一种快速分离和富集萘系和菲系化合物的小型氧化铝柱层析法

使用了一种易于操作、成本低的小型柱色谱法将原油中萘系和菲系化合物快速分离的技术。色谱质谱检测结果表明,该技术能使原油中萘系和菲系化合物得到完整的分离和纯化富集,达到了芳烃单体烃在色谱-同位素质谱(GC-IRMS)中分析的要求,为测定芳烃单体烃同位素值提供一种较为可靠的前处理方法。     

不同沉积环境烃源岩芳烃馏分单体烃碳同位素分布特征及其意义

通过对来自塔里木盆地海相(9个)、吐哈盆地沼泽相及湖相(6个)和柴达木盆地湖相(9个)共24个烃源岩样品芳烃分离、纯化后,应用色谱-同位素比值质谱(GC-IR-MS)分析技术,系统剖析了不同沉积环境中芳烃馏分单体烃碳同位素组成特征。研究结果表明,对于不同沉积环境的烃源岩芳烃馏分单体烃碳同位素组成呈现出δ13 C湖相>δ13 C沼泽相>δ13 C海相的规律,由此证明母质来源和沉积环境是影响其分布的主控因素之一。不同沉积环境1,6-DMN、1,2,5-TMN、1-MP、9-MP和1,9-DMP化合物的碳同位素组成具明显差异。芳烃同分异构体之间的同位素组成差异主要由沉岩过程中的动力学分馏效应所致,而热演化过程对芳烃单体烃碳同位素组成影响不大。     

气相色谱法分析轻油抽提芳烃中萘系物

采用５０ｍ排极性弹性石英毛细柱分析催化裂解（ＤＣＣ）轻油中抽提芳烃〈２８０℃馏分中萘系物的分布,面积归一化法定量测定萘系物的组成。借助质谱对芳烃馏分健康的各组分定性,将定性数据输入计算机,在气相色谱仪上可直接进行芳烃组成分析。     

饱和烃和芳烃的高压液相色谱法精细分离

该文介绍了用高压液相色谱对族组分中的饱和烃、单环芳烃、二环芳烃及三环以上芳烃的精细分离方法。用二级活度的氧化铝除去非烃和沥青质,用正己烷和二氯甲烷依次淋洗出(硅胶)色谱柱上的饱和烃、单环芳烃、二环芳烃及三环以上芳烃。该方法同国外方法相比具有快速、节省试剂的优点,色质谱图显示各组分有较高的分离度。     

原油轻烃单体系列GC/C/MS在线碳同位素分析方法

本文系统介绍了GC-delta S型气体同位素质谱仪的GC/C/MS在线碳同位素分析方法。该方法可获得良好的精度和准度,从各类混合烃类样品中获得大量单体烃的碳同位素数据,为油气地球化学研究提供了丰富的科学信息。     

轻烃单体烃碳同位素分析新方法问世

2005年8月18日，中国石化勘探开发研究院无锡石油地质研究所研究成功一种能够分离析出40多个轻烃组分的轻烃单体烃碳同位素分析新方法，并在有关油气田和地质应用中取得了较为满意的分析效果。     

沉积物中16种多环芳烃单体碳同位素GC-C-IRMS测定

为监测海洋沉积物中的多环芳烃（PAHs）、追踪污染物来源并控制污染,建立了沉积物中16种多环芳烃单体碳同位素GC-C-IRMS测定方法。首先采用EA-IRMS联用技术对16种多环芳烃单体碳同位素进行了定值,偏差范围在0.03‰~0.15‰（n=10）,小于0.2‰;再用该16种多环芳烃混标,运用GC-C-IRMS联用技术考察了高效薄层色谱、气相色谱进样体积、无分流时间、进样浓度等可能产生的同位素分馏,结果表明,整个方法并无明显的同位素分馏现象。根据不同浓度PAHs混标在GC-C-IRMS测定中的变化与EA-IRMS测定的差,建立了数据校正曲线,其R²大于0.99,并应用于沉积物中16种多环芳烃单体碳同位素的测定,测试数据为海域沉积物中多环芳烃溯源提供了有力证据。     

单体烃碳同位素的技术开发与应用

通过用引进的稳定碳同位素比质谱仪对毛场一马王庙地区及岳口低凸起上原油单体烃碳同位素样品正构烷烃系列的前期处理,优化并确定分析条件,以及平行性、重复性的研究,建立了碳、氢、氧、氮同位素分析方法,样品类型包括原油、烃源岩、天然气等。单体烃碳同位素分析技术在江汉油田是首次建立,填补了江汉油田稳定碳同位素分析方法的空白,它是一种十分精细、严谨的技术支撑。原油单体烃碳同位素分析技术在油源对比等地质应用方面具有可行性,同时体现出有效的实际应用价值。     

