抗氧剂对植物油氧化稳定性影响的高压差示扫描量热法评价

利用高压差示扫描量热法（ＰＤＳＣ）研究了二烷基二硫代氨基甲酸锌（ＶＡＺ）、２,２′－亚甲基双（４－甲基－６特丁基苯酚）（２２４６）、苯江三唑（ＢＴＺ）和二烷基对苯二胺（ＤＢＡ）４种抗氧添加剂对菜子油氧化稳定性的影响,得到了它们抗氧化作用的大小顺序。别外,根据队仑尼乌斯公式计算了不同油样氧化反应的活化能,证明了ＰＤＳＣ是一种快速简便评价基础油氧化稳定性的方法,适用于抗氧添加剂配方的设计工作。     

反相可切换亲水性溶剂液－液微萃取/电感耦合等离子体质谱法测定变压器油中铜和铁离子含量

以电感耦合等离子体质谱（ICP－MS）为检测手段,研究了反相可切换亲水性溶剂液－液微萃取（SHS－LLME）同时分离富集变压器绝缘油中Cu2+和Fe3+的方法。优化的萃取条件为：以50 μL三乙胺（TEA）萃取25 mL变压器油样,0.60 mol/L硝酸溶液为触发剂,TEA和HNO3摩尔比为1∶1.5,涡旋萃取反应5 min,亲水切换反应5 min,经离心分离后,取水萃取相直接进样测定。变压器油中Cu2+和Fe3+的质量浓度在0.100～10.0 μg/L范围内线性关系良好,线性系数（r2）均为0.999 6,检出限分别为16.8 ng/L和29.0 ng/L,富集倍数分别为23.7和24.1倍。对模拟老化变压器油样中Cu2+和Fe3+的含量进行测定,其加标回收率为93.3%～112%,相对标准偏差（n = 6）为3.6%～5.6%。该文所建立的样品前处理方法与现行标准所用的灰化法无显著性差异,可实现老化变压器油中痕量Cu2+和Fe3+的同时测定。     

基于支持向量机的低分辨核磁共振氢谱法快速预测喷气燃料密度

密度是喷气燃料生产、储运、加注过程中重要的质量指标。为了实现喷气燃料密度的快速、准确测定，提出了一种基于支持向量机（SVM）的低分辨核磁共振氢谱法预测喷气燃料密度。采集喷气燃料样品密度数据和低分辨核磁共振氢谱，利用网格寻优算法和训练集内部五折交叉验证方法优化建模参数。以均方误差和相关系数为指标，通过正交试验对影响模型性能的数据预处理方法进行优化，并对谱图特征的提取方式进行考察。在优化条件下建立的定量分析模型比偏最小二乘法模型预测准确度更高。所建模型对6个油样的预测值与标准值的相对偏差均低于0.3%，模型可应用于喷气燃料密度的快速分析。     

火焰原子吸收光谱法快速测定汽油中的铅

１　引　言四乙基铅是汽油中常用的抗爆剂。由于铅会造成严重的环境污染，近年来，四乙基铅在汽油中的使用日益受到严格限制，所以建立测定汽油中铅的简便的分析方法是非常重要的。现有测定汽油中铅的方法是容量分析法，需要经过萃取、蒸发、氧化、溶解等步骤处理油样，较为繁琐。本文使汽油与表面活性剂聚乙二醇辛基苯基醚（ＯＰ）、正丁醇和水形成微乳液后直接进样进行火焰原子吸收测定，该法具有简单、快速、准确的特点。２　实验部分２．１　主要仪器及试剂　ＷＹＸ－４０１型原子吸收分光光度计（沈阳分析仪器厂），铅空心阴极灯，铅标…     

