Compehensive two-dimensional gas chromatography (GC×GC) and its applicability to the characterization of complex (petrochemical) mixtures

In general, petrochemical products contain only a limited number of chemical classes of compounds (sample dimensionality). The enormous number of individual components within these classes, however, soon puts limitations upon a single chromatographic technique when it comes to adequate characterization of these products. Comprehensive two-dimensional gas chromatography (GC×GC) clearly opens the possibility of estimating the composition of hydrocarbon mixtures in a far more detailed fashion than hitherto possible. Although the emphasis of papers of GCxGC thus far almost exclusively applies to the unsurpassed peak-capacity, in the oil industry there is a need for characterization, rather than for analyzing all the individual compounds. In principle a GCxGC system can provide an almost perfect match between its intrinsic properties and the dimensionality of oil samples. To establish the applicability of GCxGC towards petrochemical analytical challenges, a commercially aavailable prototype instrument was subjected to an exhaustive characterization of a typical hydrocarbon precess stream and a fast characterization of a light gas oil. Although there are no fundamental limitations towards the quantitative aspects of a GCxGC system, this paper confines itself to qualitative results only. Quantitative aspects of GCxGC will be published in a forthcoming paper.     

Studies on crude oil‐water biphasic mixtures by low‐field NMR

Low‐field ¹H NMR was used in this work for the analysis of mixtures involving crude oils and water. CPMG experiments were performed to determine the transverse relaxation time (T₂) distribution curves, which were computed by the inverse Laplace transform of the echo decay data. The instrument's ability of quantifying water and petroleum in biphasic mixtures following different methodologies was tested. For mixtures between deionized water and petroleum, one achieved excellent results, with root mean squared error of cross‐validation (RMSECV) of 0.8% for a regression between the water content (wt %) and the relative area of the water peak in the T₂ distribution curve, or a standard deviation of 0.9% for the relationship between the water content and the relative water peak area, corrected by the relative hydrogen index of the crude. In the case of biphasic mixtures of Mn²⁺‐doped water and crude oils, the best result of RMSECV = 1.6% was achieved by using the raw magnetization decay data for a partial least squares regression. Copyright © 2012 John Wiley & Sons, Ltd.     

Interfacial p-n heterojunction of polyaniline-nickel ferrite nanocomposite as room temperature liquefied petroleum gas sensor

In this work, we introduce polyaniline–nickel ferrite (PANI-NF) nanostructured composite to detect liquefied petroleum gas (LPG) at room temperature. The composite synthesized by relatively simple method of in-situ chemical polymerization was structurally characterized by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) techniques. The presence of characteristic absorption bands of both PANI and NF in the FTIR spectrum of the composite with small shifts confirmed interfacial interaction of PANI with NF. The XRD studies also confirmed interfacial interaction between PANI and NF in the composite and its crystalline nature with an average crystallite size of 20 nm. Highly agglomerated granular porous morphology favourable for LPG adsorption was revealed by SEM image of the composite. The TEM image of the composite clearly showed nanosized NF particles embedded in PANI matrix. The LPG sensing performance of the composite at room temperature was tested using a film prepared by depositing the composite on an ordinary glass substrate by cost-effective spin coating technique. The maximum sensing response of the composite was found to be 57% at 700 ppm of LPG, with a response time of 50 s and a recovery time of 200 s. The composite was found to be stable for a period of one month. The sensing mechanism has been discussed on the basis of formation of interfacial p–n heterojunction barrier.     

Analysis of some Elements in Fuel Oil by using Neutron Capture Gamma Ray Spectroscopy

The analysis of some elements in fuel oil was done by using neutron capture gamma ray spectroscopy. The gamma rays emitted after the reaction of (n, γ) from the fuel oil atoms bombarded with the thermal neutrons emitted from a ²⁵²Cf source were investigated in the energy interval 0 … 10 MeV. The impurity elements in the sample were determined.     

