ICP-AES中基体干扰效应及其机理研究——Ⅰ.基体干扰效应的一般分布规律

本文以Na、ca、Al、Zn作为主要基体元素,在不同ICP发射光谱仪上考察了20多条分析谱线受到的干扰情况,初步总结了基体干扰效应的一般规律。结果表明,在常用分析条件下,一般金属元素具有与易电离元素类似的基体效应,即在较低观察区域对测定谱线信号产生增感,而在正常观察区域产生抑制;从增感转向抑制的零干扰点主要出现在感应圈上方8～14mm的观察区域,这一结果为实际分析条件的优化提供了有益的依据。     

Low Pass metallic mesh interference filters for operation in the 165 GHz to 880 GHz region

Low Pass metallic mesh interference filters have been designed and constructed for operation in the region 340 m (880 GHz) to 1.8 mm (165 GHz). These filters have been shown to have excellent edge characteristics and good rejection regions. The results show that the mesh filter can be effectively used in both millimetre and submillimetre regions.Part of this work was performed while this author was at Heriot-Watt University, Edinburgh, U.K.     

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。     

Mode selective directional couplers for overmoded waveguide systems

Two types of directional couplers for transverse electric (TE) modes are described: short and multihole couplers, respectively. They selectively pick one mode out of a mode mixture in an overmoded circular waveguide system. Unwanted modes are either statistically kept at low level or are suppressed by destructive interference in the coupling waveguide. Mode selectivity and directivity in multihole couplers oscillate up and down with an increasing number of holes, finally reaching a minimum of approximately 20 dB, unless there are competing modes with rational fractions of the beat wavelength. A multihole coupler for the TE₀₂ mode (28 GHz, 63.4 mm waveguide diameter, 41 holes) and a length of 1.6 m shows a calculated directivity of 68 dB and suppresses the unwanted modes TE₀₁ with 34 dB (24 dB), TE₂₂ with 37 dB (45 dB), and further modes TE_m (<5, m<6) with 17 dB to 34 dB in forward direction (figures in parentheses are for unwanted modes propagating in backward direction).A short directional coupler for the TE₀₁ mode (28 GHz, 63.4 mm waveguide diameter) with 16 holes and a length of 230 mm shows a directivity of 55 to 100 dB between 27.9 and 28.1 GHz, suppressing the TE₀₂ mode with 35 to 80 dB, the TE₀₃ mode with 30 to 65 dB, and the TE₂₂ mode with 30 to 70 dB.     

Recent development of non-faradaic potentiometry

Non-faradaic potentiometry has been plagued by a great many fundamental errors and a lack of conceptualization. Of greatest concern is the second Nernst equation hiatus. Potentiometry may be generally classified as faradaic and non-faradaic. The former deals with the redox reactions using the Nernst equation to explain the potential origin. The latter deals with the non-redox reactions using the Boltzmann and modified Boltzmann equations to explain the origin of electrode potential. Redox faradaic potentiometry has been well described in the textbooks. However, non-faradaic potentiometry has been almost completely neglected in the literature. Many well-known electrodes, such as the pH glass electrode, common reference electrodes, and ion selective electrodes (ISE) have been mistakenly interpreted as redox reactions or ion exchange reactions. New theories and experimental results show their mechanisms to be non-faradaic in nature. Furthermore, the reaction mechanisms for ISE have been confused in textbooks with redox reactions and the Nernst equation. The ISE potentials originating from adsorption of ions or charged particles based on surface charge density will be explained using the double and counterion triple layers concept. The new counterion triple layer concept may be applied to the potential development of sensors. The reason for a new concept, theory, or mechanism is to better explain the phenomena. Examples will be given of how our new concept explains the capacitor, counterion triple layer, surface adsorbed layers interactions, and the interface structure. We will also discuss the new sensor development based on the new adsorption concept. For the first time a new type of Ag/AgCl reference electrode for non-faradaic potentiometry will be presented, one without a liquid junction and with a Pt wire instead of a salt bridge. They will help open up a new horizon for electrochemical sensor research and may be used under unusual conditions, such as high temperature and high pressure, stirring, etc.     

