近年国内外毛细管气相色谱柱的进展和趋向

报道了近两年毛细管气相色谱柱的发展和趋向. 气相色谱柱制柱工艺是一个成熟的技术, 所以在制柱工艺方面的研究不够活跃. 近年新研究的固定相集中在常温离子液体和各种环糊精的衍生物. 近几年GC毛细管色谱柱的研究和改进集中在色谱柱厂家进行, 并立即成为商品柱. 本文对近两年一些重要期刊上发表的气相色谱论文进行了总结, 发现气相色谱分析所用的色谱柱大都使用毛细管柱, 并趋向于使用商品GC毛细管柱, 所使用的商品色谱柱中, 使用最多的是以含5%苯基的聚甲基硅氧烷做固定相的色谱柱, 其次是以100%甲基的聚硅氧烷做固定相的色谱柱. 极性毛细管色谱柱主要使用PEG、 OV-17和OV-1701固定相.     

气相色谱近年的发展

简要阐述了近几年气相色谱(GC)的发展和特点。GC是一个成熟的技术,广泛地应用于各个领域,近几年GC的发展除了继续研究新的固定相和高性能的毛细管色谱柱之外,主要在全二维气相色谱(GC×GC)、快速GC、便携式GC仪和微型GC仪几个方面。近几年新研究的GC固定相主要集中在常温离子液体和各种环糊精的衍生物。现在GC研究者趋向于使用商品化的GC毛细管柱,而商品化的GC毛细管柱应用最多的是以含5%苯基的聚甲基硅氧烷为固定相的色谱柱。GC×GC发展迅猛,特别是关于调制器的研究,已开发出十多种调制模式,并广泛地应用于各个领域。为了适应大量样品的分析和现场分析,研究和开发了多种快速GC方法和仪器以及便携式GC仪。为了仪器的小型化和专属性检测,μGC仪的研究也稳步地发展起来。     

近年国内固相萃取-色谱分析的进展

对近两年国内各个领域的学者在使用固相萃取做样品前处理的色谱分析方面的研究和应用作了综述, 这一综述包括10个部分: 1. 国内近两年有关固相萃取的综述报告;2. 固相萃取-色谱分析在水质分析中的应用;3. 固相萃取-色谱分析在奶制品和肉类食品分析中的应用;4. 固相萃取-色谱用于蔬菜和水果中有害物质分析的应用;5. 固相萃取-色谱用于粮食和其他食品中有害物质分析的应用;6. 固相萃取-色谱在血药浓度、体液及组织中有害物质分析中的应用;7. 固相萃取-色谱在药物分析中的应用;8. 固相萃取-色谱在其他使用色谱分析中的应用;9. 基质固相分散在色谱分析中的应用;10. 分子印迹SPE在样品前处理中的应用.     

近两年国内气相色谱的应用进展(Ⅲ)

对近两年国内各个领域的学者在气相色谱方面的研究和应用作了综述,本综述分3部分叙述,本篇为第 部分,包括:8.气相色谱在食品功效成分和其他成分分析中的应用,9.气相色谱酒分析中的应用,1 0 .气相色谱在污染物分析中的应用,1 1 .气相色谱在石油、石油化工分析中的应用,1 2 .气相色谱在化学品生产分析中的应用     

国内气相色谱近年的进展

本文对近三年国内学者在气相色谱方面的研究和应用作了综述 ,国内学者的研究基本和国际上气相色谱方面的研究类似 ,在全二维气相色谱、快速气相色谱 ,微型气相色谱仪、新型气相色谱固定相和色谱柱的溶胶 凝胶涂渍技术领域的研究方面作出了贡献。有关气相色谱的应用研究中 ,介绍了大量在药物分析、食品分析、环境分析、石油和石化分析和化工产品及高聚物分析等领域中应用的题目和摘要     

气相色谱固定相研究新进展

发展高选择性固定相是实现气相色谱(GC)高效分离样品组分及其分析测定的关键。近年,材料科学的快速发展促进了新型色谱固定相的研究和应用。该文综述了近5年有关多孔材料、石墨烯及类似物、三聚茚类材料和蝶烯类材料等作为GC固定相的研究进展,并对GC固定相研究进行了总结和展望。     

制备气相色谱在挥发性成分分离中的应用研究进展北大核心CSCD

分析型气相色谱仪对低沸点易挥发的有机化合物展现出优异的分离性能,通过在其色谱柱末端加装馏分收集装置,建立了现代制备气相色谱(Prep GC)技术,该技术可用于挥发性成分的快速分离富集。制备气相色谱仪是由分析型气相色谱仪改装而来,其进样系统、分离系统、检测系统、馏分收集系统也在不断地优化升级,以提高目标化合物的回收效率和纯度。Prep GC与现代波谱技术(如紫外可见吸收光谱、红外吸收光谱、拉曼光谱、质谱、X射线衍射、核磁共振波谱)耦合,可对分离富集得到的目标化合物的结构进行精准确证。近年来,与Prep GC在各种挥发性成分分离中的应用相关的报道逐渐增多,展现出良好的应用前景。然而,Prep GC在分离过程中也存在着无法制备热敏性化合物、分离成本高、易引入外源性污染等问题。该文根据近年来国内外研究学者的相关研究工作,对制备气相色谱仪的结构及其在精油单体化合物、昆虫信息素、食品和植物挥发性成分、地质生物标志物及持久性环境污染物的分离等领域的应用研究进展进行综述。最后,还对Prep GC在挥发性成分分离中的应用进行了总结与展望,旨在为拓展Prep GC应用领域提供参考。     

