薄层色谱-氢火焰离子检测分析重质油的族组成

报道了薄层色谱—氢火焰离子检测法在重质油的族组成分析中的应用。方法可有效分离和检测重质油的族组成(饱和烃、芳香烃、胶质等)。该方法具有快速、准确、样品及溶剂用量少等特点。在一定试验条件下，原油的种类和实际点样量不影响氢火焰离子检测的响应值。     

兖州煤与催化裂化油浆共处理及其重质产物组成性质的初步研究

采用石家庄催化裂化油浆和兖州煤共处理，考察了反应条件对兖州煤转化及产物分布的影响，并应用棒状薄层色谱分析了共处理重质产物族组成的变化规律。结果表明，催化裂化油浆与兖州煤共处理，可大大提高兖州煤的转化率，共处理既可得到部分轻质油品，又可得到相当量的重质产物。ＴＬＣ／ＦＩＤ分析表明，催化裂化油浆与兖州煤共处理的重质产物与商用高等级道路沥青族组成近似，重质产物可用于制备高等组道路沥青。     

煤系重质油的仪器分析及系统考察Ⅰ.烃族分析

采用薄层棒色谱／氢火焰离子化检测（TLC／FID）,对煤系重质油的烃族组成分析进行了研究。确定了最佳分析条件、烃族的定量因子等。在此基础上,对山西省焦化厂的典型重质油产品进行了系统测定。     

红外光谱法研究重质油分子的轻度热转化

为了从分子水平快速经济地分析重质油在热转化过程中的变化规律,利用四种模型化合物萘、四氢萘、十氢萘和正庚烷组成的混合体系来模拟重质油及其热转化缩合产物分子的基本组成,研究其红外吸收特性与平均分子参数（亚甲基和甲基的数目之比 N CH2/NCH3、芳氢率faH、芳香环系氢碳原子比NHar/NCar等）的关系。将重质油焦化重蜡油馏分进行轻度热转化,利用不同强度的系列溶剂将热转化产物的重质馏分顺序分离成系列溶剂族组分,将这些族组分进行红外分析。结果表明,混合物系列模拟体系的〖ＷＴＢＸ〗f〖ＷＴＢ１〗aH同其红外吸收在2750cm－1～3100cm－1的3000cm－1～3100cm－1强度分率（S3000~3100/S2750~3100）之间存在良好的线性关系,同时NCH2/NCH3 同2920cm－1和2960cm－1处的吸光度比值A2920/A2960之间也存在良好的线性关系。依据这些关系式可以合理解释重质油分子在热转化过程中分子结构的变化规律。随着重质油热转化的进行,NCH2/NCH3 饱和烃分子先增大后减小,芳香性族组分分子则持续降低;faH或NHar/NCar芳香性族组分分子呈现升高的趋势。     

气-液色谱联合分析煤油共炼产物族组成

建立了一项可以直接分析溶液中焦油和重质油族组成的方法。以高效液相色谱(HPLC)配以气相色谱(GC)完成分析检测。分析了煤油共处理(煤油共炼)中，各种原煤、不同催化剂、不同煤油比及操作条件对产品族组成的影响。     

重质油和焦油的族组成分析

本文采用高效液相色谱、气相色谱、过滤一称重联合分析法对含有溶剂的焦油、重质油的烃族组成进行了分析。给出样品的烷烃、芳烃、非烃和沥青质四大烃族组成，还给出了样品芳烃分布。     

棒状薄层色谱/氢火焰检测法在石油重质油烃组成分析上的应用

在石油重质油的烃组成分析中,液固色谱,质谱和高效液相色谱等已被广泛采用。但是,这些方法均存在着一些缺点,如分析时间长、定量困难等。棒状薄层色谱/氢火焰检测(TLC/FID)法则较好地克服了上述缺点。本文扼要叙述了TLC/FID法的分析原理、试验技术和在石油重质油烃组成分析中的应用实例,并对该技术的发展前景提出了看法。     

