Characterization of fuel samples by on-line LC-GC with automatic group-type separation of hydrocarbons

Characterization of fuels by LC-GC is possible by use of automatic successive transfer (multiple transfer) of HPLC fractions to a GC via an on-column interface. This paper describes the instrumentation and the methodology for the HPLC separation of the hydrocarbons (aliphatic and aromatic) into separate groups and the on-line transfer of these groups to a capillary GC column. Two HPLC methods were used with the same valve configuration: single column (silica) with column back-flush to detector; and double column (silica and amino-bonded silica) with multiple fraction transfer and back-flush. The first method was used for the analysis of total saturated compounds and total aromatic compounds; the second was used for the separation of the one-, two-, three-, and four-ring aromatic compounds present in diesel fuels. Examples are shown of the characterization of diesel fuels, and the repeatability of the data.     

Trace elemental determination in alcohol automotive fuel by electrothermal atomic absorption spectrometry

Suitable analytical methodologies were developed allowing direct determination of As, Cu, Fe, Pb, Sb and Sn in alcohol fuel samples by electrothermal atomic absorption spectrometry. Different chemical modification approaches were tested and compared in terms of analytical performance and in practical terms. Experimental conditions were optimized allowing little sample dilution and use of calibration curves prepared with aqueous inorganic analyte standards. Methodologies were tested with analyte spiked alcohol samples. Good analyte recoveries from spiked alcohol samples, precision better than 10% and limits of detection in the sub μg l⁻¹ range were achieved.     

两组份互穿网络聚合物的合成研究

以蓖麻油聚氨酯和聚醚聚氨酯的不同重量比与光敏剂、催化剂、稀释剂、促进剂所组成的多相体系为反应物,分别在紫外光照射和加热的条件下合成网络Ⅰ和网络Ⅱ的互穿网络聚合物(IPN)。改变网络Ⅱ聚醚聚氨酯中各组份的摩尔比制得系列样品。红外光谱,应力-应变曲线和动态力学性能测定发现,样品的力学性能与两组份重量比和网络Ⅱ中不同组成都存在着一定关系。这些结果,为该体系IPN的合成和应用提供了一定依据。     

原油三维荧光分析中猝灭现象辨析

研究了原油的三维荧光猝灭现象，指出浓度过高是原油产生荧光猝灭的主要原因，将会造成三维荧光等值线图畸变，致使定量分析数据失真，谱图特征变异，难以获取原油特征三维指纹图。提出了避免荧光猝灭的预试方法，并列出了不同类型原油的最佳测试浓度。     

无机胶体法制备Pt/C催化剂及其性能表征

采用无机胶体法制备用于质子交换膜燃料电池(PEMFC)的Pt/C催化剂。研究了影响PtO₂胶体生成和稳定性的因素(溶液的pH值、浓度和温度条件等)以及不同还原剂浓度对Pt/C催化剂性能的影响。透射电子显微镜测试结果表明，采用经优化的工艺条件所制备的Pt/C催化剂平均粒径为3 nm，且分散性好、粒度均匀。X-射线衍射分析表明，催化剂中Pt(111)晶面的相对含量较高，有利于加速氧还原反应。单体PEMFC的电压/电流密度曲线测试表明，所制备的Pt/C催化剂具有良好的电化学性能。     

Volatile constituents of flowers and leaves of Anthemis hyalina

The chemical composition of the essential oils of the flowers and leaves of Anthemis hyalina were analyzed by GC and GC-MS for the first time. The oils were found to contain seventy-two components. cis-Chrysanthenyl acetate (14.9% and 17.8%), camphor (11.6% and 1.7%), terpinen-4-ol (8.3% and 1.2%), germacrene-D (5.1% and 2.1%), β-caryophyllene (4.1% and 5.4%), myrcene (3.6% and 16.9%), bicyclogermacrene (3.5% and 0.9%), α-pinene (2.3% and 4.1%), cis-β-ocimene (2.1% and 4.3%) and isospathulenol (0.4% and 4.3%) were found to be the major constituents of the oils of flowers and leaves respectively. Published in Khimiya Prirodnykh Soedinenii, No. 5, pp. 428–429, September–October, 2006.     

Oxidation kinetics of timahdit and tarfaya moroccan oil shales

Organic matter evolution and kinetics of combustion of Tarfaya and Timahdit oil shales have been examined by thermogravimetry (TG) and by differential thermal analysis (DTA). An agreement is observed between both techniques where it was found that combustion of organic matter occurs in two steps. Kissinger's method applied on experimental results gives an activation energy of the same magnitude for the first step of both oil shales (103 kJ mol^–1) whereas the second is 148 kJ mol^–1 for Timahdit and 118 kJ mol^–1 for Tarfaya.The changes in specific surface area during thermal combustion of Timahdit and Tarfaya oil shales have been studied by thermogravimetric gas sorption balance and correlated with experimental results obtained on TG/DTA in air. For Timahdit oil shale oxidation products, specific surface areas calculated from nitrogen adsorption data shows a slight increase during the temperature domain of 280 to 430°C and after this temperature, they increase sharply. However, data obtained with Tarfaya oil shales shows a significant increase at the temperature of maximum oxidation of the first stage of combustion of organic matter.This revised version was published online in November 2005 with corrections to the Cover Date.     

NdOx作为助催化剂对PtRu/C电催化氧化甲醇活性的影响

采用沉积-还原法制备了PtRu-NdOx/C催化剂, 借助TEM、EDS和XRD等测试手段对其进行了微结构和组成的表征. 结果表明, 催化剂中Pt与Ru以合金形式存在, 而Nd的氧化物则以无定形形态存在. 催化剂粒子的平均粒径在2 nm左右, 晶胞参数为0.3896 nm, Nd氧化物的加入对PtRu合金的晶体结构影响不明显. 采用循环伏安法和计时电流法, 比较了PtRu-NdOx/C催化剂和PtRu /C催化剂对甲醇氧化的电催化活性, 结果表明, 加入Nd的氧化物作为助催化剂能明显提高PtRu /C催化剂对甲醇氧化的电催化性能.     

COMPOSITION OF THE ESSENTIAL OIL OF Haplophyllum myrtifolium

The chemical composition of the essential oil ofHaplophyllum myrtifoliumBoiss., endemic to Turkey, was examined by GC/MS. Ninety-seven compounds were characterized with linalool (12.8%), -caryophyllene (10.3 %), and methyleugenol (5.9 %) as the main constituents.     

以催化油浆窄馏分为添加剂的Al－MCM－41分子筛的合成

 采用阳离子表面活性剂十六烷基三甲基溴化铵为模板剂，以正硅酸乙酯为硅源，以硫酸铝为铝源，水热合成了以催化油浆窄馏分为添加剂的高比表面积Al－MCM－41介孔分子筛，并利用XRD，HREM，TG－DTA及N2吸附－脱附等测试手段对合成样品进行了表征．合成的Al－MCM－41分子筛的比表面积和孔体积分别达到1295m2／g和1．5cm3／g，其平均孔径为4．3nm．重点研究了Al－MCM－41分子筛结晶度、晶胞参数、比表面积、孔体积及平均孔径等结构性质随催化油浆窄馏分添加量及其组成的变化规律，并从合成机理上进行了解释．