润滑油中痕量铜的石墨炉原子吸收光谱法溯定

润滑油、Tween80、1％硝酸溶液三种组分按1．5：3：21的体积比可形成稳定的微乳液．采用标推加入法，微乳液直接进样，石墨炉原于吸收光措法测定润滑油中铜．进样量为20μL，对最佳原子化条件进行了试验．方法的精密度为5．1％，检出限为0.055mg.L^-1，回收率为96.77％-105.0%。     

航空润滑油热氧化衰变的高压差示扫描量热法分析

模拟实际使用条件，对ВНИИНП－50－1－4Φ航空润滑油进行热氧化试验，应用高压差示扫描量热法（PDSC）和气相色谱仪（GC）评价抗氧剂N－苯基－α萘胺（NPAN）的热氧化衰变程度；结果发现在50－1－4Φ润滑油热氧化衰变过程中，抗氧剂NPAN质量分数（w）的对数值与PDSC在一定条件下测得的氧化诱导期torr具有良好的线性相关性，表明PDSC是研究润滑油热氧化衰变程度的理想手段。     

页岩蠟合成润滑油的抗氧化稳定性及其改进

用苏联热稳定性法(4953-49)与英国石油学会氧化试验法(IP48/52)对由页岩油蜡合成的润滑油的抗氧化稳定性进行了研究。同时,将合成油舆精制的玉门润滑油、苏联航空润滑油20作了比较,并试验了加天然润滑油、与芳烃缩合、加硫磷添加剂等改进抗氧化稳定性的方法。对各种油的氧化产物的官能团均进行了分析。结果表明合成油的抗氧化稳定性低於天然油,其氧化表现类似於烷及烯等链状烃类,氧化後主要生成油溶性的酸、醇、酮醛及酯类等氧化产物。在改进稳定性方法中,以加入添加剂为最有效,与芳烃缩合者次之,加入天然油者最弱。加入玉门油後IP氧化试验所要求的粘度比的降低主要为混合作用。此外,在工作过程中看到:法可以很明显地区分各种改进方法的有效程度,IP氧化试验则不能表示出来,然而法对未加改进的合成油与天然油表示不出很大的差别,IP氧化试验则可对这种情况表示出截然不同的结果。     

聚全氟丙醚油微观结构的研究

聚全氟丙醚油是一种新型的性能独特的润滑油。本实验采用~（１９）Ｆ－ＮＭＲ波谱法，结合~１Ｈ－ＮＭＲ和ＭＳ法，较详细地研究了油品微观结构。由谱线的化学位移和强度归纳出不同链节结构的分布，同时阐明了端基结构。     

有机铜作为润滑油高温抗氧剂的研究

在高档的润滑油中除了加有主抗氧剂ZnDTP外，还需加入其它助抗氧剂以弥补其高温抗氧性的不足。本研究合成了几种有机铜盐高温抗氧剂，用DTA法评价了它们及一些常用抗氧剂对润滑油的热稳定性的影响，发现铜铜盐的高温抗氧性能比一些常用抗氧剂好，可满足高档油的需求。     

润滑油中痕量铜的石墨炉原子吸收光谱法测定

润滑油、Tween80、1%硝酸溶液三种组分按1.5∶3∶21的体积比可形成稳定的微乳液.采用标准加入法,微乳液直接进样,石墨炉原子吸收光谱法测定润滑油中铜.进样量为20μL,对最佳原子化条件进行了试验.方法的精密度为5.1%,检出限为0.055mg.L-1,回收率为96.7%～105.0%.     

加氢催化剂氟化后表面B酸和L酸酸性位的红外光谱分析

润滑油加氢精制催化剂的表面B酸是加氢脱氮的活性位,表面L酸是加氢裂解的活性位.尽管如此,人们利用红外光谱分析在加氢催化剂硫化后的表面上从未检测到B酸中心.事实上,所有固体催化剂参加的有机反应中,人们已经证实表面酸性位起了重要作用.并且在许多催化过程中,固体催化剂的酸性可以通过加氟来改变.现有两种加氟方法:(1)浸渍法或混浆法,即在催化剂制备过程中,选择合适的氟化物,浸渍到载体上,或与载体组成物混合烧结.(2)原位氟化法,即在催化过程中或在催化过程之前,加一种合适的氟化物于气体流或液体流中,使气体流或液体流通过催化剂加氟.我们首次在国内利用原位氟化技术对润滑油加氢催化剂加氟,即在催化过程中,加入了一种氟化物于润滑油中,在润滑油与催化剂发生作用时,给催化剂补氟,以使因氟流失而活性降低的催化剂恢复活性.     

