水源水中环烷羧酸的气相色谱法测定

研究了将水中环烷酸在一定条件下经三甲基氯硅烷衍生后进行气相色谱分析的方法。方法的最低检出浓度为０．０１ｍｇ／Ｌ,精密度较好,ＲＳＤ为６．７％,环己烷羧酸的平均回收率为８０．３％。     

孤岛油田含聚污水中酸性组分的分离与组成结构研究

采用石油醚和三氯甲烷分级萃取孤岛油田含聚污水中的油分,得到两个不同极性的组分F1和F2;用碱抽提法从酸值较高的F2组分中分离酸性物质并将其甲酯化,通过柱层析法将甲酯化物分成Ⅰ、Ⅱ和Ⅲ三个甲酯组分。用元素分析、红外光谱分析等对上述各组分的组成及结构进行鉴定,对甲酯组分Ⅰ进行GC MS 结构鉴定。结果表明,含聚污水中酸性乳化活性物质主要富集在F2组分中,降解HPAM是酸性物质的主要的组成部分;甲酯组分Ⅰ主要为石油酸甲酯,甲酯组分Ⅱ主要为含酰胺基的脂肪酸甲酯,甲酯组分Ⅲ除含有较多酰胺基脂肪酸甲酯外,还含有一定量的强极性含硫化合物;孤岛油田含聚污水中的轻质石油酸以单环环烷酸、四环环烷酸和脂肪酸为主,其中环烷酸的含量明显大于脂肪酸的含量。脂肪酸以C16和C18为主,单环环烷酸以C14~18为主,四环环烷酸以C18~21为主。     

微乳液进样火焰原子吸收法测定异辛酸钴中微量锰

异辛酸钴是一种常用催干剂 ,在油漆、涂料和树脂加工等行业有广泛的应用 ,异辛酸钴中锰含量的高低直接影响到产品的性能和制品质量。根据用途不同对锰含量有严格的要求 ,微量有机锰的常用分析方法是将有机锰分解 ,转化成游离的锰离子 ,用吸光光度法和原子吸收法进行测定 ,操作繁琐。魏琴、杜斌等利用微乳液进样火焰原子吸收光谱法和微乳液吸光光度法分别测定了汽油中环烷酸钴和环烷酸铁的含量 ,省去样品处理工艺 ,操作简单、快速。本文研究了微乳液进样火焰原子吸收光谱法测定异辛酸钴中锰的方法 ,使用十二烷基硫酸钠(SDS)作为乳化剂 ,丁…     

中草药地牯牛幼虫乙醇提取物GC/MS分析

通过对中草药地牯牛幼虫乙醇提取物进行GS／MS分析,发现该虫提取物中主要化学成分是脂肪羧酸和脂肪羧酸酯,其中Z,Z-9,12一十八碳二烯酸和Z-9-十八碳烯酸乙酯分别占出峰面积的22．24％和23．83％,十二烷酸乙酯、十六烷酸乙酯、十四烷酸乙酯和十四烷酸分别占出峰面积的10．00％、16．12％、11．11％和8．13％,共占峰面积的91．47％。     

环烷酸酸盐体系的红外光谱研究──Ⅰ.环烷酸钠和环烷酸钾酸盐体系

本文测量了一系列不同组成的环烷酸－环烷酸钠（钾）酸盐体系的红外光谱，结果表明酸盐体系并不是简单的混合物，而是存在较强的相互作用，包括酸与盐之间的氢键作用和配位作用，体系中存在着组成为ＫＡ·ＨＡ和ＮａＡ·ＨＡ及更多种类的酸盐缔合物．     

一元-二元羧酸镧复合热稳定剂的合成与表征

以常见的一元羧酸和二元羧酸以及硝酸镧为原料,探讨了一元-二元羧酸镧的合成条件,制备了一系列一元-二元羧酸镧复合热稳定剂产品。通过刚果红试纸法和转矩流变仪法对产品的性能进行了表征,并通过红外光谱对产品的结构进行了表征。结果表明:一元-二元羧酸镧的最优合成条件为一元酸:二元酸=1.25:1,反应温度为70℃,保温时间为50min。最优产品对PVC的动态热稳定性可达1420s。     

羧酸对复合羧酸镧热稳定剂性能的影响

以常见的一元羧酸、二元羧酸、三元羧酸和硝酸镧为原料,合成复合羧酸镧热稳定剂,采用刚果红法对产品对PVC的静态热稳定性进行表征,探讨不同羧酸之间的协同效应,进而通过转矩流变仪法对产品对PVC的动态热稳定性进行测试,并通过红外光谱对产品结构进行表征。结果表明:一元羧酸和二元羧酸之间的协同效应最好,且以硬脂酸/己二酸镧性能最佳,对PVC的动态热稳定性可达1420 s。     

