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。     

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。     

Model validation and model structure determination

This paper gives a tutorial overview of basic approaches for model validation and model structure determination.Work partially supported by the Swedish Research Council for Engineering Sciences under contract 98-654.     

Simultaneous Spectrophotometric Determination of Three Components Including Deoxyschizandrin by Partial Least Squares Regression

1IntroductionWuweizi is a traditional Chinese herb,usually usedto cure cough,asthma,neurasthenic,hepatitisetc.Theactive ingredients in wuweizi are5%-22%lignan,themain components of which include deoxyschizandrin,schizandrin andγ-Schizandrin.Forthe purpos…     

A novel method for determination of polyester end-groups by NMR spectroscopy

An efficient, convenient and quantitative method for characterising polyester end-groups is described. We have found that trichloroacetyl isocyanate (TAI) reacts rapidly and quantitatively with both carboxyl [C(O)OH] and hydroxyl (OH) chain ends to form derivatives that can be readily determined by ¹H NMR spectroscopy. The TAI capped end-groups give rise to characteristic imidic NH resonances in a normally clear region of the ¹H NMR spectrum [δ∼10-11.5 for C(O)-O-C(O)-NH-C(O)CCl₃ from C(O)OH, δ∼8-9 for O-C(O)-NH-C(O)CCl₃ from OH]. The method has been successfully applied to quantitative determination of the end-groups of a wide variety of oligomeric polyesters. It has also been applied to higher molecular weight polyesters including commercial, bottle grade, poly(ethylene terephthalate) (PET) and PET based copolyesters (e.g. PETG).     

中国的三种非同步轨道卫星移动通信系统星座方案

本文介绍基于我国的三种非同步轨道卫星移动通信系统星座方案：低、中轨系统各有２４和１８颗星，轨道高度分别为１３２６和８０３５ｋｍ，两系统各以５°和３０°的仰角对我国的覆盖率为９９．７８％和９９．９６％；椭圆轨道系统１２颗星，近、远地点分别为４２７和２９０６ｋｍ，以７°和１５°仰角对我国北纬２０°以上地区覆盖率分别为９７．９０％和８９．６１％，若增加４颗中轨卫星，以１５°仰角对我国的覆盖率为９９．９９％。     

直流电动机参数测定

根据直流电机的可逆原理并利用常规的实验仪表，可以简便、准确地测出直流电动机的主要参数－电磁转矩、输出转矩和效率．     

热重分析对高分子材料中碳酸钙的定量研究

碳酸钙是高分子材料中常用的无机填料，在高温时会同二氧化碳而失重。利用热重分析可准确定出高分子材料中碳酸钙的含量，同时还可测出聚合物，挥发物的含量，热重分析法样品用量小，灵敏度高，所需时间短。     

高温合金中微量铈的快速测定

采用DBC-偶氮胂[3-(2-胂酸基苯偶氮)-6-(2，6-二溴-4氮苯偶氮)-4，5二经基2，7-萘二磺酸]直接测定高温合金钢中微量铈和碳钢、低合金中的铈，获得满意结果。