气相色谱-裂解气相色谱联用定性参数的研究

〕研究了实验条件对气相色谱-裂解气相色谱联用的定性参数的影响,由于组分的各裂解产物的相对保留值在多数实验条件改变时重现性良好,可作为实际定性的主要依据,而裂解产物的相对峰面积可作为定性的辅助依据。     

气相色谱一四温裂解气相色谱联用仪

本文用四个并联的蒸气相裂解器在气相色谱—裂解气相色谱联用装置,四个裂解器的温度为406.554,658及768℃,解决了实用的气相色谱—裂解气相色谱联用分析要求有普遍适用的裂解温度的问题,同时得到较多较大的裂解色谱峰,使定性更加准确。     

气相色谱—四温裂解气相色谱联用分析

本文利用气相色谱—四温裂解气相色谱联用仪对一些混合物作定性分析,此方法可用来作气相色谱难分离物质的鉴定。     

裂解同时烷基化气相色谱/质谱鉴定醇酸树脂

 用裂解同时烷基化气相色谱-质谱联用技术（SPM-GC-MS）对不同类型的醇酸树脂进行分析研究,将衍生化试剂四甲基氢氧化胺与样品同时裂解,经高效毛细管气相色谱分离,质谱鉴定,可区分醇酸树脂中的多元醇、多元酸、植物油类型,由此对改性醇酸树脂作结构鉴定。与直接裂解-气相色谱-质谱联用技术比较,具有样品前处理快速、简单,用量少,灵敏度高,定性准确,谱图直观等特点。     

低分子有机物的裂解色谱定性

裂解色谱多用于不挥发的合成、天然和生物高分子的分析和鉴别,裂解色谱-质谱联用也有用于气相分子裂解反应的研究,裂解色谱作为低分子有机物的定性方法则尚未见报道。 本文用气相色谱将混合物分离,再用裂解色谱将分离的组分逐个得出裂解反应产物的色谱图,与标准物裂解色谱指纹图比较,可以得到混合物各组分的定性结果。本法设     

低分子有机物的裂解色谱定性

裂解色谱多用于不挥发的合成、天然和生物高分子物质的分析和鉴别,裂解色谱一质谱联用也已用于气相分子裂解反应的研究[1+3],裂解色谱作为低分子有机物的定性方法尚未见报导。本文作出了15类同系物数+种化合物的裂解色谱图,发现低分子有机物在一定的裂解色谱条件下有确定的指纹图,可以作为一种新的定性方法。本方法灵敏度高、设备简单。     

色谱与色谱/质谱法相结合分析热裂解汽油C9馏分

采用毛细管气相色谱-氢火焰离子化检测器（CGC-FID）和气相色谱-质谱法(GC/MS)分析了热裂解汽油C9 馏分的组成。实验使用PONA毛细管气相色谱柱(100 m×0.25 mm i.d.×0.5 μm),根据烃类化合物在PONA柱上的保留规律,以正构烷烃标样保留值作为碳数分布依据,定量分析了裂解汽油C9 馏分中烃类化合物的碳数分布和单体烃含量;用GC/MS联用技术和CGC保留值定性法相结合对裂解汽油C9 馏分中相对含量大于0.2%的39种化合物进行了定性。     

高聚物的二氧化碳激光裂解气相色谱研究

本文报导用二氧化碳激光作为裂解气相色谱的一种新型裂解源.由于二氧化碳激光的能量能够为透明或半透明的有机化合物所直接吸收,因而克服了红宝石激光或钕玻璃激光在裂解时所遇到的固有困难.一系列定性及定量的裂解谱图数据表明,二氧化碳激光裂解气相色谱对高聚物和其它不挥发性有机物质的研究是一种有用的技术.它在我们实验室有效地鉴别高聚物已逾四年.     

裂解气相色谱/质谱法检验复印墨粉

复印墨粉检验分析在经济案件侦查以及墨粉配方研究方面具有十分重要的意义。采用裂解气相色谱技术,对收集到的复印墨粉进行分离分析,并用裂解气相色谱/质谱联用技术,对所得裂解峰进行归属。分析结果的重复性与稳定性良好,复印件上墨粉与原墨粉分析结果一致。对不同厂家与牌号的墨粉进行区分与归类,为墨粉鉴别提供了依据。     

用气相色谱-质谱和气相色谱-红外联用技术分析热裂解汽油C9馏分中的组成

采用气相色谱-质谱和气相色谱-红外联用技术对热裂解汽油C9馏分中的组分进行分离和定性分析。实验使用了50m聚甲基硅氧烷毛细管色谱柱,EI电离源,电离能70eV和10eV,红外光谱仪的检测器为MCT。通过分析确定了热裂解汽油C9馏分中52个化合物的结构。降低质谱的电离能有利于确定组分的分子量。质谱可以提供被测组分的裂解碎片离子和分子量的信息,红外在确定官能团和同分异构体时要优于质谱。两种联用技术的使用较好地解决了单一方法测定复杂混合物中组分结构所存在的缺陷。     

裂解气相色谱—裂解毛细柱气相色谱联用仪

设计了一种裂解气相色谱--裂解毛细柱气相色谱联用仪。在第一级裂解气相色谱仪把聚合物裂解并分离裂解产物,分离了的产物用六通气体进样阀选取并逐个在第二级裂解气相色谱仪裂解,得到聚合物裂解产物的裂解气相色谱图。与低分子化合物的标准指纹图比较,这些裂解产物就得到确认,这样,就可以充分肯定地推断复杂聚合物的组成。     