应用TLC/FID分析重质油的族组成

〕本工作建立了应用薄层色谱氢焰扫描分析超临界抽提重质油族组成的方法,样品从分离到检定仅需一小时,并且可同时进行十个样品的分析。定量线性关系良好,准确度在薄层色谱允许误差范围之内。     

重质油超临界溶剂萃取梯级分离工艺的化学基础

超临界溶剂萃取分馏方法可实现重质油的深度精细切割分离,从而成为研究重质油化学组成结构的有力工具.本文针对以此方法为基础的重油化学基础研究进展进行专题评述,总结了在重质油超临界萃取分离组分的缔合作用、在液体及超临界戊烷溶剂中微量金属与沥青质的吸附缔合作用、分子组成变化规律、在多孔材料中的扩散规律及其热转化和加氢转化行为等方面的近期研究进展,并介绍了这些研究进展对重油超临界溶剂萃取梯级分离工艺开发的指导作用.     

渣油及超临界戊烷精密分离馏分碳化的研究

采用超临界流体精密分离（ＳＣＦＥ）的方法将辽河减压渣油切割成多个窄馏分,在４３０℃、常压条件下对各馏分进行不同时间（２～１７ｈ）的热处理,测定了反应残余物的Ｈ／Ｃ元素比并在正交偏光下对反应残余物的光学显微结构进行观察。对渣油及其超临界戊烷精密分离馏分的热反应性能及反应残余物性质与原料性质的关系进行了讨论。研究结果表明：渣油组成的变化对其在碳化过程中的中间相形成、发展有十分重要的影响,采用ＳＣＦＥ可以将渣油切割为具有不同族组成的窄馏分,窄馏分的碳化试验表明,对组成适宜的窄馏分,在反应中可以形成各向异性发达的中间相,ＳＣＦＥ是一种改善重质烃类混合物碳化性能的有效技术。     

Multiresidue analysis of fungicides in soil by sonication-assisted extraction in small columns and gas chromatography

A rapid multiresidue method for the simultaneous determination of 14 fungicides in soil was developed. Fungicides were exacted from soil, placed in small columns, by sonication-assisted extraction with ethyl acetate. The effect of residue residence time and soil moisture content on the fungicide recovery was studied. Residue levels in soil were determined by gas chromatography with electron-capture and nitrogen-phosphorus detection. Residue identities were confirmed by gas chromatography coupled with mass spectrometry, in the selected ion monitoring mode. Recovery studies were carried out at 0.5, 0.1 and 0.05 microg/g fortification levels for each fungicide, and average recoveries obtained for these compounds ranged from 80 to 104% with relative standard deviations between 1 and 8%. The method is linear over the range assayed, 0.5-0.05 microg/g, and the detection limit for the fungicides studied varied from 2 to 10 microg/kg.     

Automated multiresidue analysis of pesticides in olive oil by on-line reversed-phase liquid chromatography-gas chromatography using the through oven transfer adsorption-desorption interface

A multiresidue, automated and rapid method for the determination of pesticide residues in olive oil is presented. The method employs the through oven transfer adsorption-desorption interface for the on-line coupling of reversed-phase liquid chromatography and gas chromatography. In this fully automated system, olive oil is directly injected with no sample pre-treatment step other than filtration. Methanol-water is used as eluent in the liquid chromatography pre-separation step. The selected liquid chromatography fraction containing the pesticides is automatically transferred to the gas chromatography. The liquid chromatography column flow during elution is different from the flow during the transfer. Using a flame ionisation detector, pesticide detection limits varied from 0.1 to 0.3 mg/l.     