功能化酸性离子液体催化柴油氧化脱硫的研究

以功能化酸性离子液体为催化剂,30%双氧水为氧化剂,将加氢柴油中的含硫化合物氧化为相应的砜类物质,并用N-甲基吡咯烷酮（NMP）萃取一次。同时考察了反应温度、反应时间和催化剂用量等因素对氧化脱硫反应的影响,得出最佳反应条件为,3mL油样（硫的质量分数为200×10-6）、1.5g酸性离子液体、 0.3mL H2O2、 25℃,3.5h、VNMP/Vdiesel=1∶1,脱硫率可达到86.7%,柴油硫的质量分数仅为25×10-6左右,反应结束后,可通过简单的倾倒将油样和催化剂分离,重复使用5次,其催化活性变化不大。     

电量法测定重整原料油中微量水

本法是以卡尔-费休试剂为电解液,采用恒电流库仑分析法测定重整原料油中的微量水。用2到5毫升油样即可定量的检出1ppm的水含量。当油中水含量大于10ppm时,两次平行试验结果的相对误差不大于±5％,整个分析过程仅需3到10分钟。更换一次电解液能连续分析50毫升油样。与经典的卡尔-费休方法比较。本法具有操作方便、分析快速、灵敏度较高、再现性较好的优点。本方法也可应用于其他液体烃中微量水的分析。     

红外光谱法测定废水中石油类

通过对标准油样扫描的红外光谱特征吸收峰先进行定性分析,然后以特征吸收峰高进行定量分析,建立了用红外光谱法测定废水中石油类的方法,并以不同浓度的标准及考核油样进行了试验性测定,取得了满意的效果。     

异冰片基氧乙醛及其低级同系物的合成

异冰片基氧乙醛及其低级同系物的合成施达常，贾春华（南京林业大学基础课部２１００３７）异冰片基氧乙醛具１ａ式结构，有着强烈而持久的类似熏衣草、迷迭香、天然松木油样新鲜木香香气，可用于调制香精、香水等芳香制品。４－（２－异冰片基氧）丁醛具１ｃ式结构，其香...     

相转移催化水解-超分子溶剂萃取法测定食用油中邻苯二甲酸酯总量

建立了食用油中邻苯二甲酸酯总量的快速测定方法。在四丁基氯化铵的催化作用下,油样中的邻苯二甲酸酯水解为邻苯二甲酸,进一步利用辛醇、四氢呋喃和水形成的超分子溶剂萃取,采用高效液相色谱-串联质谱法(HPLC-MS/ MS)定量分析。本方法的水解时间为10 min,目标物的线性范围为50~2000μg/ L (r>0.999),检出限( LOD)为5.1μg/ kg,定量限( LOQ)为18μg/ kg,3个水平加标回收率为84.6%~104.5%,日内及日间精密度分别为2.6%和3.7%。选择12种实际油样进行测定,邻苯二甲酸酯总含量范围为0.30~1.09 mg/ kg。     

基于木质素-有机黏土复合水凝胶的固相萃取-SERS联用技术用于变压器油中微量1,2,3-苯并三氮唑的现场分析

该文以脱碱木质素（DAL）和硅藻土（DE）为原料,通过加入2.5%丙烯酸（AA）、0.75%过硫酸铵（APS）和0.25%N’N-亚甲基双丙烯酰胺（MBA）,基于自由基聚合法制备了DAL/DE水凝胶。利用高效液相色谱法考察了水凝胶对变压器油中1,2,3-苯并三氮唑（BTA）的吸附性能,随后使用表面增强拉曼散射（SERS）辅以固相萃取技术现场检测了变压器油中的BTA。研究结果表明,在0.6 g DAL/DE水凝胶为固相萃取填料,水为活化剂,BTA变压器油样稀释1倍,洗脱剂为1 mL乙酸的条件下,BTA在776 cm-1处的峰强于1～500mg/kg范围内与其含量呈良好的线性关系,检出限低至0.28 mg/kg。     

Selective detection of volatile nickel,vanadium, and iron porphyrins in crude oils by gas chromatography-atomic emission spectroscopy

This report describes the selective detection of volatile nickel, vanadium, and iron metalloporphyrins in crude oil samples. An atomic emission detector (AED) was used for simultaneous detection of these metals using the Ni 301.2 nm, V 292.4 nm, and Fe 302.1 nm emission lines. Detection limits for these metals range from 0.05 to 5 pg/sec. The presence of volatile forms of these metals in several crude oil samples has been confirmed.     