Qualitative and quantitative analysis of pyrolysis oil by gas chromatography with flame ionization detection and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry

Pyrolysis oils have attracted a lot of interest, as they are liquid energy carriers and general sources of chemicals. In this work, gas chromatography with flame ionization detector (GC-FID) and two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) techniques were used to provide both qualitative and quantitative results of the analysis of three different pyrolysis oils. The chromatographic methods and parameters were optimized and solvent choice and separation restrictions are discussed. Pyrolysis oil samples were diluted in suitable organic solvent and were analyzed by GC×GC-TOFMS. An average of 300 compounds were detected and identified in all three samples using the ChromaToF (Leco) software. The deconvoluted spectra were compared with the NIST software library for correct matching. Group type classification was performed by use of the ChromaToF software. The quantification of 11 selected compounds was performed by means of a multiple-point external calibration curve. Afterwards, the pyrolysis oils were extracted with water, and the aqueous phase was analyzed both by GC-FID and, after proper change of solvent, by GC×GC-TOFMS. As previously, the selected compounds were quantified by both techniques, by means of multiple point external calibration curves. The parameters of the calibration curves were calculated by weighted linear regression analysis. The limit of detection, limit of quantitation and linearity range for each standard compound with each method are presented. The potency of GC×GC-TOFMS for an efficient mapping of the pyrolysis oil is undisputable, and the possibility of using it for quantification as well has been demonstrated. On the other hand, the GC-FID analysis provides reliable results that allow for a rapid screening of the pyrolysis oil. To the best of our knowledge, very few papers have been reported with quantification attempts on pyrolysis oil samples using GC×GC-TOFMS most of which make use of the internal standard method. This work provides the ground for further analysis of pyrolysis oils of diverse sources for a rational design of both their production and utilization process.     

气相色谱仪检定结果的不确定度评定

气相色谱仪检定结果的不确定度主要来源于流速稳定性、柱箱温度稳定性、基线噪声、定量重复性和标准物质进样量的不确定度。以TCD检测器为例进行分析,对气相色谱仪检定结果的不确定度进行评定,相对扩展不确定度为5%。     

A new method for solvent-free application of polymers and inorganic materials to ferromagnetic wires used for pyrolysis-capillary gas chromatographic studies

A method is described that enables soluble and insoluble samples to be applied to ferromagnetic wires. The principle of the method consists in pressing the sample on to a flattened Curie-point wire at a pressure of 15 tonnes. It is shown that this method is suitable for a wide variety of polymers and for inorganic materials. As the pyrolysis—gas chromatographic results obtained are not only influenced by the pyrolysis itself but also to a large extent by the gas chromatographic process, a number of considerations are given with respect to the use of capillary gas chromatography in combination with a Curie-point pyrolyser. The sample application technique described has also been used to check the inertness of the chromatographic system by the preparation of Curie wires loaded with Tenax. These wires have been used for the “injection” of volatile compounds, such as a Grob mixture, with the pyrolyser system.     

Introduction to pyrolysis-capillary gas chromatography.

By breaking large molecules into characteristic smaller fragments, analytical pyrolysis extends the use of gas chromatography to the analysis of polymeric materials, including natural polymers such as cellulose as well as synthetics. An understanding of the chemistry involved permits interpretation of the information present in these molecular fragments, with application to polymer and copolymer microstructure in addition to routine identification and quality control. Whether microfurnace, Curie-point or resistively heated filament, the pyrolysis device must be interfaced efficiently to the gas chromatography to make use of the resolving power afforded by capillary columns.     

Pyrolysis—gas chromatography of quaternary ammonium salts in aqueous solution

The pyrolysis of a range of simple quaternary ammonium salts in aqueous solution has been studied by gas chromatographic procedures. The results indicate that the structure of the cation governs the thermal stability and breakdown pattern of the salts, the nature of the anion having no apparent effect on the process. The mechanism of the decomposition is discussed as is the potential of aqueous pyrolysis—gas chromatography for analytical studies of quaternary ammonium salts in general.     

裂化气、乙炔尾气及产品乙炔中H_2S、CS_2的测定

原料天然气常含有300mg/m~3以上的硫化氢、甲硫醇、乙硫醇、甲硫醚、乙硫醚等硫化物,经脱硫精制处理后,仍有少量硫化物转入到裂化气、尾气、产品乙炔中。这些硫化物的存在对甲醇合成触媒和醋酸乙烯合成触媒均有不利影响。因此,硫化物的检测对生产控制极为     

A REVIEW OF CAPILLARY AND PACKED COLUMN GAS CHROMATOGRAPHS

In this review, the essential aspects of gas chromatography are discussed. The article begins with a very brief discussion of basic chromatographic theory, followed by an in-depth treatment of the instrumentation involved. This discussion starts a discussion of chromatographic columns, the distinctions among which are used to classify the different modes of gas chromatography. Following this is an in-depth discussion of instrumentation, the treatment of which follows the classification by column types. This discussion includes the operational principles and applications of injectors, detectors and data handling systems. In conclusion, a listing of suggested further reading is provided.