航空润滑油中抗氧剂的热氧化动力学研究

模拟实际使用条件，对ВНИИНП-50-1-4Φ航空润滑油（以下简称50－1－4Φ润滑油）进行热氧化模拟试验，应用GC分析抗氧剂N－苯基－α萘胺（NPAN）的热氧化衰变程度。在50－1－4Φ润滑油热氧化衰变过程中，NPAN的热氧化反应表现为拟一级反应。补油可大大延缓NPAN的热氧化反应速率，不同的补油方式对NPAN的热氧化动力学也有显著影响。研究结果还表明粘度和总酸值不能有效反映润滑油的热氧化衰变程度。     

超声辅助制备表面修饰纳米Ca2B6O11及表征

纳米材料的制备及其应用于润滑油摩擦性能研究,对于改善油品的性能和延长设备的使用寿命具有重要的意义。首次采用超声辅助法合成了球型、粒径分布均匀的纳米硼酸钙润滑油添加剂并对其进行了表征。XRD结合热分析发现样品在室温下为非晶态,750℃结晶,且原料配比对晶态没有影响。SEM和TEM分析证明在超声波辅助下可以得到50 nm的超微粒子,而不用超声波的样品粒径为200~300 nm。在超声和搅拌下将2%的添加剂均匀分散在润滑油中,得到成品油。静置观察评价了润滑油的分散性和稳定性。在重负荷车辆与工业齿轮油中试验检验了润滑油的的润滑性能。结果表明,纳米硼酸钙添加剂具有良好的分散性、稳定性和抗磨减摩性能。     

WS2纳米棒的合成及其摩擦学性能

以十六烷基三甲基溴化铵(CTAB)作为表面活性剂,利用水热合成法在180℃条件下成功制备出WS2纳米棒。用XRD、SEM、TEM和HRTEM对WS2纳米棒的结构进行表征和分析,并提出了可能的生长机理。将WS2作为润滑油添加剂加到基础油中,用CETR UMT-2摩擦磨损仪测试其摩擦学性能。结果表明:WS2纳米棒作为润滑油添加剂表现出良好的摩擦性能。     

Development of an automated method for determining oil in water by direct aqueous supercritical fluid extraction coupled on-line with infrared spectroscopy

A direct aqueous supercritical fluid extraction (SFE) system was developed which can be directly interfaced to an infrared spectrometer for the determination of oil in water. The technique is designed to provide an environmentally clean, automated alternative to established IR methods for oil in water analysis which require the use of restricted organic solvents. The SFE-FTIR method involves minimum sample handling stages, with on-line analysis of a 500 ml water sample being complete within 15 min. Method accuracy for determining water samples spiked with gasoline, white spirit, kerosene, diesel or engine oil was 81-100% with precision (RSD) ranging from 3 to 17%. An independent evaluation determined a 2 ppm limit of quantification for diesel in industrial effluents. The results of a comparative study involving an established IR method and the SFE-FTIR method indicate that oil levels calculated using an accepted equation which includes coefficients derived from reference hydrocarbon standards may result in significant errors. A new approach permitted the derivation of quantification coefficients for the SFE-FTIR analyses which provided improved results. In situations where the identity of the oil to be analysed is known, a rapid off-line SFE-FTIR system calibration procedure was developed and successfully applied to various oils. An optional in-line silica gel clean-up procedure incorporated within the SFE-FTIR system enables the same water sample to be analysed for total oil content including vegetable oils and selectively for petroleum oil content within a total of 20 min. At the end of an analysis the SFE system is cleaned using an in situ 3 min clean cycle.     

