Capillary and packed column SFC/MS

A frit restrictor interface for capillary column supercritical fluid chromatography/mass spectrometry (SFC/MS) has been constructed and used for the analysis of high boiling point alkanes. Packed column SFC/MS is described using both a moving belt liquid chromatographic/mass spectrometric interface and a thermospray source in the filament-on mode.     

Quantitative analysis of delta9-tetrahydrocannabinol in preserved oral fluid by liquid chromatography-tandem mass spectrometry

A rapid and sensitive method for the analysis of delta9-tetrahydrocannabinol (THC) in preserved oral fluid was developed and fully validated. Oral fluid was collected with the Intercept, a Food and Drug Administration (FDA) approved sampling device that is used on a large scale in the U.S. for workplace drug testing. The method comprised a simple liquid-liquid extraction with hexane, followed by liquid chromatography-tandem mass spectrometry (LC-MS-MS) analysis. Chromatographic separation was achieved using a XTerra MS C18 column, eluted isocratically with 1 mM ammonium formate-methanol (10:90, v/v). Selectivity of the method was achieved by a combination of retention time, and two precursor-product ion transitions. The use of the liquid-liquid extraction was demonstrated to be highly effective and led to significant decreases in the interferences present in the matrix. Validation of the method was performed using both 100 and 500 MicroL of oral fluid. The method was linear over the range investigated (0.5-100 ng/mL and 0. 1-10 ng/mL when 100 and 500 microL, respectively, of oral fluid were used) with an excellent intra-assay and inter-assay precision (relative standard deviations, RSD <6%) for quality control samples spiked at a concentration of 2.5 and 25 ng/mL and 0.5 and 2.5 ng/mL, respectively. Limits of quantification were 0.5 and 0.1 ng/mL when using 100 and 500 microL, respectively. In contrast to existing GC-MS methods, no extensive sample clean-up and time-consuming derivatisation steps were needed. The method was subsequently applied to Intercept samples collected at the roadside and collected during a controlled study with cannabis.     

Retention in coupled capillary column supercritical fluid chromatography with lipids as model compounds

Summary We have investigated to which extent retention data, acquired on single capillary columns, can be used for predicting retention factors in a coupled column system. For this purpose we utilized a model mixture of 18 lipid components with widely different vapor pressures and polarities. The sample was chromatographed on two columns, SB-biphenyl-30 (70% methyl-30% biphenylpolysiloxane) and SB-cyanopropyl-50 (50% methyl-50% cyanopropylsiloxane). Experimental retention factors, acquired in coupled column systems with two columns connected in different order, were thus compared with values calculated from runs on each single column. The agreement between calculated and experimental values generally was better than 5% without any pressure drop correction.To study the possibility of predicting retention behavior in a wide pressure range from a limited number of experiments, we also investigated the relation between solute retention and mobile phase density. We found that all data could be fitted to second order equations, which gives the possibility to optimize the resolution with respect to pressure from a limited number of runs at different pressures.     

A two-step supercritical fluid extraction of polycyclic aromatic hydrocarbons from roadside soil samples

A two-step procedure for the supercritical fluid extraction (SFE) of polycyclic aromatic hydrocarbons from soil samples was developed. The procedure consists of a static supercritical fluid treatment in a closed extraction cell at a high temperature (T=250 or 340degreesC for 20 min) and an SFE with a solvent trapping. During the static phase, the sample is exposed to a supercritical organic solvent (methanol, toluene, dichloromethane, ACN, acetone, and hexane). The solvent penetrates particles of the matrix to substitute strongly bonded molecules and dissolves the analytes in the supercritical phase. At ambient temperature, supercritical fluids became liquid and lost their solvation abilities. Most of the analytes condense on the surface of the particles or on the extraction cell walls without forming strong bonds or penetrating deep into the matrix. Thus, the pretreatment liberates the analytes and they behave similar to those in freshly spiked samples. The common SFE with toluene-modified CO2 as an extraction fluid follows the static phase. With the use of the most suitable extraction phases (toluene, ACN), the extraction efficiency of the combined procedure is much higher (approximately100%). The results of the combined procedure are compared to the SFE procedure of the same untreated sample (difference less than 5%) and to the Soxhlet extraction. The extracts were analyzed using a GC with the flame ionization detection.     

