共查询到18条相似文献,搜索用时 125 毫秒
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填充毛细管液相色谱-高温毛细管气相色谱在线联用分析润滑油 总被引:6,自引:0,他引:6
建立了一套填充毛细管液相色谱-高温毛细管气相色谱在线联用装置,并应用于润滑油的全组分分析。用正相填充毛细管柱液相色谱法进行样品族分离,将润滑油分成烷烃、单环芳烃、双环芳烃、三环芳烃及胶质(多环芳烃和极性物);特殊设计的多储存位接口可完成一次LC进样,对样品所有族组成的在线切割、贮存并无损失转入GC分析,保证了复杂样品全组分分析的准确定性和定量,缩短了分析时间。GC分析结果给出各族组分的相对含量和碳数分布。 相似文献
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填充毛细管液相色谱-高温毛细管气相色谱在线联用分析重油 总被引:1,自引:0,他引:1
重油的组成分析一直是个难题,它的沸点高,族组分种类多,各族内组分的异构体又极为繁多.最好的分析方法是用高效液相色谱(HPLC)做族分离,馏分收集后再用CGC分析.但HPLC的族馏分体积比CGC进样量大100倍.本文采用填充毛细管液相色谱(μHPLC)与高温毛细管气相色谱(HTGC)在线联用技术[1]分析重油.正相μHPLC将样品按族分离,μHPLC的柱效高,族分离能力强,而小的馏分体积(<100μL)可避免GC分流进样.在一次LC进样后,多位储存型联用接口将分离后的各族组分切割、存储并分别无损失转入HTGC分析,利用FID对高于C10的有机物的响应值相… 相似文献
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填充毛细管液相色谱-毛细管气相色谱在线联用分析八角茴香挥发油 总被引:1,自引:0,他引:1
首次将填充毛细管高效液相色谱-毛细管气相色谱在线联用技术(μ-HPLC-CGC)用于分离分析八角茴香果实的挥发油成分。液相色谱选用氰基分析柱(250 mm×0.32 mm i.d.),正己烷-乙腈-二氯甲烷(体积比为80∶8∶12)为流动相,对挥发油样品做族组分分离,得到的5个族组分被依次存放在多位储存接口内,然后不分流分别转入毛细管气相色谱仪做详细分析。气相色谱柱由10 m×0.53 mm i.d.保留间隔柱和30 m×0.53 mm i.d.×1.0 μm SE-54分析柱组成。采用了不分流柱内进样模 相似文献
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填充毛细管液相色谱—毛细管气相色谱在线联用分析柴油全组成 总被引:5,自引:0,他引:5
采用填充毛细管液相色谱(PC-HPLC)与毛管气相色谱(CGC)在线联用技术分析柴油全组分。半填充硅胶、半填充氨基的PC-HPLC柱(0.32mm i.d)用于样品族分离(烷烃、单环芳烃、双环芳烃、三环芳烃和胶质)。经PC-HPLC分离后的各族组分(峰体积小于30μL)被依次存放在多位储存接口内,然后分别转入GC作单个组分定量分析,可得出各族组分的相对含量及烷烃的碳数的正异构分布。该方法是分析柴油 相似文献
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Takao TSUDA 《色谱》2000,18(5):402-411
Abstract:Capillary columns are used in both capillary liquid chromatography and capillary electrochromatography. The design for capillary liquid chromatography is discussed in comparison with capillary gas chromatography. The difference of diffusion coefficient in gas and liquid phase is a key role. The study for obtaining a high performance capillary liquid chromatography is discussed. Capillary electrochromatography is recently interesting for its instinct ability to realize a high performance chromatography. Capillary electrochromatography with and without pressurized flow is reviewed briefly. Instrumentation for capillary electrochromatography with pressurized flow is discussed. The port of splitting, and gradient elution of both solution and potential are described. The new findings of both the variation of column resistance and capacity factor according to the value of applied electric voltage are also discussed. 相似文献
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María Paz San Andrs María Eugenia Len‐Gonzlez Luis Vicente Prez‐Arribas Luis María Polo‐Díez 《Journal of separation science》2000,23(5):367-372
This paper describes a liquid chromatographic method using a reversed phase capillary column coupled to an UV detector for the quantitation of thirteen pollutant phenols. Chromatographic separation was carried out with gradient elution at 25.0 ± 0.1°C. The two major anisocratic elution modes (gradient elution and temperature programming) were evaluated. The detection limit range was 10–81 pg (100 nL injected). The chromatographic method combined with liquid‐liquid extraction was applied to analysis of these compounds in river water. Recoveries of 75–103% were achieved for most of them. 相似文献
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Expressions for the minimum detectable amount Qo and the minimum analyte concentration Co as functions of the chromatographic parameters are derived for both mass and concentration sensitive detectors. The effects of pressure drop, column inner diameter, and film thickness are given. The minimum analyte concentration for mass flow sensitive detectors, Com, can be reduced considerably by selecting the carrier gas velocity well above its optimum value (related to Hmin), however, at the cost of long columns and long analysis times. For Qo the improvements can be neglected, and so the analysis can best be performed at uopt. When the flow rate in the detector, Fd, is equal to the column flow rate Fc, the maximum permissible detector volume of concentration sensitive detectors is proportional to dc2 up to dc3, and so narrow bore columns require detectors of extremely small volume. Make-up gas has to be added when the actual volume is too large, thus worsening the detectability. Another approach, vacuum operation of the detector cell, appears to be very attractive. On the other hand, when wide bore columns are used in combination with small volume concentration sensitive detectors, very small values of Qoc and Coc are obtainable when the abundant carrier gas can be removed before entering the detector cell. Digital noise filtering can further reduce the obtainable Qo and Co values, especially for broad peaks and thus for wide bore columns. 相似文献
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Edward S. Yeung 《中国化学会会志》1991,38(4):307-312
Two new approaches for absorption detection in capillary columns are presented. They are applicable to columns as narrow as 10μm i.d. Both provide good sensitivity despite the very short optical pathlengths that are commonly available in commercial systems. The first involves irradiating the column along its axis rather than across the axis. The entire analyte zone can then participate in absorption. Gains up to 1000 fold can be expected. The second is a modification of laser-excited fluorescence. The absorbing analytes, even though they do not fluoresce efficiently, can transfer their energy to a fluorophore added to the mobile phase. The secondary emission can be used to detect absorption in the nanomolar range. 相似文献