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.     

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。     

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.     

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。     

Optimised phase compositions and improved microwave dielectric properties based on calcium tin silicates

The Ca_(1+2y)Sn_(1-x)Si_(1+y)O_(5-2x+4y) low-permittivity microwave dielectric ceramics were prepared through solid-state reaction at 1350–1450 °C for 5 h. The relations between microwave dielectric properties and phase compositions for non-stoichiometric Ca_(1+2y)Sn_(1-x)Si_(1+y)O_(5-2x+4y) ceramics have been investigated. A single CaSnSiO₅ phase with abnormally positive temperature coefficient of resonant frequency (τ_f = + 62.5 ppm/°C) was synthesised at 1450 °C. This composition was an effective τ_f compensator of CaSiO₃ and Ca₃SnSi₂O₉ phases with typically negative τ_f value. The CaSiO₃ second phase was related to the Sn deficiency in the CaSn_(1-x)SiO_(5-2x) (0 < x < 1.0) composition, whereas the Ca₃SnSi₂O₉ second phase was obtained by controlling the Ca:Sn:Si ratios on the basis of the Ca_(1+2y)SnSi_(1+y)O_(5+4y) (0 < y < 1.0) composition. A promising low-permittivity millimetre-wave ceramic with most excellent microwave dielectric properties (ε_r = 10.2, Q×f = 81,000 GHz and τ_f = −4.8 ppm/°C) was produced from the Ca_(1+2y)SnSi_(1+y)O_(5+4y) (y = 0.4) ceramic.     

氢化物原子荧光光谱法测定酱油中微量铅的方法研究

建立了一种快速、高效的QuEChERS-高效液相色谱-质谱联用法（QuEChERS-HPLC-MS/MS）测定谷类杂粮制品中脱氧雪腐镰刀菌烯醇（DON）、3-乙酰脱氧雪腐镰刀菌烯醇（3-ADON）、15-乙酰脱氧雪腐镰刀菌烯醇（15-ADON）和玉米赤霉烯酮（ZON）共4种真菌毒素。样品前处理采用乙腈-水溶剂提取，经Florisil+C18+无水硫酸镁净化后检测。以0.10%甲酸-乙腈作为流动相，在质谱检测器的多反应监测模式下进行分析。结果表明，4种真菌毒素在各自的线性范围内线性关系良好，相关系数R2均大于0.999，回收率在85.1%～102.0%，相对标准偏差（RSD）为2.11%～6.22%。该方法具有前处理简单、净化效果好、灵敏度高和检测速度快的优点，适用于谷类杂粮制品中DON、3-ADON、15-ADON 和ZON的分析和定量检测。     

复混肥料中钾含量的测定

根据作者多年工作经验，详细介绍了复混肥料中钾合量的到定，且与标准GB／T8574—1988进行了逐一比较。     

SnO2超微粒子薄膜的气敏特性研究

作者用自行设计的直流气体放电活化反应蒸发装置制备出平均粒径约为40nm的SnO_2超微粒子薄膜.研究了不同氧分压下所得SnO_2超微粒膜的形貌、结构和组成等特性,以及不同样品对各种易燃气体的气敏特性,得出了灵敏度随氧分压及灵敏度随工作温度的变化曲线.     

铜线材酸性高速电镀致密光亮锡、锡铜合金

为了寻找低成本、低腐蚀、低污染高速电镀锡、锡铜合金工艺 ,在含光亮剂、柔软剂DL0 1、0 2、0 3的硫酸槽中在不同的电流密度、不同的搅拌速度下 ,在Φ0 .5mm的铜线上电镀Sn和Sn Cu合金镀层。DL0 1、0 2的主要成分是无芳香族的希夫碱 ,DL0 3的主要成分是醇醛缩合物。结果表明 ,在含有DL0 1、0 2、0 3和 35g/LSnSO4 ,137g/LH2 SO4 的镀液中 ,在Jc=10～ 90A/dm2 ,v=16 0～ 314m/min时 ,所得镀层致密、柔软、光亮。在含CuSO4 ·5H2 O 0 .5 ,3.5g/L的硫酸镀槽中 ,在Jc=9,18A/dm2 ,v=16 0m/min时获得了致密、柔软、光亮的Sn (0 .3%～ 0 .6 % )Cu合金镀层。