Molecular characterization of organically-bound sulfur in crude oils. A feasibility study for the application of Raney Ni desulfurization as a new method to characterize crude oils

Five crude oils with varying sulfur contents (0.1 – 4.7%) were characterized on a molecular level for organically-bound sulfur. Aromatic fractions were analyzed by GC-(MS) and asphaltene and polar fractions were analyzed by flash pyrolysis-GC-(MS). The polar fractions were also desulfurized with Raney Ni and the hydrocarbons formed were analyzed by GC-MS. Major sulfur compounds in the aromatic fractions were identified as alkylbenzo- and alkyldiben-zothiophenes. The flash pyrolyzates of the asphaltene contained alkylthiophenes and alkylbenzothiophenes as major compounds, depending on the thermal maturity of the oil. Generally, the sulfur-rich crude oils contained relatively more sulfur compounds. The flash pyrolyzates of polar fractions contained a variety of sulfur compounds (alkylthiolanes, alkylthianes, terpenoid sulfides, alkylbenzothiophenes) with substantial differences between different crude oils. Raney Ni desulfurization of the polar fraction yielded hydrocarbons dominated by n-alkanes, but isoprenoid alkanes, n-alkylcyclohexanes, mid-chain methylalkanes, tricyclic terpanes, hopanes and steranes were also present. These hydrocarbons show a potential to fingerprint crude oils since their distribution patterns are more characteristic than those of the hydrocarbons present in the saturated hydrocarbon fraction.     

珊瑚姜精油的超临界萃取及其抗真菌和细菌活性

珊瑚姜(ZingibercorallinumHance)为姜科姜属植物,产于贵州、广西、广东,贵州主要分布在南、北盘江下游河谷地带,为贵州苗族习用药材,称Jabbangxhnaibdiel(加榜海丢)或阴姜,少数民族常以珊瑚姜块茎入药,具有消肿、解毒、抗菌的功能,用于治疗感冒、咳嗽、腰痛、腹泻[1]。其挥发油的药理研究表明,有抑制离体肠肌引起的痉挛性收缩的自发运动、拮抗组织胺引起的胃肠收缩反应和解除毛果芸香碱、乙酰胆碱、氯化钠等引起的肠痉挛性收缩[2]。挥发油还具有显著的抗真菌作用[3],用于治疗皮癣[4]。超临界CO2萃取是一项新兴的提取分离技术,在中药…     

气相色谱-质谱法测定变压器油正构烃含量

环烷基油是生产高性能变压器油的优质原料,以此为基础油生产的变压器油其凝点一般都小于-40℃,而变压器油在使用过程中对凝点(即低温流动性)有着非常高的要求,凝点的高低直接影响着油品的物理化学性能及电器性能。而油品的低温流动性与其组成中的正构烃(蜡)含量密切相关,据有关     

人参茎叶挥发油中含氧化合物的分离与结构鉴定

组成鉴定;人参茎叶挥发油中含氧化合物的分离与结构鉴定     

Physico-chemical characterization of crystalline phases in fly ashes

Fuel oil combustion in power plants, domestic heating systems and diesel engines, causes the emission in the environment of particles with a typical structure and composition: the cenospheres.These particles are produced during the microdrop fuel oil combustion, when air and fuel are injected into the combustion chamber; they have a spheroidal morphology and a spongy structure.Cenospheres are constituted by an amorphous component rich in C, S, Si, Fe and Al; phases composed by microcrystals of sulphates, oxides and pure metallic elements or their alloys, are frequently present in the cenospheres.These crystalline phases are important from environmental and toxicological points of view both because they are composed of heavy metals, and because they can play an important role in heterogeneous catalysis.We started to study these crystalline phases by analytical electron microscopy techniques and electron energy loss spectrometry to define and characterise their structure and composition.     

用GC/MS分析几种葱属植物挥发油中的有机硫化物

采用蒸汽蒸馏的方法,分别提取了大葱(Allium fistulosum L)、薤白(Allium macrostemonBunge)和大蒜(Allium sativum L)中的挥发油,用GC/MS方法鉴别了它们中的主要硫化合物,并进行了比较。     

Thermogravimetric investigation on combustion characteristics of oil shale and high sulphur coal mixture

Co-combustion experiments of mixture of Huadian oil shale and Heshan coal with high sulphur content have been conducted using a thermogravimetric analyzer. The effects of five different Ca/S mol ratios on the combustion characteristics of mixture fuel are analyzed using TG and DTG curves. The results show that the initial temperature of combustion of mixture fuel is decreased with an increase in the oil shale content of mixture fuel. The combustion characteristic of mixture fuel is superior to that of Heshan coal. Adding about 20 mass% Huadian oil shale into Heshan coal is feasible for desulfurization of mixture fuel during combustion.     

羰基铁催化黄樟油素、丁香酚异构化反应的研究 Ⅳ.应用十二羰基三铁催化合成异黄樟油、异丁香酚

本文使用十二羰基三铁催化黄樟油素,丁香酚异构化反应,它的催化性能比其它羰基铁化合物优良,而且合成方便,不必经过光照反应,因此开辟了异黄樟油,异丁香酚可在加热条件下使用羰基铁催化合成的途径。     

液相色谱–大气压化学电离串联质谱法测定油脂中9种胆固醇氧化物

建立一种准确测定油脂中9种胆固醇氧化物含量的同位素稀释液相色谱-串联质谱测定方法。向油脂样品中加入无水乙醇和60%氢氧化钾溶液,在室温下避光皂化22 h,使用乙醚-石油醚混合液(1∶1)作为提取溶液,采用液-液萃取方式提取目标物,再使用硅胶柱进行净化,采用5 mmol/L乙酸铵溶液与甲醇-乙腈混合液(1∶1)为双流动相梯度淋洗,使用Agilent ZORBAX SB-C18色谱柱分离,在大气压化学电离(APCI)正离子模式下,采用多反应监测模式内标法定量测定。在10~500μg/L范围内,9种胆固醇氧化物的质量浓度与色谱峰面积线性良好,相关系数(r2)均大于0.995,检出限均为0.5 mg/kg,在1,5 mg/kg两个添加水平时,加标回收率为71.2%~94.4%,相对标准偏差小于10%(n=6)。该方法满足动植物油脂中胆固醇氧化物含量测定需要。     

The Effect of Start-Up Conditions on Deactivation of Hydrotreating Catalyst for Heavy Residue with High Asphaltene Content

This article describes a pilot plant test, which was carried out to examine the effect of start-up operation conditions on catalytic performance in the commercial hydrotreating equipment. From the simulated several pilot tests, it was found that the operation conditions of this commercial equipment were very severe and the hydrogen supply to the catalyst active site was critical. When the heavy residue containing large amount of asphaltene was supplied at the start of run (SOR) in the commercial equipment, the permanent adsorption of carbonaceous deposit on the active site should cause leading the catalyst deactivation.