A procedure for sampling and analysis of air for energetics and related compounds

A procedure for the sampling and analysis of energetics and related compounds in the atmosphere is described. The basic procedure consists of the collection of air samples using sampling cartridges containing XAD-2 resin, extraction of the resin with isoamyl acetate, and an analysis of the extract using gas chromatography with electron capture detection. Modifications and additions to this procedure are discussed, such as the use of a prefilter before the resin sampler to collect particulates and the use of a mass selective detector to analyze for some propellant compounds of interest or for quantitative confirmation purposes. Two differing sizes of samplers are evaluated according to the air volumes required for collection. The procedure is tested through the analysis of spiked resin samples, which had air pulled through them for periods of time corresponding with the required sampling volumes. This procedure has application toward the measurement of energetic residues in atmospheres resulting from weapons testing and operations during training exercises involving munitions.     

Guidelines for CITAC projects and CITAC procedure for support of conferences and workshops

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Guidelines for CITAC projects and CITAC procedure for support of conferences and workshops     

Possibilities for separation and simultaneous determination of N-unsubstituted- and N-substituted nitroimidazoles and criteria for their identification

The N-unsubstituted nitroimidazoles have an imino hydrogen atom in contrast to the N-substituted derivatives, and react with hydroxide to give the yellow nitroimidazole anions. The difficulty of reducing the nitro-group in these anions, together with the shift of the absorption maximum to longer wavelengths makes it possible to analyse polarographically or spectrophotometrically a mixture of N-unsubstituted nitroimidazole with N-substituted derivatives. The presence of the N-unsubstituted nitroimidazole and the N-substituted derivatives is first established by chromatography. Other criteria are also proposed for distinguishing between these substances.     

Photocaging strategy for functionalisation of oligonucleotides and its applications for oligonucleotide labelling and cyclisation

We have used a photocaging strategy to develop novel phosphoramidites and expand the repertoire of protecting groups for modification of oligonucleotides by solid-phase synthesis. We synthesised five photolabile phosphoramidites and four new photolabile controlled pore glasses (CPGs). By using these photolabile phosphoramidites and CPGs, modified oligodeoxynucleotides (ODNs) with phosphate, amine, acid, thiol and carbonyl moieties at 5' and/or 3' ends were readily synthesised. To the best of our knowledge, this is the first report of introducing a carbonyl at the 5' end and thiol groups at both ends of ODNs with photolabile modifiers. Terminal labelling was also easily realised in solution or by on-column solid-phase synthesis. By using the photolabile amine modifier and the photolabile acid CPG, cyclisation of an oligodeoxynucleotide was achieved with good yields. This study provides an alternative way to introduce functional groups into oligonucleotides and expand the scope of oligonucleotide bio-orthogonal labelling.     

Rapid potentiometric methods for vanadium and for analysis of ferrovanadium and some vanadium steels

Rapid and reliable potentiometric methods are given for determination of vanadium based on titrating unreacted KBr or KI in H₂SO₄ acid medium with Hg(I) or Hg(II), using silver amalgam as the indicator electrode. The methods are successfully applied to the analysis of ferrovanadium, three varieties of vanadium steels and synthetic mixtures of about identical constitution. In all cases the potential breaks were sharp enough for the accurate determination of the end points.     

Techniques and procedures for preparation of aquatic samples for chromatographic analyses

The measurement of low levels of organic compounds in environmental samples presents the researcher with a number of possible pathways to effectively obtain and analyze samples. Numerous sampling methods, sample preparation techniques, and extraction procedures are available. A number of different approaches to sampling strategy, isolation, concentration, cleanup and fractionation will be discussed. Objectives for collecting environmental samples differ from those for many other types of samples because reliable measurements at very low levels are frequently required. Often, specific analytes need to be measured at the μg/kg and even ng/kg levels in complex matrices. Advances in analytical methodology continue to lower the levels at which reliable measurements can be made. At these levels, many factors that are of little or no concern in other analytical measurements are of critical importance in influencing the outcome and reliability of environmental analyses. Analytical measurements are used for determining the composition and the quantities of analytes in the defined system at various concentration levels. Environmental analytical measurements provide data about the transportation and transformation of an environmental contraminant and for determination of its concentration in a sample.     