Water content of a Brazilian refinery oil sludge and its influence on pyrolysis enthalpy by thermal analysis

Residual oil sludges represent an environmental problem in the oil industry and need a proper destination in order to allow sustainable industrial processes when exploring natural resources. In the present paper, the influence of the water content on the oil sludge pyrolysis process was studied by thermal analysis. A method using thermogravimetry on calcined mass basis was developed to estimate the water content of oil sludges. The water present in the sludge vaporizes during the first thermal processing stage, interfering in the initial process of the organic components pyrolysis and increasing the total oil sludge pyrolysis enthalpy. By quantitative differential thermal analysis (DTA) it can be seen that the water content of the sludge may significantly affect the thermal balance of its industrial pyrolysis process.     

非色散红外法在地表水油类测定中的应用

对非色散红外法应用于地表水油类测定的主要影响因素进行了探讨。指出使用该法在测定样品时如何采取正确处理方法，减少测量误差，并与紫外法测定结果作了比较。同时进行了方法论证。     

Analysis of the Phase Changes During Evaporation of Emulsions with Different Oil Phases

Emulsions surfer alterations in their microstructure after applied on the skin, because of the interaction with skin constituents and mainly by the evaporation of volatile components. These alterations are not even considered by cosmetic formulators, but they are extremely important because they can act on formulation stability, on delivery and on permeation of actives and also on the ability to build the occlusive film, responsible for skin's moisturization. This research studied the phase changing during evaporation of emulsions made with three different oil phase: mineral oil, avocado oil, and isocethyl/stearoil stearate, as a function of the decrease on water ratio, using phase diagrams and evaporation test. It was observed the formation of liquid crystalline phases and their transition along the evaporation path for emulsions with the three different oil phases. It was also observed that these transitions occurred in different water ratios.     

A many-body dissipative particle dynamics study of forced water-oil displacement in capillary

The forced water-oil displacement in capillary is a model that has important applications such as the groundwater remediation and the oil recovery. Whereas it is difficult for experimental studies to observe the displacement process in a capillary at nanoscale, the computational simulation is a unique approach in this regard. In the present work, the many-body dissipative particle dynamics (MDPD) method is employed to simulate the process of water-oil displacement in capillary with external force applied by a piston. As the property of all interfaces involved in this system can be manipulated independently, the dynamic displacement process is studied systematically under various conditions of distinct wettability of water in capillary and miscibility between water and oil as well as of different external forces. By analyzing the dependence of the starting force on the properties of water/capillary and water/oil interfaces, we find that there exist two different modes of the water-oil displacement. In the case of stronger water-oil interaction, the water particles cannot displace those oil particles sticking to the capillary wall, leaving a low oil recovery efficiency. To minimize the residual oil content in capillary, enhancing the wettability of water and reducing the external force will be beneficial. This simulation study provides microscopic insights into the water-oil displacement process in capillary and guiding information for relevant applications.     

Oil powders and gels from particle-stabilized emulsions

We report on the use of silica particle-stabilized oil-in-water emulsions as a template for the preparation of oil powders and gels obtained in a single step by either slow or rapid evaporation of water using freeze-drying or spray-drying, respectively. Using olive oil and partially hydrophobic fumed silica nanoparticles, an oil powder containing nearly 90 wt % oil can be formed by spray-drying, which shows no sign of oil leakage over several months. Upon slow evaporation of water by freeze-drying, a transparent oil gel with oil content as high as 98 wt % can be formed, in which the silica particles form a space-filling network thickening the oil. Comparisons are made throughout with a typical surfactant-stabilized emulsion which does not produce oil powders or gels.     

