyridylazo)-resorcinol (PAR) and UV–visible detection at 520 nm was tested using different gradient elution profiles and pH values to optimize separation and recovery, primarily for Sc but also for yttrium and the individual lanthanides, from iron present in the samples. The separation was performed in less than 20 min by use of a mobile phase gradient. The concentration of -hydroxyisobutyric acid (-HIBA), as eluent, was altered from 0.06 to 0.4 mol L^–1 (pH 3.7) and 0.01 mol L^–1 sodium salt n-octane sulfonic acid (OS) was used as modifier. Very low detection limits in the nanogram range and a good resolution for Sc and REEs except for Y/Dy were achieved. Before application of the method to the red mud samples and to the corresponding bauxites, Sc and REEs were leached from red mud with 0.6 mol L^–1 HNO₃ and mostly separated, as a group, from the main elements by ion exchange/selective elution (6 mol L^–1 HNO₃) in accordance with a pilot-plant process developed in this laboratory. After evaporation of the eluent to dryness the extracted elements were re-dissolved in the mobile phase. By use of this chromatographic method Sc, which is the most expensive of the elements investigated and occurs in economically interesting concentrations in red mud, could be separated not only from co-existing Fe but also from Y/Dy, Yb, Er, Ho, Gd, Eu, Sm, Nd, Pr, Ce and La. All the elements investigated were individually recovered. Their recoveries were found to be nearly quantitative.     

Immunosensors Based on Layer‐by‐Layer Self‐Assembled Au Colloidal Electrode for the Electrochemical Detection of Antigen

Colloidal Au particles have been deposited on the gold electrode through layer‐by‐layer self‐assembly using cysteamine as cross‐linkers. Self‐assembly of colloidal Au on the gold electrode resulted in an easier attachment of antibody, larger electrode surface and ideal electrode behavior. The redox reactions of [Fe(CN)₆]^4?/[Fe(CN)₆]^3? on the gold surface were blocked due to antibody immobilization, which were investigated by cyclic voltammetry and impedance spectroscopy. The interaction of antigen with grafted antibody recognition layers was carried out by soaking the modified electrode into a phosphate buffer at pH 7.0 with various concentrations of antigen at 37 °C for 30 min. Further, an amplification strategy to use biotin conjugated antibody was introduced for improving the sensitivity of impedance measurements. Thus, the sensor based on this immobilization method exhibits a large linear dynamic range, from 5–400 μg/L for detection of Human IgG. The detection limit is about 0.5 μg/L.