近两年国内气相色谱的应用进展(Ⅱ)

对近两年国内各个领域的学者在气相色谱方面的研究和应用作了综述,本综述分3部分叙述,本篇为第Ⅱ部分,包括：5．中药中有效成分的气相色谱分析。6．西药的气相色谱分析。7．气相色谱在食品中有害物质分析的应用。     

多种气相色谱联用技术分析陕西刺五加茎挥发油的化学成分

采用气相色谱/四极杆质谱(GC/qMS)、气相色谱/正交加速飞行时间质谱(GC/oaTOFMS)和气相色谱/傅里叶变换红外光谱(GC/FTIR)联用技术,对一种陕西产刺五加Acanthopanax senticosus (Rupr. et Maxim.) Harms茎挥发油的化学成分进行了分析。基于GC/qMS谱库的检索功能,结合GC/FTIR在结构鉴别上的优势和GC/oaTOFMS对质谱碎片离子精确的质量测定功能,成功地实现了对68个色谱组分的定性分析。与使用单一的联用技术(例如GC/qMS)相比,利用多种色谱联用技术在定性分析上的互补性,可以明显提高对组成复杂的挥发油类样品分析的可靠性。     

国内石化分析中的气相色谱技术进展

气相色谱(GC)技术在石化分析领域的应用是较为普及的,随着气相色谱技术本身的不断成熟,其在石化分析中的应用也日益普遍。以标准化专用色谱柱和多维色谱切换技术为基础,针对行业特定应用需求开发各种专用色谱分析系统和应用包,是近年来石化分析领域色谱技术应用的一个显著特点。这是专业化分工与商品化服务结合后给色谱技术工业化应用带来的新气象,可最大限度地降低对操作人员的技术要求、促进分析系统开发的专业分工。与这种趋势相应,国内石化行业的GC应用工作也有同样的特点。总体来看,专用系统的硬件平台以国外主要仪器生产厂的产…     

Analysis of coal tar and petroleum pitches by computerized pattern recognition

Pyrolysis gas chromatography (P/GC) has been successful in differentiating coal tar pitches which are used in the manufacture of high temperature graphite materials [1,2]. In the present study, coal tar and petroleum pitches received from five suppliers were readily differentiated using three distinct methods of polymer analysis: dynamic headspace and pyrolysis gas chromatography mass spectrometry (DH/GC/MS and P/GC/MS, [3]), and pyrolysis mass spectrometry (P/MS, [4,5]). All of these methods are appropriate for the analysis and pattern recognition study of coal and petroleum products; however, methods which incorporate GC usually necessitate long analysis times and are subject to problems associated with gas chromatographic reproducibility (e.g. active sites [6], and nonconstant retention times). As a fingerprint analysis method, P/MS is rapid and ideally suited to computerized pattern recognition study of pitches due to the simple format of P/MS data (computer tabulation of normalized intensities versus masses); whereas, in the present study, the normalized peak area versus retention time date from DH/GC/MS and P/GC/MS analyses were not suitable for direct input to a computerized pattern recognition analysis program, (due to non-constant retention times and improper data format). One limitation is that P/MS does not provide positive identification of thermally evolved products (as can DH/GC/MS and P/GC/MS) due to the complexity of the spectra of a mixture of compounds produced by P/MS. Within the limits of the commercial instrumentation and computer programs used in this study, a combination of all three techniques provided the greatest capability for the differentiation of the five coal tar and petroleum based pitches studied.     

全二维气相色谱在石油地质样品分析中的应用进展

对石油地质样品的化学组成进行全面准确的剖析,可以获得丰富的地球化学信息,为油气勘探工作提供科学依据。然而,该类样品除了组成复杂之外,还易受到各种物理（如蒸发、乳化、扩散、溶解和吸附）、化学（如光降解）和生物（如微生物降解）过程的影响。这些特点给样品的分析研究工作带来了极大的困难,传统的一维气相色谱/质谱技术很难对其进行理想的分离。全二维气相色谱（GC×GC）作为新发展起来的一种分离技术,在复杂样品分析方面具有独特的优势,虽然在石油地质样品分析中的应用相对较晚,但也日益受到关注。本文主要综述了近5年来GC×GC在石油地质方面国内外的研究进展以及存在的主要问题,并对今后的研究进行了展望。     

New valve switching modulator for comprehensive two-dimensional gas chromatography

This paper describes a new design for a valve switching modulation system developed for comprehensive two-dimensional gas chromatography (GC x GC). This system is based on the differential flow and is different from the earlier reported in the literature. It has several advantages and constructed of inexpensive, commercially available parts that are easily installed on most gas chromatographs. Operation is easy and robust and requires no external coolants. This new design allows GC x GC analysis to be conducted in any laboratory environment capable of supporting conventional GC and imposes no additional consumable costs. The system is flexible and permits the use of a wide range of stationary phase combinations. The system has been successfully tested for complete material transfer and is suitable for quantitative analysis. The flexibility of this system is demonstrated using several test mixtures that show its extended application in petroleum, biochemistry, and environmental studies.     

