Fourier Transform Infrared Spectroscopy and Solid Phase Extraction Applied to the Determination of Oil and Grease in Water Matrices

 The solid phase extraction as a solvent-free method for the analysis of oil and grease in waters was studied. The use of a PTFE surface as a solid phase allows the retention of the volatile fraction of oil and grease, and further analysis of carbon–hydrogen bonds using infrared spectroscopy can be done on the surface. Various oils and grease samples were tested: n-hexadecane, n-tetradecane, n-nonadecane, n-docosane, isooctane, diesel oil and gasoline. Temperatures from 25° to 90 °C and a range of heating times were checked for extraction. Precision tests showed relative standard deviation values of around 10% in several samples of the same concentration. Calibration lines of n-hexadecane showed high correlation coefficients from 0.9 to 30 mg/l. Recoveries for the various oils using different calibration lines showed values from 90 to 110%. The method described here is fast and clean, and allows reproducible measurements of oil and grease in water that do not require the use of a solvent. Received March 1, 2001; accepted August 15, 2001; published online July 15, 2002     

Efficient Oxidation of Cyclohexane over Bulk Nickel Oxide under Mild Conditions

Nickel oxide powder was prepared by simple calcination of nickel nitrate hexahydrate at 500 °C for 5 h and used as a catalyst for the oxidation of cyclohexane to produce the cyclohexanone and cyclohexanol—KA oil. Molecular oxygen (O₂), hydrogen peroxide (H₂O₂), t-butyl hydrogen peroxide (TBHP) and meta-chloroperoxybenzoic acid (m-CPBA) were evaluated as oxidizing agents under different conditions. m-CPBA exhibited higher catalytic activity compared to other oxidants. Using 1.5 equivalent of m-CPBA as an oxygen donor agent for 24 h at 70 °C, in acetonitrile as a solvent, NiO powder showed exceptional catalytic activity for the oxidation of cyclohexane to produce KA oil. Compared to different catalytic systems reported in the literature, for the first time, about 85% of cyclohexane was converted to products, with 99% KA oil selectivity, including around 87% and 13% selectivity toward cyclohexanone and cyclohexanol, respectively. The reusability of NiO catalyst was also investigated. During four successive cycles, the conversion of cyclohexane and the selectivity toward cyclohexanone were decreased progressively to 63% and 60%, respectively, while the selectivity toward cyclohexanol was increased gradually to 40%.     

HKD-1型航空润滑油特征剪切应力及有效粘压系数确定的研究

在球盘式拖动力试验机上,对HKD-1型航空润滑油进行拖动力测量,给出了根据拖动力试验曲线的非线性上升段确定润滑油有效粘压系数和特征应力的方法,对HKD-1型航空润滑油在试验条件下的粘压系数和特征应力进行分析,并建立了其计算公式.结果表明:特征应力和有效粘压系数的求解方法简单合理,其计算公式的拟合精度较高,可为轴承动态特性设计提供计算依据;随着接触压力、入口油温和滚动速度增加,HKD-1型航空润滑油的特征应力增大,其粘压系数减小;滚动速度对特征应力和粘压系数的影响小于接触压力和入口油温.     

考虑油膜力作用的船舶主推进系统冲击研究

舰船推进轴系是舰船动力装置的重要组成部分,它的稳定性是舰船生命力的基本保证.本文以舰船主推进轴系为研究对象,考虑了非线性油膜力的作用,在推进轴的非线性油膜力模型中,考虑了油膜涡动效应和挤压效应以及多个轴承油膜力的耦合影响,并考虑了轴承结构本身的刚度.文中采用弹性体动力学方法对推进轴建模,考虑了在外冲击作用下转速和轴承油膜力对于转轴冲击响应的影响,考虑横向运动与转动耦合作用,导出以非线性偏微分方程描述的舰船主推进轴的动力学方程,并用经典理论对其进行离散,最后采用龙格-库塔法进行数值仿真.实例分析指出转速对于转轴冲击响应的影响不可忽略.     