Retention behaviour of carboxylic acid methyl esters in supercritical fluid chromatography

The study on retention behavior in supercritical fluid chromatography (SFC) is necessary to understand the mechanism of the various interactions in SFC. The retention of SFC in carboxylic acid methyl ester/polymethylsiloxane/CO2 system was studied systematically and the retention behavior of this kind of compounds under various typical operation conditions was described using the method of an alternative unified theory of chromatographic retention. The results illustrated that expression: Ink.= a + b/T + cp + dp/T + ep2/T can be used to describe quantitatively the retention behavior of carboxylic acid methyl ester/polymethylsiloxane/CO2 system in the ranges of reduced density from 0.549 to 1.411. It was also found that the entropy of solute in stationary phase is dependent on the density of supercritical fluid (SF) under typical operating conditions of SFC.     

Separation of fatty acid methyl esters by comprehensive two-dimensional supercritical fluid chromatography with packed columns and programming of sampling duration

Fatty acid methyl esters from various fats and oils were separated by comprehensive two-dimensional supercritical fluid chromatography with conventional packed columns and FID detection. The first dimension was a silica gel column and the second dimension was an ODS column. This combination was largely orthogonal for the separation of fatty acid methyl esters. The first dimension separations were primarily based on the number of double bonds while the second dimension separations were based on the chain length. The highly-ordered chromatograms and improved resolution allowed the easy detection and identification of minor components. Although the first dimension separations were performed under isobaric conditions where the peak width increased in proportion to the retention, the programming of the sampling duration allowed us to maintain the optimum re-injection frequency (3–4 times) per peak into the second dimension and so to minimize the total analysis time without deteriorating the resolution.     

鄂尔多斯盆地北部天然气钻井技术研究

鄂尔多斯盆地北部(简称鄂北)工区钻井技术已配套成龙，优选的井身结构经济效益明显；3KP钾基聚合物钻井液、TG无固相完井液可保证井内安全；低密度水泥浆技术已成功应用。     

新疆东天山典型金矿床成矿物质来源探讨

作者根据对新疆东天山典型金矿床的沉淀成矿环境、地球化学特征、稳定同位素特征等的系统分析和研究，论证了形成金矿床的硅质流体最初是一种以水为主要溶剂，以溶解态、胶体态氧化硅为主要溶质的高温高压(超临界态)溶液，其来源于地幔，是一种溶解了大量SiO2的地幔流体。而成矿元素主要来源于硅质流体上升运移过程中所经围岩，以致成矿物质来源具异源性。这对研究内生金矿床的成矿机制和成因有着十分重要的意义。     

计算流体力学的发展及应用

计算流体力学是流体力学的一个分支。它用于求解固定几何形状空间内的流体的动量、热量和质量方程以及相关的其它方程，并通过计算机模拟获得某种流体在特定条件下的有关信息，是分析和解决问题的强有力和用途广泛的工具。对计算流体力学的发展和应用进行了综述并对其发展趋势做了探讨。     

地板送风静压层内气流的数值模拟与送风特性实验

采用计算流体力学(CFD)技术,对地板送风静压层的空气流动进行了数值模拟,并进行了典型的实验来验证计算结果.通过对计算结果与实验结果的比较,说明对于地板送风静压层内空气流动的CFD模拟,采用0 1 m的网格划分间距、标准k ε湍流模型是合理的.实验和计算结果一致表明,对于高度为170 mm的地板送风静压层,地板送风口的速度和送风量分布受到入口射流的影响,处于不同位置的地板送风口,其速度分布不同,有的均匀,有的速度值相差10倍.由数值模拟的地板送风静压层内空气流动特征,可展示和分析地板送风静压层的以上送风特性.