Improved extraction method for the determination of iron, copper, and nickel in new varieties of sunflower oil by atomic absorption spectroscopy

A simple and fast procedure is proposed for the extraction of iron (Fe), copper (Cu), and nickel (Ni) in 16 varieties of sunflower seed oil samples using an ultrasonic bath. The experimental parameters of the ultrasonic-assisted extraction (UAE) method were optimized to improve the sensitivity and detect the metals at trace levels in minimum time. Conventional wet acid digestion method was used for comparative purposes. The optimum recovery of all 3 metals was obtained by UAE for 7 min, while the separation of aqueous and organic phases after extraction using centrifugation (UAE-2) required 3 min, as compared to the conventional equilibration method (UAE-1) that required 90 min. The respective recoveries of Cu, Fe, and Ni obtained with UAE-2 were in the range of 95.8-97.5, 93.5-98.3, and 95.6-98.2%, respectively, for different varieties of sunflower oil samples. Accuracy was determined by the standard addition method. Under the optimum operating conditions, the limits of detection obtained from the standard addition curves were 21.7, 20.4, and 35.6 ng/mL for Fe, Cu, and Ni, respectively. The fact that all varieties of sunflower oil contain significant amounts of Fe, Cu, and Ni indicates the deterioration of sunflower oil quality immediately after extraction from seeds, which poses a threat to oil quality and human health.     

Metal fractionation in olive oil and urban sewage sludges using the three-stage BCR sequential extraction method and microwave single extractions

The conventional three-stage BCR sequential extraction method was employed for the fractionation of heavy metals in sewage sludge samples from an urban wastewater treatment plant and from an olive oil factory. The results obtained for Cu, Cr, Ni, Pb and Zn in these samples were compared with those attained by a simplified extraction procedure based on microwave single extractions and using the same reagents as employed in each individual BCR fraction. The microwave operating conditions in the single extractions (heating time and power) were optimized for all the metals studied in order to achieve an extraction efficiency similar to that of the conventional BCR procedure. The measurement of metals in the extracts was carried out by flame atomic absorption spectrometry. The results obtained in the first and third fractions by the proposed procedure were, for all metals, in good agreement with those obtained using the BCR sequential method. Although in the reducible fraction the extraction efficiency of the accelerated procedure was inferior to that of the conventional method, the overall metals leached by both microwave single and sequential extractions were basically the same (recoveries between 90.09 and 103.7%), except for Zn in urban sewage sludges where an extraction efficiency of 87% was achieved. Chemometric analysis showed a good correlation between the results given by the two extraction methodologies compared. The application of the proposed approach to a certified reference material (CRM-601) also provided satisfactory results in the first and third fractions, as it was observed for the sludge samples analysed.     

Characterization of North Sea drilling cuttings by metal binding form patterns and diffuse reflectance spectroscopy (DRIFT)

Samples of marine sediments collected in the vicinity of and remote from an oil production platform have been analysed for several metals (Cr, Cu, Fe, Mn, Ni, and Pb) and for total hydrocarbons. The same samples have been examined by diffuse reflectance IR spectroscopy (DRIFT) after drying, and an attempt has been made to classify the samples according to the patterns of the metals and the reflectance spectra, and to correlate this classification with that based on the sampling site. It is suggested that DRIFT is a faster technique than the conventional solvent-extraction IR method for total hydrocarbons and — while less sensitive — is adequate for screening such samples for significant levels of hydrocarbon pollution. Classification of the samples according to the metals present also distinguishes between the two groups of samples.     