含纳米添加剂的润滑体系在摩擦过程中的接触电阻研究

采用UMT-2型微摩擦磨损试验机考察了4种纳米颗粒LaF3、Ag、SiO2 及Al2O3作为润滑油添加剂在摩擦过程中的接触电阻随时间变化的情况,并由此监测摩擦副表面的成膜状况;采用X射线光电子能谱仪分析4种纳米添加剂润滑下磨损表面典型元素的化学状态,并结合接触电阻测试结果分析纳米油润滑添加剂的润滑机理.结果表明:接触电阻测试能够适时监测添加剂在摩擦副表面的成膜过程,4种纳米润滑油添加剂在边界润滑条件下均能够在磨损表面沉积成膜,其在试验过程中的化学状态没有发生变化,但4种纳米润滑油添加剂在摩擦过程中的成膜性能不同,Ag和LaF3在摩擦过程中的沉积速率、沉积膜厚度及其在摩擦副表面的结合强度优于SiO2和Al2O3.     

碱液萃取前后原油中酸性化合物组成的高分辨质谱分析

采用改进的碱液萃取方法分离杜巴原油中的酸性化合物(主要是环烷酸),通过高分辨质谱分析萃取过程中不同组分酸性化合物组成,以研究碱萃取前后酸性化合物的分布与组成特征。实验结果表明,电喷雾傅立叶变换离子回旋共振高分辨质谱(ESI-FT-ICR-MS)是分析原油中酸性化合物的强有力的手段;酸性化合物分布于碱萃取前后的各个组分中,但其组成有明显的差异,碱液萃取出的石油酸主要是相对分子质量小于500的酸性组分,增加反萃取溶剂的用量和极性有利于脱除萃取物中的非碱性氮化合物,对石油羧酸的组成影响不大。     

A Fault Detection Method for Electrohydraulic Switch Machine Based on Oil-Pressure-Signal-Sectionalized Feature Extraction

A turnout switch machine is key equipment in a railway, and its fault condition has an enormous impact on the safety of train operation. Electrohydraulic switch machines are increasingly used in high-speed railways, and how to extract effective fault features from their working condition monitoring signal is a difficult problem. This paper focuses on the sectionalized feature extraction method of the oil pressure signal of the electrohydraulic switch machine and realizes the fault detection of the switch machine based on this method. First, the oil pressure signal is divided into three stages according to the working principle and action process of the switch machine, and multiple features of each stage are extracted. Then the max-relevance and min-redundancy (mRMR) algorithm is applied to select the effective features. Finally, the mini batch k-means method is used to achieve unsupervised fault diagnosis. Through experimental verification, this method can not only derive the best sectionalization mode and feature types of the oil pressure signal, but also achieve the fault diagnosis and the prediction of the status of the electrohydraulic switch machine.     

HPLC法测定辣椒油中苏丹红染料的测量不确定度评定

建立了HPLC法分析辣椒油中苏丹红染料的不确定度模型,分析了方法中的不确定度分量及其来源,计算了各不确定度分量和合成标准不确定度。     

佩兰挥发性化学成分的固相微萃取研究

采用固相微萃取-气相色谱-质谱法分析佩兰中挥发性化学成分,共分离出84个组分,并鉴定了67个组分,用归一化法测定其质量分数,占总挥发性组分峰面积的98.05%。主要成分是对-伞花烃(5.19%)、芳樟醇(3.72%)、β-石竹烯(12.35%)、α-律草烯(13.39%)、α-姜黄烯(2.11%)、(-)-石竹烯氧化物(8.25%)、. /-.-4-乙酰基-1-甲基环己烯(8.91%)。     

冷蒿挥发油化学成分的分离和鉴定

采用水蒸气蒸馏法提取了冷蒿挥发油,气相色谱-质谱联用结合计算机检索对其化学成分进行了分析和鉴定,共分离出106个峰,确定了101种化合物,它们主要是二甲基-甲撑基环庚(17.67%)、3,3,6-三甲基-1,5-庚二烯醇-2(16.40%)、3,3,6-三甲基-1,4-庚二烯醇-6(8.55%)、桉树脑(5.57%)、3,7-二甲-基2,6-辛二烯醇-1(3.85%)、神圣亚麻三烯(3.73%)、1-甲基-3-异丙基苯(3.26%)、桥环[2,2,1]萜烯(2.91%)、樟脑(2.26%)、香叶烯(2.20%),以上10种化合物占挥发油总量的66.40%。