Characterization of polyacrylonitrile ultrafiltration membranes

Various methods have been used to characterize ultrafiltration membranes, such as gas flux measurements, (field emission) scanning electron microscopy, permporometry and liquid-liquid displacement. Significant differences in the pore size distributions determined from permporometry and liquid-liquid displacement were found.     

In situ evaluation of defect size distribution for supported zeolite membranes

The permporometry measurements are performed with respect to a series of zeolite membranes with different defect sizes, which can be further applied for in situ measurement of the defect size distribution in zeolite membranes. Gas permeation experiments are conducted for CO₂/N₂ gas mixture to test the separation performance of the studied zeolite membranes. By taking into account the “t-layer” on defect walls, a mathematical model and the corresponding procedure are developed so that the defect size distribution in zeolite membranes can be calculated by using the results of permporometry measurements. The defect size distribution and the maximal defect size show a good correlation with the separation performance of CO₂/N₂ gas mixture for zeolite membranes. It is demonstrated that the separation performance of zeolite membranes is mainly determined by large defects. It has been shown that the permporometry-based methodology proposed in this contribution is an effective way for the quality evaluation of zeolite membranes.     

Trends in speciation analysis of vanadium in environmental samples and biological fluids--a review

A comprehensive review is presented addressing recent trends in the speciation and determination of vanadium in environmental and biological sample matrices, including important analytical aspects such as sample clean up, pre-concentration and method development. Methodology based on both separation and spectroscopic techniques for the determination of vanadium speciation is discussed. A brief outline of analytical principles, together with an overview of the recent developments and applications of vanadium speciation determination is included. The newer methods for detecting metal ions including hyphenated spectroscopic techniques and sample preparation schemes are also discussed.     

Modern Methods of Pre-Treatment of Plant Material for the Extraction of Bioactive Compounds

In this review, recent advances in the methods of pre-treatment of plant material for the extraction of secondary metabolites with high biological activity are presented. The correct preparation of the material for extraction is as important as the selection of the extraction method. This step should prevent the degradation of bioactive compounds as well as the development of fungi and bacteria. Currently, the methods of preparation are expected to modify the particles of the plant material in such a way that will contribute to the release of bioactive compounds loosely bonded to cell wall polymers. This review presents a wide range of methods of preparing plant material, including drying, freeze-drying, convection drying, microwave vacuum drying, enzymatic processes, and fermentation. The influence of the particular methods on the structure of plant material particles, the level of preserved bioactive compounds, and the possibility of their release during the extraction were highlighted. The plant material pre-treatment techniques used were discussed with respect to the amount of compounds released during extraction as well their application in various industries interested in products with a high content of biologically active compounds, such as the pharmaceutical, cosmetics, and food industries.     

Advances in passive sampling in environmental studies

Passive sampling is based on the phenomenon of mass transport due to the difference between chemical potentials of analytes in a given environmental compartment and the collection medium inside a dosimeter. The subsequent laboratory procedure (i.e. extraction, identification and determination of analytes) is the same as in the case of classic sampling techniques.Passive sampling techniques are characterized by simplicity with regard to the dosimeter's construction as well as its maintenance. Therefore, they find ever increasing application in the field of environmental research and analytics. When choosing a passive sampling method, one should not forget that some passive samplers require the time-consuming calibration step before being used in the field.Novel solutions and modifications of existing sampler designs have been presented. Practical application of passive dosimetry in environmental analytics, including sampling of water, soil, air and other atypical media are discussed. Some aspects of calibration methods in passive dosimetry are also described. The latest trends in the application of passive sampling are highlighted.     

燃料电池Pt基核壳结构电催化剂的最新研究进展

综述了用于燃料电池的Pt基核壳结构电催化剂的制备方法和表征方法的最新研究进展.首先,详细介绍了核壳结构催化剂的制备方法,主要包括胶体法、电化学法和化学还原法等.其中胶体法的应用最为广泛,制备过程简单易控;电化学法和化学还原法在最近几年得到了迅速发展,并有望用于核壳结构电催化剂的批量化生产.其次,简单阐述了核壳结构电催化剂特用的表征方法.其中高角度环形暗场-扫描透射电子显微镜是近年来发展的一种新技术,它利用暗场强度与原子序数的比例关系可以有效地表征核壳电催化剂的特殊结构.最后,总结了存在的问题并展望了可能的发展方向.     