Studies for simultaneous quantitative electrodeposition of plutonium and americium for alpha-spectrometry

For high resolution alpha-spectrometric studies, the sources of alpha-emitting actinides are generally prepared by electrodeposition. Usually, by electrodeposition of only one element can be achieved quantitatively. A method was developed for the simultaneous quantitative electrodeposition of plutonium and americium, in two hours using 0.005M oxalic acid with saturated ammonium chloride. The alpha-spectral characteristics of sources prepared by this method were better than those prepared by the drop deposition method. This electrodeposition procedure was validated with nuclear fuel samples containing plutonium and americium.     

Reaction kinetics and mechanism for hydrothermal degradation and electrolysis of glucose for producing carboxylic acids

Electrolysis in subcritical water can convert biomass-derived saccharides into value-added chemicals and fuels without any additives. In this work, we aim to understand reaction behaviours of glucose under subcritical water degradation or electrochemical conditions for the purpose of developing a new method for producing useful carboxylic acids. Degradation of glucose was carried out using a continuous flow-type reactor in subcritical water at various operating conditions, and electrochemical reactions of their product solutions were conducted at identical conditions with a 500-mL batch autoclave. Gaseous products obtained were analyzed by gas chromatography-thermal conductivity detection (GC-TCD), and liquid products were analyzed by high-performance liquid chromatography (HPLC) and gas chromatography-flame ionization detection (GC-FID). The total organic carbon (TOC) in the aqueous product solution was determined by using a TOC analyzer. Based on the experimental results, a reaction pathway for glucose is proposed for subcritical water degradation and electrolysis.     

Homotherapy for heteropathy active components and mechanisms of Qiang-Huo-Sheng-Shi decoction for treatment of rheumatoid arthritis and osteoarthritis

Qiang-Huo-Sheng-Shi decoction (QHSSD), a classic traditional Chinese herbal formula, which has been reported to be effective in rheumatoid arthritis (RA) and osteoarthritis (OA). However, the concurrent targeting mechanism of how the aforementioned formula is valid in the two distinct diseases OA and RA, which represents the homotherapy-for-heteropathy principle in traditional Chinese medicine (TCM), have not yet been clarified. In the present study, network pharmacology was adopted to analyze the potential molecular mechanism, and therapeutic effective components of QHSSD on both OA and RA. A total of 153 active ingredients in QHSSD were identified, 142 of which associated with 59 potential targets for the two diseases were identified. By constructing the protein-protein interaction network and the compound-target-disease network, 72 compounds and 10 proteins were obtained as the hub targets of QHSSD against OA and RA. The hub genes of ESR1, PTGS2, PPARG, IL1B, TNF, MMP2, IL6, CYP3A4, MAPK8, and ALB were mainly involved in osteoclast differentiation, the NF-κB and TNF signaling pathways. Moreover, molecular docking results showed that the screened active compounds had a high affinity for the hub genes. This study provides new insight into the molecular mechanisms behind how QHSSD presents homotherapy-for-heteropathy therapeutic efficacy in both OA and RA. For the first time, a two-disease model was linked with a TCM formula using network pharmacology to identify the key active components and understand the common mechanisms of its multi-pathway regulation. This study will inspire more innovative and important studies on the modern research of TCM formulas.     

小分子有机电致发光器件和材料的研究及应用

有机电致发光器件(OLED)是在电场作用下,以有机材料为活性发光层的器件.由于OLED具有亮度高、响应快、视角宽、工艺简单、可柔性等优点,在现代科学研究及技术应用中备受关注.其商业化应用,诸如平板显示(FPD)和固体照明(SSL)等,正在不断向前推进.本文综述了小分子OLED的各种器件结构和功能材料研究进展以及该领域存...     

Material issues for construction of organic and polymeric driving circuits for display and electronic applications

Organic and polymeric driving circuits may be a possible alternative to realize low cost flexible and large area flat panel displays. Recent efforts have been directed to the discovery of solution processable polymeric semiconductors for the ease of fabrication and low cost. In this paper, we report the investigation of various 3‐substituted regioregular polythiophenes as active semiconductors for field‐effect transistors. The best transistor performance has been found with regioregular poly(3‐heaxylthiophene). The difference in their device performance was correlated to the structure and morphological behavior of these regioregular polythiophenes.     