杨村烟煤与石油渣油共处理反应特性的研究

用共振搅拌反应器研究了山东兖州杨村的烟煤与北京燕山石化公司的石油渣油共处理液化的反应过程，考察了反应温度和反应时间对煤液化转化率及产物中前涸青烯，苯可溶组分的影响。     

Simultaneous determination of cobalt,copper, iron and vanadium in crude petroleum oils by HPLC

Summary A method has been developed for the simultaneous formation and solvent extraction of cobalt (II), copper (II), iron (II) and vanadium (IV) complexes of bis (acetylpivalylmethane)ethylenediamine (H₂APM₂en) in methyl isobutyl ketone. The complexes are eluted from a reversed phase HPLC column with a mixture of methanol:water:acetonitrile and detection was at 260 nm. The method has been applied to the simultaneous determination of cobalt, copper, iron and vanadium in crude petroleum oils at the ng level.     

正烷酵母作为饲料的最近研究

本文叙述了近十年来我国对正烷烃酵母研究的进展。我们用的菌种是热带假丝酵母Y-17,本所实验厂的生产规模是年产一百吨酵母。发酵罐为6米~3的内或外循环空气提升式,两级连续发酵,50％废水循环利用。生产能力为2克/升·小时。酵母产品的化学分析,包括蛋白质、氨基酸、脂肪、核酸、维生素等,都证明该产品为一优良蛋白饲料。有毒物质含量(如苯骈(a)芘、重金属)符合国际标准。动物试验(包括用大白鼠、鸡、猪的营养试验,慢性毒性试验,传代试验)证明该正烷烃酵母为安全可靠的优良饲料。我们也研究了酵母的核酸和脂肪的综合利用、并筛选了一株高产新菌株球拟嗜烷烃酵母(新种)4B-2,使生产能力提高至2.8克/升·小时。     

Determination of Traces of Vanadium with 5-Bomosalicylhydroxamic Acid by Solid-Phase Spectrophotometry

Abstract

A microdetermination method at μg 1^?1 levels for vanadium by solid-phase spectrophotometry has been developed. 5-Bromosalicylhydroxamic acid was used as chromogenic reagent to form a 1:2 violet complex which is easily sorbed and concentrated on a dextran-type anion-exchange resin. The resin-phase absorbances at 560 and 850 nm were measured directly. Vanadium can be determined in the 5 - 60 μg 1^?1 range with a RSD of 4.3%. The method is applied to the determination of vanadium in pet roleiim crudes and natural water, samples.     

镁铝混合氧化物负载镍催化剂上液化石油气的预重整

采用共沉淀-浸渍法并在较低温度(400～700℃)下焙烧制备了镁铝混合氧化物(MgmAl)负载的Ni催化剂.X射线衍射和程序升温还原结果表明,Ni物种高度分散于催化剂表面,没有形成尖晶石NiAl2O4.在650℃可被还原成金属Ni纳米晶粒,在400℃和较低水/碳摩尔比(S/C=2)条件下表现出较好的催化液化石油气(LP...     

Determination of linear alkylbenzene sulfonates by ion-pair solid-phase extraction and high-performance liquid chromatography

In this paper, the potential use of multiwalled carbon nanotubes (MWCNTs) as solid phase extraction (SPE) adsorbent was evaluated for preconcentration of linear alkylbenzene sulfonates (LAS) using ion-pair (IP)-SPE with tetrabutylammonium hydroxide (TBAH). The LAS homologues present in the aqueous sample were ion-paired with TBAH and the solution was passed through the MWCNT cartridges. The analytes retained in the cartridge were eluted with methanol and the concentrated methanol extract was analysed by HPLC-UV. In order to obtain the satisfactory recovery of LAS homologues, various parameters including the type and amount of the ion-pair reagents, the desorption and enrichment conditions such as the effect of eluent and its volume, pH, the flow rate, the ultrasonic time of sample, and the volume of sample solution were systematically optimized. Under the optimal conditions, LAS homologues could be easily extracted by the proposed SPE cartridge. The favorable limits of detection (LOD) for LAS homologues were in the range from 0.02 to 0.03 μg L⁻¹, and the relative standard deviations (RSDs) were 1.55-2.54% for 10 μg L⁻¹ LAS (n = 6). The proposed method has been successfully applied for the analysis of LAS homologues in aqueous environmental samples. A comparison study with ion-pair solid extraction on MWCNTs, C8 and C18 as adsorbents for LAS demonstrated that ion pair-based solid extraction on MWCNTs adsorbent was advantageous over C8 and C18, the widely used traditional adsorbents.