碳五馏分组分的HP-1毛细管色谱法测定

提出用ＨＰ－１毛细管色谱柱分析测定碳五馏分中组分含量的分析方法,研究了其测定条件,并对分离后的组分用质谱方法进行定性,按确定的分析条件,碳五馏分中各组分得到较好的分离,精密度好,分析结果准确可靠。     

毛细管柱气相色谱法测定液化石油气中二甲醚含量

建立毛细管柱气相色谱法测定液化石油气中二甲醚含量的分析方法。采用静止进样法直接进样,用PLOT–Q毛细管色谱柱进行分离,以FID检测器进行检测,外标法进行定量分析。液化石油气中二甲醚的含量(体积分数)在0%~20.0%范围内与其色谱峰面积呈良好线性关系,线性相关系数r=0.999 9,方法检出限为0.05%(体积分数),测定结果的相对标准偏差小于5%(n=6),回收率在98.2%~102.9%之间。该方法与校正面积归一法测定结果相一致。该方法准确、快速、简便,适用于液化石油气中二甲醚含量的检测。     

PHOTOCYCLOADDITION REACTION OF 5,7-DIMETHOXYCOUMARIN TO THYMIDINE

Abstract— The photocycloaddition reaction of 5,7-dimethoxycoumarin to thymidine on direct irradiation (λ > 300 nm) is studied as a model for photosensitization reaction of furocoumarins. The major photoadducts were isolated by silica gel column and gel permeation chromatography. Each component of the photoadducts was further separated by reverse phase, paired-ion high performance liquid chromatography. The structure of these photoproducts isolated is consistent with 1:1 C₄-cycloadducts in accordance with characteristics of their UV, IR, NMR and mass spectra and elemental analysis data. The stereochemistry of each isomer was studied by Fourier transform NMR, UV and IR spectra. The fraction C has the anti head-to-tail configuration and the fraction D has the configuration of anti head-to-head. The fractions A and B probably have the syn configuration.     

Liquid chromatography/tandem mass spectrometry of unusual phenols from Yucca schidigera bark: comparison with other analytical techniques

Qualitative and quantitative analyses of phenolic compounds are of interest for both medicinal and food plants. In the present work, the phenolic fraction from Yucca schidigera, a plant bearing the GRAS (Generally Recognized as Safe) label approved by the US Food and Drug Administration, was studied. Crude extracts of Y. schidigera bark were investigated by liquid chromatography/UV spectrophotometry with diode-array detection, liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) and liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS), in order to develop and optimize simple and rapid techniques to determine both stilbenes and yuccaols for the purposes of quality control of collected material. With optimal LC and MS conditions, stilbenes and yuccaols were quantified with all the proposed methods and the results were compared. Sensitivity was evaluated and the results indicated that MS/MS detection in the multiple reaction monitoring mode is easily applicable to this plant and allows the rapid and direct identification and quantification of these peculiar compounds in crude plant extracts.     

生物样品中多氯联苯的微波皂化萃取气相色谱法测定

以KOH－甲醇－正己烷为皂化萃取溶剂,利用微波皂化萃取－气相色谱法测定了生物样品中的多氯联苯（PCBs）,实现了在皂化的同时对待测物的萃取。方法的检出限为质量分数6.25×10     

气相色谱法测定三聚氰氯的研究

气相色谱法测定三聚氰氯的研究李秀梅赵树岚＊田锦霞＊孙维星（东北师范大学化学系长春１３００２４）关键词气相色谱法三聚氰氯三聚氰氯（ＣＮＣｌ）３是活性染料的重要中间体及合成树脂、橡胶、塑料等的防老剂，也常用于除草剂、增白剂、药物、炸药等的生产中。传统的分...     

气相色谱法测定榄香烯水针剂中有效成分含量

建立了测定榄香烯水针剂的有效成分含量的气相色谱方法,解决了多次进样造成对色谱柱和检测器的污染以及色谱柱效下降的问题,方法操作,灵敏度高,重现性好,相关系数为0．9999,相对标准偏差为0．41％。     

Thin-layer chromatography of the MBTH derivatives of some aliphatic aldehydes

A rapid, simple method for resolution and detection of mixtures of aliphatic aldehyde by thin-layer chromatography of their MBTH derivatives is proposed. Less than 1 mg l . levels of each aldehyde in the original aqueous solution can be detected.