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1.
夏丹  高丽荣  郑明辉 《色谱》2017,35(1):91-98
持久性有机污染物(POPs)组分复杂,在自然界中超痕量存在,其分离分析十分困难。全二维气相色谱(GC×GC)作为一种新型色谱技术,与传统的一维气相色谱相比,具有峰容量大、分辨率和灵敏度高等优势,越来越广泛地应用于环境有机污染物的分析。该文综述了近十年来全二维气相色谱在持久性有机污染物分析中的应用进展,主要包括全二维气相色谱在解决一些复杂POPs定性定量分析难题方面的应用,如二恶英、毒杀芬和短链氯化石蜡等;概述了全二维气相色谱对多种POPs同时定性定量分析的应用进展;讨论了全二维气相色谱在非目标有机污染物筛查分析中的应用,并对发展趋势及相关应用前景进行了总结展望。  相似文献   

2.
刘布鸣  苏小川 《色谱》2006,24(2):211-211
多廿醇是从制糖滤泥中分离得到的一种高级脂肪伯醇天然混合物,其化学组成分析未见报道。本文采用气相色谱法(GC)和气相色谱/质谱法(GC/MS),对其组分和结构进行了分析和鉴定。  相似文献   

3.
全二维气相色谱用于轻质石油馏分中芳烃含量的测定   总被引:2,自引:0,他引:2  
李艳艳 《色谱》2006,24(4):380-384
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。  相似文献   

4.
李海静  刘国柱  张香文 《色谱》2018,36(8):780-785
采用全二维气相色谱-质谱联用(GC×GC-MS)考察了色谱柱系统、程序升温条件和调制周期3个主要因素对样品组分分离结果的影响,建立了煤油基吸热型碳氢燃料烃族组成的定性分析方法,并利用GC×GC-FID通过有效碳数校正因子对烃族组成进行定量。对选取的9种燃料的分析结果表明,该方法对链烷烃和环烷烃的定量结果与标准方法ASTM D2425的结果高度一致,相对误差基本均在±10%以内。利用该方法计算的碳含量结果与元素分析法相比误差均在0.5%以下。该方法无需复杂的前处理,稀释后可直接进样分析,操作简单,而且可直观地看出不同样品之间的差异,为改进燃料的性能提供了必要的分析手段。  相似文献   

5.
石油样品全二维气相色谱分析的分离特性   总被引:13,自引:0,他引:13  
汽油、柴油等石油产品是典型的复杂混合物体系。一维气相色谱 (1DGC)分离能力不够 ,重叠十分普遍 ,定性不准确 ,族之间也不能分离干净。研究了全二维气相色谱 (GC×GC)用于石油样品分析的分离特性。对一特定的石脑油进行研究 ,一次进样实现了烷、环烷和芳烃 (PNA)的族分离。与 1DGC比较 ,GC×GC的正交分离、族分离、瓦片效应等特性使其峰容量大、灵敏度高、定性更简单准确 ,适合复杂混合物体系的分析 ,也是一种检测痕量杂质的有效手段。  相似文献   

6.
通过优化GC×GC的柱系统、温度程序和调制参数等色谱条件,建立了分析中药莪术挥发油组成的全二维气相色谱/飞行时间质谱(GC×GC/TOFMS)方法,实现了莪术挥发油的单个组分与族组分分析.采用所建立的GC×GC/TOFMS方法,鉴定出匹配度大于800的组分有249种,其中单萜18种,单萜含氧衍生物34种,倍半萜35种,倍半萜含氧衍生物37种,有69种组分的体积分数大于0.02%.  相似文献   

7.
超临界流体色谱在生物工程中应用的新进展   总被引:4,自引:0,他引:4  
超临界流体色谱(SFC)是高效液相色谱(HPLC)和气相色谱(GC)的重要补充技术。用SFC可以分离多数不能用GC分离的低挥发性物质。与传统的HPLC相比,SFC的分离速度更快、效率更高。本文综述了SFC在生物分子分离分析方面应用的新进展。引用文献74篇。  相似文献   