全二维气相色谱用于轻质石油馏分中芳烃含量的测定

建立了采用全二维气相色谱(GC×GC)技术一次进样完成轻质石油馏分中非芳烃、一环芳烃和二环芳烃的分离、定性 和定量。通过对柱系统的选择和色谱条件的优化,实现了一次全二维气相色谱分析即完成轻质石油馏分的族组成分离以及 目标化合物的分离。方法的加标回收率为89.5%～106.1%;样品中各组分含量重复测定的相对标准偏差均不大于5.8%,能 够满足样品测定的精密度和准确性要求,且完成1次分析最多只需要30 min。     

Universal and discriminative detection using a miniaturized pulsed discharge detector in comprehensive two-dimensional GC

A miniaturized pulsed discharge detector (Mini-PDD) has been successfully demonstrated for comprehensive 2-D GC (GC x GC) analysis of pyrolysis gasoline and the pyrolysis GC x GC analysis of a polyethylene copolymer. The detector cell volume of the Mini-PDD is reduced to 25% of the Valco plug-in PDD D-3. An n-C11 peak width at base is 96 ms for the Mini-PDD, about 23% larger than a peak width of 78 ms detected by a flame ionization detector (FID). The Mini-PDD has sufficient response time for most GC x GC applications. When Mini-PDD is operated in helium photoionization mode (Mini He-PDD), it is a universal detector for both inorganic and organic compounds. This is especially useful when detection of water is needed in GC x GC applications. When krypton is doped in the helium discharge gas (Mini Kr-PDD), it can suppress signals of compounds having higher ionization potentials and enhance relative signal intensities of aromatic compounds. The determination of aliphatic to aromatic hydrocarbon ratios is essential to the operation of petroleum crackers. Comparison of the signal from two modes of the Mini-PDD is a simple and fast way to verify the location of aromatics in comprehensive 2-D gas chromatograms.     

Gas chromatographic retention of alkyl phosphates on ionic liquid stationary phases

Retention behaviors of alkyl phosophates were studied on a series of ionic liquid gas chromatography columns. The selectivity of the IL columns for alkyl phosphates were compared with a 5% phenyl column as a route to evaluating the potential use of IL columns in the analysis of alkyl phosphates in petroleum samples in both one- and multi-dimensional GC. Most interestingly, we demonstrate for the first time the dependence of elution order on separation temperature for members of a homologous series of compounds. At low temperatures it was found that trihexyl phosphate eluted before trioctyl phosphate, while at higher temperatures this pattern was reversed.     

High-temperature two-dimensional gas chromatography of hydrocarbons up to nC60 for analysis of vacuum gas oils

In a tense energetic context, the characterization of heavy petroleum fractions becomes essential. Conventional comprehensive two-dimensional gas chromatography (2D-GC or GC × GC) is widely used for middle distillates analysis, but only a few applications are devoted to these heavier fractions. In this paper, it is shown how the optimization of GC × GC separation allowed the determination of suitable high-temperature (HT) conditions, adjusting column properties and operating conditions. 2D separations were evaluated using 2D separation criteria and a new concept of 2D asymmetry (As_2D). New HT conditions allowed the extension of GC × GC range of applications to heavier hydrocarbons, up to nC₆₀. A first application of high-temperature two-dimensional gas chromatography (HT-2D-GC) to a full vacuum gas oil (VGO) feed stock is described. Comparisons with other standardized methods illustrate the high potential of HT-2D-GC for heavy fractions analysis.     

Applications of comprehensive two-dimensional gas chromatography to the characterization of petrochemical and related samples

This article discusses the application of comprehensive two-dimensional gas chromatography (GC x GC) to samples derived from petrochemicals. The use of GC x GC for characterization of petroleum and petroleum derivatives, through group type analysis, such as benzene, toluene, ethylbenzene, xylenes (BTEX), total aromatic hydrocarbons, polyaromatic hydrocarbons, and heteroatomic sulfur-, oxygen-, and nitrogen-containing compounds is presented. The capability of GC x GC to provide additional chemical-specific information regarding petroleum-processing steps, such as linear alkanes dehydrogenation, Fischer-Tropsch process, hydrogenation and oligomerization, is also described. In addition, GC x GC analyses of petrochemical biomarkers and environmental petrochemical-derived pollutants are reported. The role of comparison of samples through use of simple fingerprint approaches is highlighted.