Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits

Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation.     

Simultaneous determination of bisphenol A and alkylphenol in plant oil by gel permeation chromatography and isotopic dilution liquid chromatography-tandem mass spectrometry

A simple analytical method was developed for the simultaneous analysis of bisphenol A (BPA), nonylphenol (NP) and octylphenol (OP) in plant oil. The target compounds were extracted by cyclohexane/ethyl acetate (1:1), purified by gel permeation chromatography (GPC), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) in the negative ion mode. An isolator column was attached in front of the injection valve of the LC to separate background contaminants. Recovery studies were performed at three fortification levels. Mean recoveries were from 92.9% to 119.0%, with an acceptable coefficient of variation (4.4-18.5%, n=6). The limits of quantification of the method were 2, 2 and 0.5 μg/kg for BPA, NP and OP, respectively. This method can be applied for screening and confirming target compounds in plant oil.     

icoshift: An effective tool for the alignment of chromatographic data

The Interval Correlation Optimised Shifting algorithm (icoshift) has recently been introduced for the alignment of nuclear magnetic resonance spectra. The method is based on an insertion/deletion model to shift intervals of spectra/chromatograms and relies on an efficient Fast Fourier Transform based computation core that allows the alignment of large data sets in a few seconds on a standard personal computer. The potential of this programme for the alignment of chromatographic data is outlined with focus on the model used for the correction function. The efficacy of the algorithm is demonstrated on a chromatographic data set with 45 chromatograms of 64,000 data points. Computation time is significantly reduced compared to the Correlation Optimised Warping (COW) algorithm, which is widely used for the alignment of chromatographic signals. Moreover, icoshift proved to perform better than COW in terms of quality of the alignment (viz. of simplicity and peak factor), but without the need for computationally expensive optimisations of the warping meta-parameters required by COW. Principal component analysis (PCA) is used to show how a significant reduction on data complexity was achieved, improving the ability to highlight chemical differences amongst the samples.     

Speciation analysis of arsenic compounds in edible oil by ion chromatography-inductively coupled plasma mass spectrometry

An inductively coupled plasma mass spectrometer (ICP-MS) was used as an ion chromatographic (IC) detector for the speciation analysis of arsenic in edible oil. The arsenic species studied include arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine and arsenocholine. Gradient elution using (NH(4))(2)CO(3) and methanol at pH 8.5 allowed the chromatographic separation of all species in less than 8 min. Effluents from the IC column were delivered to the nebulizer of ICP-MS for the determination of arsenic. The concentrations of arsenic species have been determined in several used and fresh vegetable oil samples. In this study, a microwave-assisted extraction method was used for the extraction of arsenic species from oil samples. The extraction efficiency was better than 92% and the recoveries from spiked samples were in the range of 90-105%. The precision between sample replicates was better than 8% for all determinations. The limits of detection were in the range of 0.008-0.024 ng mL(-1) for various arsenic species based on peak height, which corresponded to 0.08-0.24 ng g(-1) in the original oil sample. The major arsenic species in the used oil samples varied based on the food items cooked.     

Experimental investigation of air–oil slug flow using capacitance probes,hot-film anemometer,and image processing

Despite the importance of air–oil slug flows to many industrial applications, their available data reported in the literature are limited compared to air–water slug flows. The main objective of the present study is to explain how air–oil slug flow parameters can be experimentally investigated using hot-film anemometry, capacitance sensors and image processing. Experiments were performed using air–oil slug flow through a horizontal pipe for air superficial velocities ranged from 0.01 m/s to 0.65 m/s and oil superficial velocities ranged from 0.03 m/s to 2.3 m/s. The signal obtained from the hot-film anemometer was used to determine the time-averaged local void fraction and liquid velocity and turbulence intensity for air–oil slug flow. The capacitance signals along with the data obtained by image processing of the flow were used to determine the elongated bubble length and velocity. The measurements techniques used found to describe in detail the internal structure of the slug flow. Finally, the experimental results were compared to existing models and correlations.     

