Analysis and proposition of limiting current density measurement protocol

Limiting current density at different temperatures, backpressures, and balance gases can be used to separate molecular diffusion resistance, Knudsen diffusion resistance and local transport resistance of membrane electrode assembly (MEA). However, the measurement of limiting current density has no unified protocol. The diverse choices in the literature, either in the control of current or voltage or in the atmosphere like relative humidity and O₂ concentrations, make it difficult to compare the results and identify the true bottleneck hindering the mass transport. In this work, the current-voltage curves obtained by current scanning/stepping and voltage scanning/stepping methods under dilute O₂ of different concentrations and a wide range of relative humidity were measured and analyzed systematically. It is found that the voltage stepping method is superior to the other three ways of control for the reliable determination of the limiting current density. Aided with simultaneous electrochemical impedance spectroscopy measurement, the limiting current density can be determined with pinpoint accuracy. When the limiting current density is just used to qualitatively evaluate different MEA, the voltage scanning method can be used instead for its high time efficiency. The selection of the atmosphere also plays an important role in suppressing the distortion from excessive water and reducing the spurious contribution from proton conduction resistance. It is found that O₂ concentrations at 0.5 vol% and relative humidity at 90% can give the best estimation of O₂ transport resistance in membrane electrode assembly.     

催化共振光散射法测定空气中痕量甲醛的研究

吖啶橙分子聚集体微粒可在513nm波长处出现最大的共振光散射强度(RLS)。在稀硫酸介质中,甲醛能催化溴酸钾氧化吖啶橙的反应,促使其RLS强度减弱。在最佳实验条件下,甲醛质量浓度ρ在0.020～0.25μg/mL的范围内与△I值呈良好的线性关系,线性回归方程为△I=1113.99ρ+49.23,线性相关系数r为0.9986。本法与国标法进行对照,在置信度等于95%时,用Cochran检验,两种方法间不存在显著性差异,方法操作简单、灵敏度高,用于室内外空气中甲醛测定,结果满意。     

亲水作用色谱-串联质谱法测定动物源运动食品中3种氨基糖苷类抗生素的残留量

该研究建立了一种亲水交互作用色谱-串联质谱（HILIC-MS/MS）法测定动物源运动食品中潮霉素B、新霉素、安普霉素3种氨基糖苷类抗生素残留量的方法。结果表明，样品经Sielc Obelisc R柱分离，采用0.1%甲酸水溶液-乙腈梯度洗脱，可以实现3种目标物组分的分离。在此条件下，3种氨基糖苷类抗生素在5～500 ng/mL的质量浓度范围内线性关系良好，相关系数R2为0.999 5～0.999 9，检出限均为15 μg/kg，定量限均为50 μg/kg，保留时间的日间和日内相对标准偏差（RSD）分别为3.5%～7.9%和3.5%～4.1%，峰面积的日间和日内RSD分别为3.6%～7.4%和3.2%～3.9%，加标回收率为85.7%～93.6%，回收率试验结果的RSD为3.1%～5.2%。该方法可以满足动物源运动食品中3种氨基糖苷类抗生素的检测需求。     

应用膨胀算法提取目标的直接定位算法

为了解决被动雷达系统中的多发射源定位问题，提出了一种基于多重信号分类(MUSIC)算法和图像膨胀(IE)算法的直接定位方法。该方法结合了谱分析中的MUSIC思想，通过对接收量测协方差矩阵进行特征分析求解目标的位置。首先，在目标个数未知的前提下，利用Akaike信息准则(AIC)来确定模型阶数；然后，推导了基于MUSIC的定位代价函数；之后，利用图像膨胀算法处理得到的代价函数平面；最后，膨胀处理后的输出为目标个数及目标位置的估计值。提出的算法有效地解决了目标检测及提取的问题，能够确定多个目标的位置坐标，为后续的定位性能分析提供可能性，也保证了算法的完整性。进一步地分析了多个临近目标情况下影响目标提取性能的主要因素。     

Deposition of UF5 on the surface of steel material having oxide coating in contact with gaseous UF6

When UF6 is handled in leak tight system, the amount of uranium compound formed on the surface of containers, valves, and others in UF6 handling facilities is not so significant for a short term that special attention has not been given to this problem. The present work was done to throw some more light on this problem based on the recent experiment. We discuss the possibility that the intermolecular transfer of a fluorine atom from UF6 to UF5 may participate in the formation of uranium compound. The discussion includes also the unique features contained in the experimental result, the reaction processes assumed in this problem, and the derivation of a rate equation for expressing the deposition of uranium compound. Furthermore, we propose a new method for determining nonlinear parameters included in a governing differential equation having two variables for expressing the deposition of uranium compound from experimental raw data.     

液相色谱-串联质谱法测定豆类中左旋多巴

文章建立一种豆类中左旋多巴的液相色谱-串联质谱测定方法。样品经0.3 mol/L乙酸水溶液超声提取,Agilent Proshell 120 SB-C18(2.1 mm×150 mm,2.7μm)色谱柱分离,以0.1%甲酸水-甲醇为流动相进行梯度洗脱,多反应监测(MRM),内标法定量。结果表明,左旋多巴在0.1~5.0 mg/L范围内线性关系良好,相关系数为0.9994,检出限为1.5 mg/kg,定量限为5.2 mg/kg,方法的平均加标回收率为96.9%~105.5%,日内精密度和日间精密度均小于4%,具有操作简单、灵敏度高、准确度高、重现性好等特点,能够很好满足豆类中左旋多巴含量的检测需要。     

卡系费休法测定氯乙烯单体中水含量的影响因素

介绍了卡尔费休法的测定原理,具体分析了采用卡尔费休法测定氯乙烯单体中水含量的影响因素,指出采用闪蒸仪进样器,能有效提高分析结果的准确性和工作效率。     

温度和放散空间体积对等容变压法测定瓦斯放散初速度的影响分析

在煤矿煤与瓦斯突出防治工作中，瓦斯放散初速度（ΔP）是一个重要的指标。通过资料对比、理论分析、实验研究对瓦斯放散初速度测定中温度、放散空间体积等对测定的影响进行了研究。研究表明瓦斯放散初速度在煤样一定的情况下与放散空间体积和实验温度有关。随着温度的升高，瓦斯放散初速度减小，减小的幅度和煤样自身的瓦斯放散初速度大小有关。放散空间体积越大，瓦斯放散初速度越小；不同煤样放散空间体积对瓦斯放散初速度影响不同。建议瓦斯放散初速度测定应在恒定温度下进行，实验温度建议与井下温度相同，仪器的放散空间体误差应小于1 mL。