Sample preparation methods for subsequent determination of metals and non-metals in crude oil—A review

In this review sample preparation strategies used for crude oil digestion in last ten years are discussed focusing on further metals and non-metals determination. One of the main challenges of proposed methods has been to overcome the difficulty to bring crude oil samples into solution, which should be compatible with analytical techniques used for element determination. On this aspect, this review summarizes the sample preparation methods for metals and non metals determination in crude oil including those based on wet digestion, combustion, emulsification, extraction, sample dilution with organic solvents, among others. Conventional methods related to wet digestion with concentrated acids or combustion are also covered, with special emphasis to closed systems. Trends in sample digestion, such as microwave-assisted digestion using diluted acids combined with high-efficiency decomposition systems are discussed. On the other hand, strategies based on sample dilution in organic solvents and procedures recommended for speciation analysis are reported as well as the use of direct analysis in view of the recent importance for crude oil field. A compilation concerning sample preparation for crude oil provided by official methods as well as certified reference materials available for accuracy evaluation is also presented and discussed.     

Determination of metals in lubricating oils by X-ray fluorescence spectrometry

The determination of common wear metals, namely iron, chromium, copper, zinc and lead, in a wide range of lubricating oil samples was investigated for the use of a low-cost, wavelength-dispersive X-ray fluorescence spectrometer. The procedure provided results in satisfactory agreement with inductively coupled plasma spectrometry used as reference method after microwave digestion of the samples in concentrated nitric acid. Statistical tests following extensive regression analyses of the data indicated that interelement effects were not statistically significant and that a simple linear regression was adequate for the calibration of individual metals.     

Determination of Heavy Metal Content in Vegetables and Oils From Spain and Morocco by Inductively Coupled Plasma Mass Spectrometry

An optimized inductively coupled plasma mass spectrometry method was used to analyze trace metals (As, Cd, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sb, and Sn) in vegetable and oil samples. Prior to analysis, the samples were accurately weighed into a Teflon digestion vessel and the metals extracted from their matrix by using nitric acid and hydrogen peroxide in a closed-vessel digestion system. The proposed method is sensitive, with limits of detection between 5 and 38 ng/kg, and precise, with relative standard deviations from 2.8 to 6.1%. In order to verify its accuracy, the method was used to analyze the Standard Reference Materials NCS ZC85006 Tomato and Certified Used Oil HU-1. The method was successfully applied to the comparative determination of residues of the studied metals in vegetable (tomato, pepper, onion, spinach, lettuce, carrots, and marrow squash) and oil samples (virgin olive, maize, sunflower, and olive pomace) from Spain and Morocco. The results obtained revealed that the contents in metal residues depend on the particular type of food and its origin, probably due to the different production, processing, storage, and preservation methods.     

Neutron activation method in the analysis of geological materials for noble metals

The paper is concerned with various applications of the neutron activation method in the analysis of geological samples for noble metals. A technique is suggested to estimate a priori detection limit values for noble metals in the nondestructive analysis of various samples. Also discussed are new schemes of separation and isolation of elements, the technique of obtaining comparison standards, and constraining factors in application of the method in terms of representation of samples to be analyzed.     

Screening of biosorption bacteria tolerance towards copper and cadmium from oil sludge pond

Certain bacterial strains can be employed in the removal of heavy metals from the environment. The aim of this study was to screen potential bacteria that were tolerant towards Cu and Cd and instrumental neutron activation analysis (INAA) was used to determine the concentrations of heavy metals in the sludge samples. The sludge samples from oil refinery plant in Malaysia contained Cr, Cs, Cu, Eu, Fe, Hg, Mn, Sb, Sc, Th, U and Zn. Seven bacterial isolates were identified to be tolerant to 100 mg/kg of copper and cadmium.     

A precise method for the generation of standard metal salt particulates

A convenient precise method for producing standard dusts has been developed. Metal-containing particulate samples are generated by aspirating solutions containing metals or interest into an atomizer-burner employing an oxygen-acetylene flame. The particulates thus generated are collected by means of a miniature stack by conventional isokinetic sampling techniques. The particulate samples are deposited on filter tapes and are suitable for calibrating trace analytical methods. Particulate samples containing one or more metals, in any desired ratios of their concentrations, can be generated. Initial studies of particulate sizes indicate that the size range generated is in the respirable range, i.e.. 0.1-5 μm.