自组装方法与三维光子晶体制作

光子晶体,特别是三维光子晶体,可能成为信息处理和通信等领域的新型功能材料.光子晶体的制作方法可分为"自上而下"的物理方法和"自下而上"的化学自组装方法.化学自组装方法是制作三维光子晶体最为经济有效的方法.本文在阐述自组装方法的种类、一般过程、优点和不足等内容的基础上,分别分析和总结了带有各种功能缺陷的三维光子晶体的制作,这些缺陷主要包括线缺陷、面缺陷和点缺陷.从研究中可以看出,化学自组装方法通常需要结合其他方法才能实现缺陷的嵌入.近些年,三维光子晶体制作在材料选取、结构设计和方法改进等方面都有一些最新进展,本文对此进行了较为详尽的评述,并对我们课题组的研究进行了总结.最后对光子晶体的研究和制作方向进行了展望.     

Soil SO-1 reference material for trace analysis

Summary The preparation of soil SO-1 reference material is described as well as an evaluation of the results provided by 30 laboratories for 41 elements, including outlier rejection step by four concurrent tests. The influence of different chemical pretreatment methods preceding various instrumental analytical techniques is also discussed. Based on the numbers of outliers, confidence limits and numbers of different analytical methods used for a given element some criteria for the classification of the results are proposed.

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Referenzmaterial Soil SO-1 für die Spurenanalyse

     

基于色谱-质谱联用的脂质分析样品前处理技术研究进展

脂质作为细胞膜和亚细胞膜的主要结构成分,在能量来源、细胞信号传导等多种生物学过程中发挥着重要作用。近年来,脂质分析受到越来越多的关注,其中色谱-质谱联用技术在脂质分析中占据主导地位。由于样品基质复杂,样品前处理有富集痕量物质和减少基质干扰的作用,成为脂质分析中的一个关键步骤。该文综述了近年来基于色谱-质谱联用技术的脂质分析中样品前处理技术的研究进展和应用,对各种样品前处理技术进行了阐述和总结。基于液相的萃取方法有液-液萃取和单一有机溶剂萃取。基于固相的萃取方法包括固相萃取和固相微萃取。场辅助萃取方法包括超临界流体萃取、加压流体萃取、微波辅助萃取和超声辅助萃取。此外,还介绍了在线联用样品前处理方法和用于活体分析的样品前处理方法。最后,对基于色谱-质谱联用的脂质分析样品前处理技术存在的问题及发展趋势进行了探讨。样品前处理技术的发展将提高脂质分析的灵敏度、选择性和分析速度。     

Analytical Methods for Determination of Non-Nutritive Sweeteners in Foodstuffs

Sweeteners have been used in food for centuries to increase both taste and appearance. However, the consumption of sweeteners, mainly sugars, has an adverse effect on human health when consumed in excessive doses for a certain period, including alteration in gut microbiota, obesity, and diabetes. Therefore, the application of non-nutritive sweeteners in foodstuffs has risen dramatically in the last decade to substitute sugars. These sweeteners are commonly recognized as high-intensity sweeteners because, in a lower amount, they could achieve the same sweetness of sugar. Regulatory authorities and supervisory agencies around the globe have established the maximum amount of these high-intensity sweeteners used in food products. While the regulation is getting tighter on the market to ensure food safety, reliable analytical methods are required to assist the surveillance in monitoring the use of high-intensity sweeteners. Hence, it is also necessary to comprehend the most appropriate method for rapid and effective analyses applied for quality control in food industries, surveillance and monitoring on the market, etc. Apart from various analytical methods discussed here, extraction techniques, as an essential step of sample preparation, are also highlighted. The proper procedure, efficiency, and the use of solvents are discussed in this review to assist in selecting a suitable extraction method for a food matrix. Single- and multianalyte analyses of sweeteners are also described, employing various regular techniques, such as HPLC, and advanced techniques. Furthermore, to support on-site surveillance of sweeteners’ usage in food products on the market, non-destructive analytical methods that provide practical, fast, and relatively low-cost analysis are widely implemented.     

Electronic structure of highly conducting conjugated polymers: evolution upon doping of polyacetylene, polythiophene, and polyemeraldine

The electronic properties of three types of conducting polymers: trans-polyacetylene (proto-typical of systems with a degenerate ground state), polythiophene (as an example of compounds with a nondegenerate ground state), and polyemeraldine (which can be doped via protonation) are reviewed. The structural and electronic band structure properties of these systems are studied at various defect concentrations corresponding to undoped, lightly doped, and highly doped polymers. Geometry optimizations of oligomeric equivalents to the undoped and doped polymers are performed using the semi-empirical MNDO and AM1 methods. The electronic band structures are calculated using the VEH method. The interpretation of the optical absorption data is discussed in terms of interband transitions; for doped trans-polyacetylene including soliton defects and for doped polythiophene including bipolaron defects. For highly doped trans-polyacetylene and polythiophene as well as for protonated polyemeraldine, the electronic structure of a polaron lattice conformation is discussed and shown to be in agreement with existing optical and magnetic data on these polymers.     