塔北隆起北缘原油轻烃单体烃碳同位素特征

对塔北隆起北缘原油进行了轻烃单体烃碳同位素组成分析,刻画了原油的轻烃组成特征.所有轻烃化合物中,环戊烷系列化合物碳同位素在不同原油之间差异最小,对原油成因的鉴别意义小于其他化合物.优选的其他化合物碳同位素在不同成因原油中呈现出显著规律,轮台油气田煤成油轻烃单体烃碳同位素较重,主要位于-21‰-19‰之间;大涝坝油气田湖相油次之,位于-25‰-21‰之间;雅克拉油气田海相油最轻,位于-31.5‰-28‰之间.典型寒武系—下奥陶统来源的YN2井原油分布特征独特.上述分布特征揭示轻烃单体烃碳同位素组成可作为可靠的原油成因判识指标,尤其对于凝析油与轻质油更为有效.     

不同沉积环境生成的原油单体烃碳同位素分布特征

本文应用原油单体烃类的气相色谱和同位素质谱在线分析技术(GC/C/MS),通过对原油单体烃类碳同位素分布的讨论,初步按其源岩的沉积环境进行了成因分类,这在油-油、油-源对比中,不失为一个有效的方法。     

芳香族化合物绿色氧化技术研究进展

综述了芳香族化合物绿色氧化技术的研究进展,重点讨论了芳香族化合物在超临界水、超临界二氧化碳和离子液体中的氧化,同时探讨了芳香族化合物的臭氧和过氧化氢氧化技术。     

正构烷烃分布模式判断柴西主力烃源岩

柴西原油正构烷烃分布多呈偶奇优势(CPI<1),而烃源岩样品则多呈奇偶优势分布,只有少数呈偶奇优势分布。从正构烷烃分布模式出发,结合单体烃碳同位素分析,对柴西原油和烃源岩进行对比,以确定柴西原油形成的主力烃源岩。研究表明,柴西深层主力烃源层为E23,次要烃源层为E1+2和N31;浅层主力烃源层为N1,次要烃源层为N2。从生烃性能角度看,正构烷烃分布呈偶奇优势的烃源岩样品,其有机碳、氯仿沥青"A"、总烃含量、转化系数等都比呈奇偶优势分布的样品高,生烃性能较好,应为柴西主力烃源岩。     

基于反相柱系统分析的原油烃类化合物全二维色—质谱图特征

原油中烃类化合物是最复杂的混合物体系,而全二维气相色谱—飞行时间质谱是目前分离复杂混合物体系的最有效方法之一。该文采用反相柱系统对原油烃类化合物进行了详细分析,并对其中重要的化合物系列进行了识别,为原油中烃类化合物的反相柱系统分析和谱图识别提供了参考。分析结果表明,反相柱系统对饱和烃,尤其是低分子量的异构烷烃和环烷烃等化合物在二维上具有很好的分离效果,因此,反相柱系统对生物降解油饱和烃馏分的"鼓包"化合物(UCM)的分离与研究可能将起到一定作用。      

东濮凹陷北部芳烃色谱-质谱分析及石油地质应用

芳烃生物标志物热稳定性好、抗降解能力强,指标参数可持续应用到干气阶段,尤其是东濮凹陷深层热演化程度高。开展芳烃生物标志物研究就更为重要。通过对东濮凹陷北部深层原油及烃源岩芳烃气相色谱-质谱分析,鉴定出约200种芳烃系列化合物．确立出芳烃生物标志物在研究区有效的石油地质应用指标。研究认为,该区芳烃组成以三环芳烃为主,浅层芳甾类化合物较多,三芴系列相对组成中以高硫芴为特征,三方甾烷参数、甲基菲指数及烷基二苯并噻吩化合物比值均可作为该区有机质热演化特征研究的有用指标。     

气相色谱技术在聚合级气态烯烃原料分析中的应用进展

介绍了聚合级气态烯烃原料中杂质的形成原因及其对聚烯烃催化剂活性的影响。根据气态烯烃原料中不同杂质的类型,阐述了气相色谱技术在烃类化合物分析、硫化物分析、氧化物分析、氯化物分析、氮化物分析、砷化氢和磷化氢分析、CO和CO2分析、水含量分析、进样系统及定量分析中的应用现状与可能的发展趋势。     