丙烯酸酯共聚物中少量羧酸的鉴定

丙烯酸酯聚合物用作表面涂层、粘合剂、油漆时,常含有1～10％不饱和酸或酰胺与其共聚以改进其粘结性能。常用的酸是甲基丙烯酸和丙烯酸。 Anderson用红外光谱的方法,根据精确测定羧基在1700cm~(-1)附近最大吸收可区别丙烯酸酯聚合物中含量高于10％的甲基丙烯酸和丙烯酸等不饱和酸。Pachasky从聚合物中分离出来残留的游离酸,然后用红外光谱和气相色谱可区别不挥发和挥发的不饱和酸。Sharp     

气相色谱/化学电离-质谱法检测石油中的环烷酸

采用柱色谱和阴离子交换树脂法分离出原油200~420 ℃馏分中的羧酸,通过红外光谱仪检验分离效果及分离出的羧酸的类型。采用气相色谱及以异丁烷为反应气的化学电离(CI)质谱法分析分离出的羧酸。在对其结构进行推断和归类中,以纯脂肪酸、环烷酸以及分离出的石油酸的CI质谱数据为基础,结合环烷酸z系列通式CnH2n+zO2,分别得到了不同碳数的脂肪酸及一环、二环……六环环烷酸的分析结果。结果表明,含酸原油中的羧酸主要是环烷酸,相对分子质量分布为170~510,碳数分布为C10~C35,其中双环、三环环烷酸含量较高。     

吡啶基羧酸苄基锡配合物的红外光谱

研究了７ 种吡啶基羧酸苄基锡配合物的红外光谱, 归属了它们的主要红外吸收峰, 探讨了它们随化学结构而变化的规律, 确定了吡啶基羧酸与锡原子的配位形式。     

Characterization of C80 Naphthenic Acid and Its Calcium Naphthenate

A C80 naphthenic acid (tetraacid) and its calcium naphthenate have been characterized with respect to their interfacial properties at both the oil/water and the air/water interfaces as well as their thermal properties. Naphthenic acids in crude oils may give rise to different problems in oil production including naphthenate deposition and formation of stable emulsions. This may lead to severe disturbances of regularity and shut‐in in the oil production. The interfacial activity and film properties of the compounds were examined by the oscillating drop method. The calcium naphthenate film was primarily elastic and solid‐like. Measurements on the acid gave similar results, an elastic, solid‐like film was formed, but the effect was less pronounced than for the calcium naphthenate. Langmuir‐Blodgett films of the acid and its naphthenate were deposited on conducting substrates and subsequently analyzed by scanning electron microscopy, SEM. It was found that the pure acid formed crystalline structures in the interfacial film on compression. The calcium naphthenate, on the other hand, form a continuous amorphous film on the substrate.     

Characterization and screening of metals,metalloids and biomarkers in crude oil by ICP–MS/OES,and GC–MS techniques after digestion by microwave‐induced combustion

A method for digestion of light and medium Iraqi crude oils (Basrah and Khanaken oils) using microwave‐induced combustion (MIC) in closed vessels is described for the determination of Hg, Au, Cu, Al, Ca, Co, K, Mg, Si and Sr by inductively coupled plasma optical emission spectrometry (ICP–OES) and Mo, Ti, Mn, Li, Se^?1, Rb, Ag, Ba, Pb, As, Cd, Cr, Fe, Ni, V and Zn by inductively coupled plasma mass spectrometry (ICP–MS). Upon using MIC it was possible to obtain lower limits of detection by ICP–MS and also by ICP–OES compared with those obtained by microwave‐assisted digestion. The MIC was the best choice with regard to the possibility of using dilute nitric acid as an absorbing solution, which is important to minimize the interference encountered by ICP–MS and ICP–OES.The physicochemical parameters and some contaminants of crude oil samples were analyzed to classify and assess the quality of the crude oils. This study determines the viability of the use of Fourier transform infrared spectroscopy as an alternativee to traditional petroleum geochemical methods for crude oil characterization. The infrared fingerprints agree with the results obtained from GC–MS analysis.     

Interfacial Shear Rheology of Calcium Naphthenate at the Oil/Water Interface and the Influence of pH,Calcium, and in Presence of a Model Monoacid