Simultaneous Determination of Oil and Water in Soybean by LF-NMR Relaxometry and Chemometrics

A fast, non-destructive and eco-friendly method was developed to simultaneously determine the oil and water contents of soybean based on low field nuclear magnetic resonance(LF-NMR) relaxometry combined with chemometrics, such as partial least squares regression(PLSR). The Carr-Purcell-Meiboom-Gill(CPMG) magnetization decay data of ten soybean samples were acquired by LF-NMR and directly applied to the PLSR analysis. Calibration models were established via PLSR with full cross-validation based on the reference values obtained by the Soxhlet extraction method for measuring oil and oven-drying method for measuring water. The results indicate that the calibration models are satisfactory for both oil and water determinations; the root mean squared errors of cross-validation(RMSECV) for oil and water are 0.2285% and 0.0178%, respectively. Furthermore, the oil and water contents in unknown soybean samples were predicted by the PLSR models and the results were compared with the reference values. The relative errors of the predicted oil and water contents were in ranges of 1.25%-4.96% and 0.44%-2.49%, respectively. These results demonstrate that the combination of LF-NMR relaxometry with chemometrics shows great potential for the simultaneous determination of contents of oil and water in soybean with high accuracy.     

Revealing the properties of oils from their dissolved hydrocarbon compounds in water with an integrated sensor array system

This paper presents a system and method developed to identify a source oil's characteristic properties by testing the oil's dissolved components in water. Through close examination of the oil dissolution process in water, we hypothesise that when oil is in contact with water, the resulting oil-water extract, a complex hydrocarbon mixture, carries the signature property information of the parent oil. If the dominating differences in compositions between such extracts of different oils can be identified, this information could guide the selection of various sensors, capable of capturing such chemical variations. When used as an array, such a sensor system can be used to determine parent oil information from the oil-water extract. To test this hypothesis, 22 oils' water extracts were prepared and selected dominant hydrocarbons analyzed with Gas Chromatography-Mass Spectrometry (GC-MS); the subsequent Principal Component Analysis (PCA) indicates that the major difference between the extract solutions is the relative concentration between the volatile mono-aromatics and fluorescent polyaromatics. An integrated sensor array system that is composed of 3 volatile hydrocarbon sensors and 2 polyaromatic hydrocarbon sensors was built accordingly to capture the major and subtle differences of these extracts. It was tested by exposure to a total of 110 water extract solutions diluted from the 22 extracts. The sensor response data collected from the testing were processed with two multivariate analysis tools to reveal information retained in the response patterns of the arrayed sensors: by conducting PCA, we were able to demonstrate the ability to qualitatively identify and distinguish different oil samples from their sensor array response patterns. When a supervised PCA, Linear Discriminate Analysis (LDA), was applied, even quantitative classification can be achieved: the multivariate model generated from the LDA achieved 89.7% of successful classification of the type of the oil samples. By grouping the samples based on the level of viscosity and density we were able to reveal the correlation between the oil extracts' sensor array responses and their original oils' feature properties. The equipment and method developed in this study have promising potential to be readily applied in field studies and marine surveys for oil exploration or oil spill monitoring.     

Bestimmung des hei?wasserl?slichen Borgehalts in B?den mit der induktionsgekoppelten Plasma-Atom-Emissionsspektrometrie

Summary The purpose of this study is to find out whether the previously applied procedures for determining hot water soluble boron trace contents in soils using dianthrimide or azomethin-H can be substituted by ICP-AES. Research was made into chemical and spectral interferences which can arise in all three methods. The 249.678 nm boron emission line is not affected by the sample matrix indicated. The boron content from more than 60 extracts was determined using the three methods mentioned and the results were compared by means of regression calculations. It was found that ICP-AES and the dianthrimide procedure do not differ significantly, whereas the azomethin-H technique leads to somewhat higher values. The accuracy of the results achieved by means of ICP-AES was confirmed by a collaborative study. In order to determine the concentration of boron in soils in the range of 0–2 mg/kg the ICP-AES can be applied following the hot water extraction without further pretreatment of samples. This method is superior in particular when additional elements are to be considered in the soil.     

GC／MS法测定木香挥发油化学成分

用气相色谱-质谱法对木香挥发油进行化学成分的分析。采用水蒸气馏法从木香中提取挥发油。试用不同类型的毛细管柱进行分析,找出最佳分析条件,用归一化法测定其含量,并用气相色谱-质谱法对化学成分进行鉴定。共鉴定了38个成分,占挥发油总成分的86%以上。方法稳定可靠。重现性好,适用于中药挥发油的化学成分分析。