基于油膜干涉法的表面摩擦应力测量技术研究

本文应用油膜干涉法及速度型方法在平板模型上进行低速湍流的表面摩擦阻力测量,探索了油膜法测量表面摩擦阻力的实验技术,分析了不同实验方式对测量结果的影响以及实验误差产生的原因.研究表明,模型安装方式、油膜布置方式以及重力作用的影响在油膜干涉法中基本都可以忽略,在精度要求不高的情况下,不需要对结果进行修正.通过采用热膜法和油...     

石油钻井物料清单的随机数量模型研究

针对石油钻井物料投资大、物料消耗随机不确定、管理控制难的现状,本文通过构建石油钻井物料清单,提出以石油钻井物料损耗数量为随机变量,按钻井开次分阶段计算方式,分别采用期望值和渴望水平原则方法,构建石油钻井物料清单的随机数量模型。该模型的建立与应用,为石油钻井企业缩短物资供应周期、降低库存成本,实现钻井物料供应的优化管理提供了辅助支持。     

中美燃料油期货价格引导研究

本文利用ADF单整检验、EG协整检验、误差修正模型、引导关系检验等方法研究中美燃料油期货价格之间的互动关系,结果表明:我国燃料油期货在价格和价格收益方面均与国际燃料油市场存在明显的即时引导关系;国际燃料油期货市场上的价格变动对国内燃料油期货价格以及价格收益的变动具有单向的滞后引导作用;我国燃料油期货市场的价格和收益方面的信息对于国际市场几乎不产生影响,我国尚不具备制定价格的话语权。     

国际油价波动跳跃性特征的实证分析

根据国际油价波动中存在异常跳跃的情况,本文运用EGARCH-Jump模型对国际油价波动的跳跃性特征进行了实证分析。结果表明,加入跳跃因素的模型减缓了国际油价波动的持续性,同时杠杆效应消失,表明跳跃性因素是国际油价波动的影响因素之一,也证实了国际油价波动的跳跃性特征是国际石油市场产生杠杆效应的原因。但从长期来看,跳跃性因素对国际油价波动的扰动影响并不大,国际油价的波动仍主要受正常信息的影响。总体上,EGARCH-Jump模型比普通GARCH族模型能更好地捕捉国际油价波动的动态性特征。     

一种油田原油含水率的近红外光谱检测与分析方法

石油作为重要战略资源,对其组分进行实时分析检测在石油化工领域有着重要意义。随着石油资源的不断开发,在已长时间开采油井的生产过程中以及新油井开采前,需要对井下原油组分进行分析检测,以判定开采的必要性。原油组分实时检测,在原油开采、生产、储运以及销售过程中都起着关键的作用,针对传统检测方法存在精度低、效率低等问题,近年来在原油组分检测技术的研究方法上引入了在测量领域得到广泛、有效应用的近红外光谱测量技术。以井下原油作为研究对象,利用从大庆油田获得的提纯原油与水按体积比配制了原油占比分别为1%~20%共39个组分的实验样品来模拟井下原油。研究了近红外光谱透射法测量原油组分的基本原理,并利用SW2520型近红外光谱仪与卤素光源以及配套组件集成了原油样品近红外光谱数据测量系统,完成了系统的标准化实验并利用此标准化后的系统采集了39个组分原油样品的近红外吸收光谱数据。利用移动窗口平滑法、Savitzky-Golay卷积平滑法以及Savitzky-Golay卷积求导法对原油近红外光谱数据进行预处理以消除噪声,利用偏最小二乘法和支持向量机回归方法SVR两种分析方法对预处理后的原油样品近红外光谱进行建模,分别建立了原油组分分析预测模型。研究结果表明,利用偏最小二乘法模型预测均方根误差为0.003 755 14,决定系数R2为0.999 999,预测精度优于0.1%,预测效果十分理想。利用近红外光谱技术对配制的不同比例的井下原油模拟测试样品进行测试建模和分析,为井下原油组份检测提供了一种新的思路,该方法可以有效的解决原油含水率的检测问题,为开发油田现场实时原油检测分析装备提供技术支撑。