共查询到20条相似文献,搜索用时 15 毫秒
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Mark van Lieshout Rico Derks Hans-Gerd Janssen Carel A. Cramers 《Journal of separation science》1998,21(11):583-586
Savings in analysis time in capillary GC have always been an important issue for chromatographers since the introduction of capillary columns by Golay in 1958. In laboratories where gas chromatographic techniques are routinely applied as an analytical technique, every reduction of analysis time, without significant loss of resolution, can be translated into a higher sample throughput and hence reduce the laboratory operating costs. In this contribution, three different approaches for obtaining fast GC separations are investigated. First, a narrow-bore column is used under conventional GC operating conditions. Secondly, the same narrow-bore column is used under typical fast GC conditions. Here, a high oven temperature programming rate is used. The third approach uses a recent new development in GC instrumentation: Flash-2D-GC. Here the column is placed inside a metal tube, which is resistively heated. With this system, a temperature programming rate of 100°/s is possible. The results obtained with each of these three approaches are compared with results obtained on a column with conventional dimensions. This comparison takes retention times as well as plate numbers and resolution into consideration. 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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Peter G. Van Ysacker Henri M. Snijders Hans-Gerd M. Janssen Carel A. Cramers 《Journal of separation science》1998,21(9):491-497
The use of hot splitless, cold splitless, and on-column injections for trace analysis in narrow-bore capillary GC is evaluated. Despite the low flow rates for the columns used, the required splitless times for splitless injections can be surprisingly short if liners with a small inside diameter are used. On-column injection can be applied by using an appropriate normal-bore precolumn coupled to the narrow-bore analytical column using a specially designed low dead volume column connector. The effects of the experimental conditions such as sample volume, injection temperature, and initial oven temperature on peak focusing and the discrimination and degradation behavior of the analytes are discussed. The possibilities to obtain sensitive and fast separations are illustrated by various applications. 相似文献
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Rapid separations of selected environmentally important polar compounds using polymer-encapsulated silica stationary phases and a carbon dioxide mobile phase under solvating gas chromatography (SGC) conditions are reported. Ten underivatized short chain aldehydes and ten nitrogen-containing herbicides were separated within 1 min and 5 min, respectively, using a 30 cm×250 μm i. d. column packed with diol-bonded, polyethylenimine (PEI)-coated, and hexamethyldisilazane (HMDS)-end-capped silica particles (5 μm, 120 Å). Seven organophosphorus pesticides were resolved in less than 5 min using a 30 cm×250 μm i. d. column packed with polymethylhydrosiloxane-deactivated and SE-54 encapsulated silica particles. Separation numbers per unit time increased with pressure and temperature ramps. Both rapid pressure and temperature programming can be used to increase the speed of SGC. The effects of pressure and temperature on apparent retention factors of solutes with various polarities were investigated using diol-PEI-HMDS silica particles in SGC. 相似文献
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《Analytical letters》2012,45(9):619-628
Abstract A glass injection system consisting of a packed precolumn and gasphase splitter has been developed for the introduction of derivatized biological samples on glass capillary columns. The precolumn provides complete sample evaporation before the splitter zone, traps contaminating nonvolatiles, and prevents decomposition or adsorption of components. In addition, a carrier gas control system is described that permits stable and repeatable adjustment of split ratio and capillary inlet pressure. The linearity of the splitter has been established using a hydrocarbon mixture covering the range of methylene unit (MU) values in which the steroid derivatives are eluted. 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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Stop-flow techniques are occasionally needed in combinations of LC-NMR and LC-MS. During the interval when there is no flow
on the column, axial diffusion of components not yet eluted can be expected to take place. In this paper the size of the band
broadening which is caused by diffusion during stop-flow has been determined for two peptides on reversed-phase packed micro
columns. Within a temperature range of 20–40 °C, stop-flow could be extended to 30 minutes for peptides having k values in the range of 0.7–5.1 with little increase in band width on 1.0 mm i.d. columns at isocratic conditions. Stop-flow
for 6 h at 20 °C increased the peak width of bradykinin and leucine-enkephalin by 25% and 60%, respectively, depending on
the secondary interactions of the peptides. The peak broadening increased with increasing temperature (from 20 to 40 °C),
as expected, and the impact was significant at stop-flow times larger than 2 h. Stop-flow during gradient elution resulted
in less increase in peak width than isocratic elution due to the peak compression obtained when re-entering the gradient.
At 20 °C the effective diffusion coefficients of leucine-enkephalin and bradykinin were determined to 6.5 × 10−7cm 2/s and 5.5 × 10−7 cm2/s, respectively, on the packed micro column. 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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Gregorio Meira Miloš Netopilík Martin Potschka Irene Schnöll-Bitai Jorge Vega 《Macromolecular Symposia》2007,258(1):186-197
Summary: This article reviews some recent developments on the determination of the Band Broadening Function (BBF) in Size Exclusion Chromatography (SEC) of polymers. It was carried out in the frame of the IUPAC Project: “Data Treatment in Size Exclusion Chromatography of Polymers”. The correction for band broadening (BB) is important for quantitative determinations of the molar mass distribution (MMD) of narrow-distributed (or highly multimodal) polymers, and of derived variables such as kinetic parameters. In the narrow range of a molar mass standard, the BBF is uniform and of positive skewness. In a broad chromatographic range, the BBF is non-uniform and skewed; and it can be adequately represented by an exponentially-modified Gaussian function (EMG) of 2 parameters that vary slightly with elution volume: an increasing Gaussian variance and a decreasing exponential decay. Additionally, the total BBF variance remains almost constant if not close to the total exclusion limit. The following methods for determining BBF parameters are reviewed: a) a direct method based on assuming Poisson-distributed MMDs; b) a direct method based on measuring the mass- and molar mass chromatograms of narrow standards; c) a theoretical method based on a stochastic model that is equivalent to the Giddings-Eyring model; and d) a theoretical method based on a deterministic model obtained through an extension of the classical van Deemter expression. Ideally, the correction for BB requires a robust numerical inversion algorithm. However, alternative simplified solutions are also possible. 相似文献
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研究出一种改进的毛细管分流进样器,设计了一种新型螺旋进样内衬管。使分流进样的重复精度有显著提高,沸点歧视效应减小,色谱峰尾尖锐,使毛细管色谱柱的高分离效能得以充分发挥。对4种常用的进样内衬进行了考察,得到了有重要实用意义的结果,并从理论上解释了与传统观点相悖的实验现象,深化了对分流进样动态过程的理解。 相似文献
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毛细管气相色谱法鉴定分析杆菌 总被引:1,自引:0,他引:1
本文利用OV-101熔融石英毛细管柱,对15种标准分枝杆菌的色谱特征进行了研究,得到了特异性指纹图。并对42株临床菌株进行了鉴别。 相似文献
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毛细管气相色谱法测定染发剂中七种染料组份 总被引:2,自引:0,他引:2
采用毛细管气相色谱法对染发剂中苯酚、邻苯二酚、对苯二酚、间苯二酚、邻苯二胺、对苯二胺和间苯二胺七种染料进行了分析。结果表明,该方法能有效地分离这七种染料,其检出限为苯酚50ng、邻苯二胺160ng、对苯二胺240ng、邻苯二酚280ng、间苯二胺180ng、对苯二酚190ng、间苯二酚180ng。方法测定精密度为2.07-4.33%,回收率为96.1%-103.3%。方法具有操作准确、简单、快速、实用等特点。 相似文献
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