国内聚烯烃管材料市场分析及应对措施

对国内外聚烯烃管材生产技术及市场需求现状进行了深入研究和分析,重点剖析国外进口管材料对我国聚烯烃管材市场的影响,找出我国在聚烯烃管材生产方面存在的问题,提出我国在聚烯烃管材新产品开发及生产工艺方面的发展建议。     

Application of solid phase extraction and two-dimensional gas chromatography coupled with time-of-flight mass spectrometry for fast analysis of polycyclic aromatic hydrocarbons in vegetable oils

A fast and simple solid-phase extraction (SPE) method followed by comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC × GC–TOFMS) has been developed for analysis of 15 + 1 carcinogenic polycyclic aromatic hydrocarbons (PAHs) in vegetable oils. Of three critically assessed sample preparation approaches – (i) gel permeation chromatography (GPC), (ii) GPC followed by silica based SPE, and (iii) SPE employing PAHs-dedicated molecularly imprinted polymers (MIPs), the latter one was selected as the best option. Recoveries of the overall analytical procedure ranged from 70 to 99%, with repeatabilities in the range of 2–11%. Limits of quantitation (LOQs) ranging for individual PAHs from 0.1 to 0.3 μg kg⁻¹, were fairly below the maximum level 2 μg kg⁻¹ established for the PAHs representative, benzo[a]pyrene (BaP), by EU Legislation for this commodity. Within the mini-survey in which the new method was employed for examination of 35 samples of various kinds of vegetable oils collected at the Czech market, the highest PAH4 levels, i.e. the sum of BaP, benz[a]anthracene (BaA), benzo[b]fluoranthene (BbFA) and chrysene (CHR) were found in sea buckthorn (708 μg kg⁻¹) followed by rapeseed oil (99.8 μg kg⁻¹). Altogether 8 samples from 35 examined vegetable oils exceeded the maximum limit 2 μg kg⁻¹ for BaP and 10 samples exceeded 10 μg kg⁻¹ set for PAH4 which is fixed by Commission Regulation (EU) no 835/2011 for oils.     

Simultaneous analysis of 10 polycyclic aromatic hydrocarbons in roasted coffee by isotope dilution gas chromatography-mass spectrometry: Optimization,in-house method validation and application to an exploratory study

The presence of polycyclic aromatic hydrocarbons (PAHs) in food implies a potential risk to human health. Although the coffee has been appointed as an important matrix to be monitored for contamination by PAHs, there is still a gap in the literature regarding to the methods of analysis appropriately validated for this scope and also related to the occurrence of contamination in Brazilian commercial samples. In this paper, a method for the determination of ten priority PAHs in roasted coffee by isotope dilution gas chromatography coupled to mass spectrometry was optimized, validated and applied to an exploratory study with 24 commercial samples. The samples were extracted with simultaneous clean-up using pressurized liquid extraction (PLE), followed by liquid–liquid extraction (LLE) and clean-up using silica columns. Linearity was obtained in the concentration range from 0.25 to 4.00 μg kg⁻¹. Matrix effects were not significant. The precision was demonstrated with relative standard deviations varying from 3.3 to 24 % under repeatability and from 3.3 to 33 % under intermediate precision conditions. The average recovery values ranged between 87 and 111%. These values, as well as the limits of detection, limits of quantification and uncertainties of measurements, met the performance criteria established by European Union regulations. The contamination of the commercial samples ranged from 1.00 ± 0.35 to 11.29 ± 2.33 μg kg⁻¹, indicating the need of further occurrence studies and establishment of monitoring programs in Brazil.     

Method for analysis of 68 organic contaminants in food contact paper using gas and liquid chromatography coupled with tandem mass spectrometry

Food contact materials (FCMs) have been reported as a source of various xenobiotics. This study investigates the possibility of simultaneous analysis of 68 potential contaminants in paper FCMs, specifically phthalates, polycyclic aromatic hydrocarbons, photoinitiators, bisphenols, and polyfluorinated compounds. Target compounds were co-isolated using a technique based on ultrasonic extraction by mixture of acetonitrile and water followed by QuEChERS-like liquid–liquid partition in the presence of inorganic salts. Resulting extracts were analyzed using gas and high performance liquid chromatography coupled with tandem mass spectrometry (GC–MS/MS, HPLC–MS/MS). Acceptable recoveries (70–120%) and RSDs (<20%) were achieved for most of the analytes at spiking levels of 0.05, 0.2 and 1 mg/kg. LOQs ranged from 0.0013 to 0.22 mg/kg. The proposed method was successfully applied to analysis of 15 real samples. Complex mixtures of contaminants reaching levels up to 48 mg/kg were identified in the samples.