8.
本文报道了用GC/FTIR方法分析气相催化氨化合成的CFC12的替代物HFC134a粗产品、中间体及副产物的化学组成。该法选择石英PLOTAl2O3柱(35mX0.32mm)分离、FID检测。分析结果表明:上述样品基本上是C1~C2的CFCs复杂混合物。由于采用不分流进样、不加补偿气、适当增大进样量及计算机差谱等技术,使各种样品的可检出组分合计达24种以上并确定了其中20种组分的分子结构。已确定组分一般都占所分析样品色谱总馏出峰面积的95%以上。  相似文献   

9.
全二维气相色谱法用于不同石油馏分的族组成分布研究   总被引:17,自引:0,他引:17  
一直以来采用化学法、色谱法或质谱法等多种方法联用分析不同石油馏分中一 些目标化合物和芳烃含量,但这些方法操作繁琐,迫切需要改进。作者采用全二维 气相色谱方法(GC×GC)研究不同沸程范围的蒸馏汽油、煤油柴油和裂化柴油的烷 烃(P)、烯烃+环烷烃(O+N)和1-4环芳烃(A)的族分离新方法。经过对柱系 统进行选择和对色谱条件进行优化,一个GC×GC方法即可实现对不同石油馏分的族 组成分离和目标化合物分离。用标准物对油品中一些特征组分进行定性,并对特征 组分和不同沸程的石油馏分的P,(O+N),A族组成进行定量和比较,定量结果的 相对标准偏差(RSD)≤2.3。一个GC×GC方法便可完成原来要几个美国测试和材料 协会(ASTM)方法才能完成的任务。  相似文献   

10.
建立了烟叶中酸性化合物(挥发性、 半挥发性羧酸类和酚类)组成研究的全二维气相色谱/飞行时间质谱(GC×GC-TOFMS)分析方法, 并用此方法对香料烟中的酸性化合物进行了表征. 用同时蒸馏萃取样品的前处理方法, 采用TOFMS谱图库检索结合全二维特有的包含结构信息的二维谱图, 通过族分离和结构谱图, 鉴定出了香料烟中143种挥发性及半挥发性酸性组分, 包括10种酸酐和呋喃二酮, 43种有机酸和90种酚类化合物. 同时对不同类别的化合物在二维气相色谱上的分布模式进行了研究. 结果表明, 全二维气相色谱飞行时间质谱的高分辨率非常适合于烟叶这类复杂体系的分离分析.  相似文献   

11.
近两年国内气相色谱的进展   总被引:1,自引:0,他引:1  
傅若农 《分析试验室》2011,30(5):88-122
对近两年国内学者对气相色谱(GC)的研究和应用进行了综述.GC已经是一门十分成熟和广泛应用的分析技术,近两年国内学者的研究发展近似于国外的GC研究和发展,基础性GC研究不多,大多为GC在各个领域的应用研究.应用研究包括在食品、中药、水、气、石油、石化、工业品、农残和烟草分析中的应用.  相似文献   

12.
谢园园  花磊  陈平  侯可勇  蒋吉春  王艳  李海洋 《色谱》2015,33(2):188-194
建立了一种气相色谱(GC)与单光子电离-飞行时间质谱(SPI-TOF MS)联用(GC/SPI-TOF MS)的分析方法。首先,设计了一种双层套管的传输管用于连接GC与SPI-TOF MS,实现了GC与单光子电离离子源的无缝连接。在此基础上,以n-十五烷标准品和苯/甲苯/二甲苯的标准气为对象,对电离源的重要电压参数进行了优化,得到了纯净的分子离子峰,实现了对各类有机物的快速和准确定性。最后,将该方法用于分析柴油中的挥发性与半挥发性有机物,获得了柴油组分的二维GC×SPI-TOF MS谱图。不需要复杂的谱图解析和数据处理,根据谱图中离子的质荷比(m/z)归纳了柴油的主要成分,包括脂肪烃、芳香烃和含量很低的苯并吡咯等含氮化合物;根据色谱的保留时间将柴油中的同分异构体区分开来。结果表明GC/SPI-TOF MS法是一种简单、有效的分析方法,非常适于柴油及复杂环境样品等的分析表征。  相似文献   