Total synthesis of novel 6-substituted lavendamycin antitumor agents

[structure: see text] Novel 6-substituted lavendamycins have been synthesized for the first time. The key step in these syntheses is a Pictet-Spengler condensation (Scheme 1). Efficient methods for the synthesis of each compound, including a novel reaction for the facile introduction of alkylamino groups at the C-6 position of the lavendamycin system, are discussed. Possible mechanisms for these reactions are also presented.     

Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.     

Current analytical methods for plant auxin quantification – A review

Plant hormones, and especially auxins, are low molecular weight compounds highly involved in the control of plant growth and development. Auxins are also broadly used in horticulture, as part of vegetative plant propagation protocols, allowing the cloning of genotypes of interest. Over the years, large efforts have been put in the development of more sensitive and precise methods of analysis and quantification of plant hormone levels in plant tissues. Although analytical techniques have evolved, and new methods have been implemented, sample preparation is still the limiting step of auxin analysis. In this review, the current methods of auxin analysis are discussed. Sample preparation procedures, including extraction, purification and derivatization, are reviewed and compared. The different analytical techniques, ranging from chromatographic and mass spectrometry methods to immunoassays and electrokinetic methods, as well as other types of detection are also discussed. Considering that auxin analysis mirrors the evolution in analytical chemistry, the number of publications describing new and/or improved methods is always increasing and we considered appropriate to update the available information. For that reason, this article aims to review the current advances in auxin analysis, and thus only reports from the past 15 years will be covered.     

A review of separation methods for the determination of estrogens and plastics-derived estrogen mimics from aqueous systems

Recent methods of separation and detection for the quantification of trace-level concentrations of selected endocrine disrupting compounds (EDCs) from aqueous systems are reviewed. A brief introduction of the selected EDCs (natural and synthetic estrogens and plastics-derived xenoestrogens), including their characteristics and importance, is presented. Sample preparation and extraction trends are discussed. Various types of separation techniques are presented, with the express goal of emphasizing time and cost-effective methods that isolate and quantify trace-levels of multiple endocrine disruptors from aqueous systems.     

Automatic estimation of pressure-dependent rate coefficients

A general framework is presented for accurately and efficiently estimating the phenomenological pressure-dependent rate coefficients for reaction networks of arbitrary size and complexity using only high-pressure-limit information. Two aspects of this framework are discussed in detail. First, two methods of estimating the density of states of the species in the network are presented, including a new method based on characteristic functional group frequencies. Second, three methods of simplifying the full master equation model of the network to a single set of phenomenological rates are discussed, including a new method based on the reservoir state and pseudo-steady state approximations. Both sets of methods are evaluated in the context of the chemically-activated reaction of acetyl with oxygen. All three simplifications of the master equation are usually accurate, but each fails in certain situations, which are discussed. The new methods usually provide good accuracy at a computational cost appropriate for automated reaction mechanism generation.     

Transition levels of defects in ZnO: Total energy and Janak's theorem methods

Transition levels of defects are commonly calculated using either methods based on total energies of defects in relevant charge states or energy band single particle eigenvalues. The former method requires calculation of total energies of charged, perfect bulk supercells, as well as charged defect supercells, to obtain defect formation energies for various charge states. The latter method depends on Janak's theorem to obtain differences in defect formation energies for various charge states. Transition levels of V(Zn), V(O), and V(ZnO) vacancy defects in ZnO are calculated using both methods. The mean absolute deviation in transition level calculated using either method is 0.3 eV. Relative computational costs and accuracies of the methods are discussed.     

The role of synchrotron radiation in examining the self-assembly of crystalline nanoporous framework materials: from zeolites and aluminophosphates to metal organic hybrids

This tutorial review describes the role of synchrotron-based techniques in the study of the formation of Crystalline Nanoporous Framework Materials (CNFMs), such as zeolites, aluminophosphates (AlPOs) and metal organic frameworks (MOFs). Initially, a general formation process for CNFMs is described and the 'tool kit' (including synchrotron and non-synchrotron-based techniques) used to examine this complex process is presented. The need for realistic in situ conditions and the balance between this, data quality and time resolution, are also discussed with reference to commonly utilized in situ synchrotron-based experimental cells. The experimental studies into the formation of several CNFM systems are then examined and the role of the synchrotron-based experiments, in context with those obtained from other techniques, is discussed. From this the importance of the synchrotron-based technique is demonstrated, however it is also shown that, to obtain a more complete understanding of the formation process, complementary independent measurements are still often required. During these discussions some of the most common experimental techniques and analytical methods are also discussed in detail and critically assessed.