In this article, the interfacial shear rheological properties of calcium naphthenate with a model tetraacid at the chloroform/xylene-water interface has been investigated as a function of aqueous pH, calcium concentration and monoacid concentration. The experiments are carried out using an interfacial rheology system with an electro commutated motor, direct strain oscillation and a biconical bob geometry. The model tetraacid used, BP10, has previously been shown to have similar bulk and interfacial properties as a narrow group of tetraprotic, so-called Arn acids, and these acids are known to be responsible for formation of hard deposits during oil recovery. A great increase in the elastic modulus was observed around pH 6.2, which is in agreement with observations from oil fields with calcium naphthenate deposition problems. The gel strength and elastic nature is highest around the gelation onset, believed to be due to a bilayer-like conformation of the tetraacid generating a densely packed interface with high cross-linking density and possible film growth. As a function of calcium concentration, both a reduction of the gel strength and slower gel formation was observed when decreasing the calcium concentration from 10 to 4 mM. Myristic acid, a linear C14 fatty acid, was employed as a model for indigenous monoacids and the influence onto the viscoelastic properties of the Ca²⁺-TA film was studied as a function of myristic acid concentration at pH 8.0 and 6.5. A great reduction of both the gel strength and elasticity was obvious in the range of 100 to 1000 higher monoacid than tetraacid concentration. This is however typical indigenous acid concentrations for an acidic crude oil, and may indicate that indigenous monoacids have the ability to act as indigenous inhibitors towards formation of calcium naphthenate. This could explain why some Arn-containing acidic crude oils have deposition problems while others do not. Moreover, all parameters should be taken into account when predicting the deposition risk for a given crude oil, such as concentrations of Ca²⁺, Arn, monoacids and other indigenous acids.     

高效除草剂快杀稗标准物质的制备及表征

从快杀稗工业品出发 ,经活性炭纯化、硅胶柱层析分离制得快杀稗标准物质 ,并进行熔点、高效液相色谱、紫外光谱、元素分析、红外光谱、质谱、核磁共振等方法的表征 ,以高效液相色谱法测得该标准品纯度在99%以上     

Archaeal C80 isoprenoid tetraacids responsible for naphthenate deposition in crude oil processing

The structure of a novel class of octaterpene tetracarboxylic acids which is responsible for naphthenate deposition in crude oil processing has been determined by NMR and mass spectroscopy.     

The chemistry of tetrameric acids in petroleum

This article reviews the properties of a novel class of molecules: the tetrameric acids. These molecules have brought a large interest in petroleum science since the discovery of the family of molecules named ARN in 2004. ARN, which is naturally present in oil, is responsible, by reaction with calcium ion, of the formation of calcium naphthenate deposits; organic deposits that cause irregularities in crude oil production and processing. In order to study the properties of ARN, a model tetrameric acid molecule mimicking some of its properties named BP-10 has been developed in 2008 by Nordgård and Sjöblom and has been extensively used since then.     

Rapid chelometric determination of lead in lubricating oils via mercaptoacetate extraction

A rapid complexometric method for the estimation of lead in lubricating oil has been developed. The lead naphthenate present in the oil is extracted with a mixture of dilute thioglycollic acid and nitric acid. The aqueous extract containing lead mercaptoacetate is titrated with EDTA at pH 5 with Xylenol Orange as indicator. The lead content can be determined within 15-20 min.     

混合溶剂火焰原子吸收法直接测定原油中的镍

混合溶剂火焰原子吸收法直接测定原油中的镍刘广东袁存光张丙华刘文钦（石油大学（华东），山东东营２５７０６２）彭力（中国石油天然气总公司环保处，北京１００７２４）关键词原油，混合溶剂，无机盐标准，原子吸收法，镍测定原油中，微量元素镍、钒、铁、铜的存在对...     

环丙烷甲酸-2-萘甲酯(杀螨剂)的合成

采用一种新的方法合成了环丙烷甲酸-2-萘甲酯。这种杀螨剂的合成过程为, 在碱、季胺型TOMAC相转移催化作用下, 1,2-二溴乙烷与丙二酸二乙酯反应合成1,1-环丙烷二羧酸, 然后脱羧, 得到环丙烷甲酸, 再制成环丙烷甲酸钠, 在Bu~4NBr(TBAB)季胺型相转移催化作用下, 与2-(溴甲基)萘合成得环丙烷甲酸-2-萘甲酯。其总产率为12.9％, 纯度为95.5％。初步证明对螨类害虫─柑桔红蜘蛛有效。     

元素-红外分析法测定海上油田含聚油泥中聚合物的含量

注聚驱油是海上油田高效开发的重要手段. 随着注聚产液量的提升,部分返出聚合物形成的含聚油泥堵塞流程,影响到采出液处理设备运行的问题亟待解决. 通过将含聚油泥中的油、泥、聚合物分离,联合运用元素分析、红外光谱（IR）、气相色谱、X射线衍射（XRD）、分光光度法对其组成进行分析,不同取样点的含聚油泥其主要组成是含油量为22.9%~42.12%,含水量为38.34%~62.3%,含固量为14.8%~19.54%. 其中聚合物含量为3.37%~7.42%,无机矿物含量1.30%~3.74%. 含聚油泥中的原油与SZ36-1标准原油组分一致,注入聚合物AP-P4性质没有发生变化,其结果对指导含聚油泥中原油、聚合物的回收利用研究和油泥分离技术开发有重要意义.