13.
The detailed characterisation of middle distillates is essential for a better understanding of reactions involved in refining process. Owing to higher resolution power and enhanced sensitivity, comprehensive two-dimensional gas chromatography (GC x GC) is a powerful tool for improving characterisation of petroleum samples. The aim of this paper is to compare GC x GC and various ASTM methods -- gas chromatography (GC), liquid chromatography (LC) and mass spectrometry (MS) -- for group type separation and detailed hydrocarbon analysis. Best features of GC x GC are demonstrated and compared to these techniques in terms of cost, time consumption and accuracy. In particular, a new approach of simulated distillation (SimDis-GC x GC) is proposed: compared to the standard method ASTM D2887 it gives unequal information for better understanding of conversion process.  相似文献   

14.
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.  相似文献   

15.
李海静  张香文 《色谱》2017,35(8):867-874
采用全二维气相色谱-质谱联用仪(GC×GC-MS),通过优化程序升温和调制周期,建立了喷气燃料裂解产物中芳烃的定性定量分析方法。该方法对多环芳烃(PAH)同分异构体具有良好的分离能力。利用MS检测器谱库检索结果、芳烃标准品及相关的文献报道,对喷气燃料裂解产物中常见的单环芳烃、二环芳烃、三环芳烃及四环芳烃等共27种芳烃进行了准确定性,并利用外标GC×GC-FID法对其进行定量。定量结果表明,芳烃含量均随着裂解产气率的增加而增大,当裂解产气率达到22%时,二环芳烃开始产生,且其含量随着裂解产气率的增加呈指数形式增加。该方法与传统的气相色谱-质谱相比,具有更好的分离及定性能力,可应用于复杂样品的分离及其定性定量分析。  相似文献   

16.
In a context of environmental preservation, purification and conversion of heavy petroleum cuts into high‐quality fuel becomes essential. The interest for the characterization of those very complex matrices becomes a trendy analytical challenge, when it comes to get molecular information for the optimization of industrial processes. Among new analytical techniques, high‐temperature 2‐D GC has recently proved its applicability to heavy petroleum matrices, but lacks in selectivity to separate all chemical groups. To gain resolution, heart cutting is demonstrated for LC separation of saturated, aromatic and polar compounds prior to high‐temperature 2‐D GC. Therefore, an extended global resolution was obtained, especially by a better distinction of saturated compounds. This includes iso‐paraffins and biomarker polynaphthenic structures, which are impossible to quantify with MS methods. This new way to analyze heavy petroleum fractions gives innovative opportunities for the construction of global weight distributions by carbon atoms number and by chemical families. This can right now be employed for quantitative analysis of heavy petroleum fractions and for studying conversion processes.  相似文献   

17.
Several recently developed analytical techniques, based on high-end mass spectrometry and chromatography, for dealing with challenges in petroleum characterization are reported. Folded flight path time-of-flight mass spectrometry provides resolving power up to 100000, enabling accurate mass measurement for molecular formula determination with high confidence. Atmospheric pressure chemical ionization (APCI) can be used in both gas chromatography (GC, as APGC) and liquid chromatography (LC) for analyzing non-polar hydrocarbons as well as polar compounds. The improvement in chromatography facilitates the mass spectrometric analysis through online coupling. Comprehensive two-dimensional gas chromatography (GC×GC) resolves overlapping components, rendering accurate identification and quantitation. Supercritical fluid extraction has been developed as an alternative method to replace traditional solvent extraction methods and eliminate the use of large volumes of solvents that can be harmful to health and environment. Supercritical fluid chromatography (SFC) has been developed as a convergence of GC and LC chromatographic techniques. The use of SFC for heavy oils and residua has been demonstrated. Prospective developments in the use of mass spectrometric and chromatographic methods for petroleum characterization are also described.  相似文献   

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