Determination of molar absorptivity coefficients for major type-B trichothecenes and certification of calibrators for deoxynivalenol and nivalenol

This paper presents results from the European Commission-funded project Doncalibrant, the objective of which was to produce calibrators with certified mass fractions of the Fusarium toxins deoxynivalenol (DON), 3-acetyldeoxynivalenol (3-Ac-DON), 15-acetyldeoxynivalenol (15-Ac-DON), and nivalenol (NIV), in acetonitrile. The calibrators, available in ampoules, were sufficiently homogeneous, with between-bottle variations (s _bb) of less than 2%. Long-term stability studies performed at four different temperatures between −18 and 40 °C revealed no significant negative trends (at a confidence level of 95%). Molar absorptivity coefficients (in L mol⁻¹ cm⁻¹) were determined for all four toxins (DON: 6805 ± 126, NIV: 6955 ± 205, 3-Ac-DON: 6983 ± 141, 15-Ac-DON: 6935 ± 142) on the basis of a mini-interlaboratory exercise. The overall uncertainty of the calibrators’ target values for DON and NIV were evaluated on the basis of gravimetric preparation data and include uncertainty contributions from possible heterogeneity, storage, and transport. The Doncalibrant project resulted in the production of calibrators for DON (IRMM-315) and NIV (IRMM-316) in acetonitrile with certified mass fractions of 25.1 ± 1.2 μg g⁻¹ and 24.0 ± 1.1 μg g⁻¹, respectively. Both CRMs became commercially available from the Institute for Reference Materials and Measurements (IRMM, Geel, Belgium) at the beginning of 2007.     

Simple and rapid methods for on-site determination of radon and thoron in soil-gases for seismic studies

The determination of soil-gas anomalies especially ²²²Rn anomalies, are important to precisely locate fault traces, as well as to investigate earthquake precursors. In this paper, we have studied and compared new rapid methods for on site determinations of radon (²²²Rn), thoron (²²⁰Rn) and total radon (²²²Rn+²²⁰Rn) in soil-gas. These new techniques pump the soil-gas continuously from the soil through a simple sampling tube to the counting cell for one-minute with discarding the excess. Then, either four one-minute counting periods (5-minute technique) or nine one-minute counting intervals (10-minute technique) are followed immediately. In all the methods, conversely to Morse"s method, the first counting period (C1) was not employed for calculations. Three calculation methods for the five-minute technique, two for the ten-minute technique and a modified Morse"s method are compared with theoretical values and different real soil-gases with different radon/thoron ratios. The affect of different flow rates of soil-gases into the counting cell was also investigated. Finally, the ten-minute technique seems to be a little more accurate, but the 5-minute technique is much more suitable for seismic field studies when a much larger number of determinations are required in a short time.     

引言

正分离性能优异的色谱技术是现代分离测定的重要手段,在食品、药品、医疗、化工、环境、生物技术等领域获得了广泛应用,尤其在食品领域,被称为食品安全检测的最佳利器。由于食品基质复杂、有害物种类繁多、含量范围宽泛等特征,加之有害物结构与形态变化多样、代谢情况复杂,为食品分析带来极大的挑战。近年来,随着色谱、质谱、化学计量学、材料学与生物技术等学科的不断交叉发展,新型分离技术及装置、新型固定相、新型富集净化材料、新型质谱联用技术等不断涌现,为色     

Shortcut method for evaluation and design of a hybrid process for enantioseparations

Hybrid processes for enantioseparations have a considerable potential for reducing investment and operational costs. An example is the combination of simulated moving bed (SMB) chromatography and selective crystallisation. However, the design of integrated processes is a difficult task. A shortcut method is presented that can serve as a tool for design and estimation of the potential of such processes. The approach requires only limited experimental data and thus allows for systematic parameter studies. The method is based on the determination of the purity-performance characteristic of the SMB process and rigorous application of mass balances. The use of relative mass fluxes allows derivation of simple algebraic expressions for essential process parameters. The significant potential of combining SMB and crystallisation is demonstrated for the example of the separation of mandelic acid enantiomers.