用于测量亚硝酸的长光程吸收光谱仪的研制

This article has been retracted at the request of the authors.     

Effects of ion-pairing reagents on the electrospray signal suppression of sulphonated dyes and intermediates

High-performance liquid chromatography/mass spectrometry (HPLC/MS) analysis of anionic species such as sulphonic acid dyes and intermediates requires volatile ion-pairing mobile phase additives. Six di- and trialkylammonium acetates were compared with tetraalkylammonium salts and ammonium acetate in the concentration range 0-20 mmol l(-1) as mobile phase additives for HPLC/MS of polysulphonated compounds. The effects of the structure and concentration of the ion-pairing reagents on the electrospray response of mono-, di- and tetrasulphonic aromatic acids and acid dyes were studied in detail. Further, five different mass analysers and instrument geometries were compared. A higher signal decrease is observed with linear geometry instruments in comparison to orthogonal or even Z-spray geometry mass spectrometers. The concentration of mobile phase additives has a significant influence on the abundance ratios of multiply charged ions in the mass spectra of polysulphonated compounds. The competing ions of sulphonic acids may also cause significant signal suppression.     

退火温度对KDP晶体光学均匀性的影响研究

 研究了磷酸二氢钾（KDP）晶体热退火前后光学均匀性的变化，发现适当温度下退火可以降低KDP晶体的内应力，提高晶体的消光比，从而提高晶体的光学均匀性。实验证明，50℃下退火即可消除部分内应力，110℃下退火可以消除生长鬼影和鬼线。但是,退火温度太高（如170℃）,也可能使晶体的均匀性降低。     

Computer Controlled AAS Scanning Method to Study Flame Atomization Processes

By slightly changing the optical and burner systems of the conventional atomic absorption spectrometer, a computer controlled scanning method has been developed, which enables us to get a picture of absorbance distribution over the entire cross section of the analytical flames quickly, reproducibly and in high resolution. The plotting of different distribution functions obtainable by computerized data processing and the conclusions drawn from them are illustrated with some examples of flame atomization of cobalt and magnesium salts. The newly discovered method, by its reliability and little demand on time, allows the extension of the general applicability of AAS in revealing analytical interference effects and in the study of flame-chemical processes.     

Investigation into the structural composition of hydroalcoholic solutions as basis for the development of multiple suppression pulse sequences for NMR measurement of alcoholic beverages

An eight‐fold suppression pulse sequence was recently developed to improve sensitivity in ¹H NMR measurements of alcoholic beverages [Magn. Res. Chem. 2011 (49): 734–739]. To ensure that only one combined hydroxyl peak from water and ethanol appears in the spectrum, adjustment to a certain range of ethanol concentrations was required. To explain this observation, the structure of water–ethanol solutions was studied. Hydroalcoholic solutions showed extreme behavior at 25% vol, 46% vol, and 83% vol ethanol according to ¹H NMR experiments. Near‐infrared spectroscopy confirmed the occurrence of four significant compounds (‘individual’ ethanol and water structures as well as two water–ethanol complexes of defined composition – 1 : 1 and 1 : 3). The successful multiple suppression can be achieved for every kind of alcoholic beverage with different alcoholic strengths, when the final ethanol concentration is adjusted to a range between 25% vol and 46% vol (e.g. using dilution or pure ethanol addition). In this optimum region, an individual ethanol peak was not detected, because the ‘individual’ water structure and the 1 : 1 ethanol–water complex predominate. The nature of molecular association in ethanol–water solutions is essential to elucidate NMR method development for measurement of alcoholic beverages. The presented approach can be used to optimize other NMR suppression protocols for binary water–organic solvent mixtures, where hydrogen bonding plays a dominant role. Copyright © 2014 John Wiley & Sons, Ltd.