白油乳状液稳定性实验研究与机理分析

乳状液的微观特征影响着油包水乳状液的稳定性,从而影响油基钻井液的稳定性能。室内选用3^#白油、26%CaCl₂水溶液、JH主辅乳化剂,采用超声分散乳化方法,配制得到油包水型白油乳状液。采用显微图像技术,研究了JH主辅乳化剂加量、油水比、有机土对白油乳状液微观特性的影响;以油水界面张力、动态界面张力以及界面扩张粘弹性等为参数分析了乳状液稳定性的机理。结果表明：JH主辅乳化剂配比为4∶1,加量为4%,油水比为80∶20时,白油乳状液中的分散相呈球形液珠,直径为3.31～12.93μm;油水界面张力为0.559 mN·m^-1;JH主辅乳化剂形成的油水界面膜强度大,白油乳状液稳定性好;有机土与JH主辅乳化剂的协同作用使白油乳状液和油基钻井液的稳定性能显著提高。     

原油乳状液破乳的动态法研究

The stability of different crude oil emulsions from ASP flooding production well is studied by the method of a stirred tank. The demulsifying of crude-oil emulsion by different demulsifying agents is discussed. The breakage of the crude oil emulsions from the well PO11 by the different types and concentrations of the emulsifying agents is also discussed. The breaking mechanism of the demulsifying agent is described microscopically.     

低场核磁共振法测定五种肉类中不同状态水分含量

利用低场核磁共振技术(Low-field Nuclear Magnetic Resonance,LF-NMR)采集牛、猪、羊、鸡和鸭肉五种肉类中水分子的1H信号,通过T-12(弛豫时间倒数)与CuSO4溶液浓度、峰面积与CuSO4溶液质量2条标准曲线,对肉中结合水、不易流动水与自由水的含量进行定量测定,同时与烘箱干燥法测定的体相水(不易流动水和自由水之和)含量进行对比分析。结果显示,LF-NMR法测定的牛肉、猪肉、羊肉、鸡肉和鸭肉中的结合水含量分别为3.49%、3.33%、4.10%、2.17%和3.96%;不易流动水的含量分别为71.0%、72.30%、76.78%、76.61%和77.78%;自由水的含量分别为2.48%、1.90%、2.85%、2.27%和2.14%。烘箱法测定的五种肉类的体相水含量分别为73.04%、73.47%、76.83%、77.11%和77.56%,与LF-NMR法测定的结果差异不显著(p0.05)。LF-NMR可以准确测定上述五种肉类中不同状态水的含量。     

拥挤环境中表面活性剂胶束化过程的低场核磁共振研究

利用长弛豫低场核磁共振(LF-NMR)方法研究了由聚乙二醇(PEG)构建的拥挤溶液环境中表面活性剂的聚集行为。通过Carr-Purcell-Meiboom-Gill(CPMG)脉冲序列所得的回波数据及反演拟合数据对不同的表面活性剂-PEG体系进行分析,结果发现:不同分子量和不同浓度的PEG溶液可用低场核磁共振方法进行区分;高浓度的PEG溶液中均能监测到胶束形成过程,而较低浓度的PEG溶液不利于其胶束化过程监测;NaCl对含有离子型表面活性剂体系的影响较为明显,而对含有非离子型表面活性剂的体系几乎无影响。该研究丰富了低场核磁共振弛豫技术在表面活性剂胶束表征过程中的应用,同时对理解生物体系中分子的自组装及功能也具有重要意义。     

基于核磁共振T2谱测量水包油型原油乳状液含水率的实验探索

采用超声波制备出不同含水率的水包油型原油乳状液样品,采用CPMG自旋回波法测量了核磁共振T_2谱。根据实验结果分析,提出了分别基于水包油型原油乳状液T_2谱中T_2N峰的弛豫时间T_(23),T_2谱各峰面积和加入过量MnCl_2·4H_2O后T_2谱总峰面积测量含水率的3种可能方法。验证实验表明:两种基于T_2谱峰面积的测量方法具有较强的可行性和有效性;基于横向弛豫时间的测量方法因受原油乳状液乳化程度的影响较大,可行性较差。该研究成果为测量水包油型原油乳状液的含水率提供了新的方法。     

低场核磁共振技术分析不同来源水分在烟丝中的分布状态及含水率的研究

采用低场核磁共振分析技术(LF-NMR)对不同来源水处理后的烟丝进行分析,研究了不同处理工艺样品的含水率及水分分布状态的变化。结果表明:水的种类对烘丝关键工序烟丝水分含量及分布状态具有明显影响。其中反渗透水和磁化水处理的样品含水率高于自来水处理后的样品,分别高0.43%和0.72%。得到薄板适宜的加工温度为140~150℃,气流干燥适宜的加工温度为180~210℃。     

基于低场核磁共振弛豫特性结合多元线性回归同步评价菜籽煎炸油品质

油脂作为煎炸食品的重要配料,其品质对产品质量安全和行业发展具有重要意义。以菜籽油为研究对象,系统分析了菜籽油在煎炸过程中品质指标的变化规律及其对低场核磁共振(Low-field nuclear magnetic resonance,LF-NMR)弛豫信号的影响,研究了菜籽油品质指标与弛豫特性之间的相关性,通过LF-NMR弛豫特性结合多元线性回归建立了菜籽煎炸油品质指标同步检测模型,并探究了自变量数对模型性能的影响。结果表明,菜籽油的酸价、极性组分、茴香胺值、羰基价、黏度和吸光度均随煎炸时间延长而增大,而碘值逐渐减小;煎炸过程中菜籽油回波衰减曲线的衰减速率呈上升趋势;弛豫特性指标(T_2w、T₂₁、T₂₂、S₂₂和S₂₃)与菜籽煎炸油的品质指标(酸价、极性组分、茴香胺值、羰基价、黏度、吸光度和碘值)呈显著相关(p<0.05);同步检测模型的决定系数(R²)大于0.93,相对平均偏差(RAD)小于0.15,与单变量检测模型相比,除茴香胺值外,其它指标的RA...     

低场核磁共振结合化学计量学方法快速检测掺假核桃油

以掺假核桃油样品为低场核磁共振检测对象,利用主成分分析法(PCA)和偏最小二乘回归法(PLSR)分析处理Carr-Purcell-Meiboom-Gill(CPMG)序列的核磁共振弛豫数据,旨在探求一种能快速检测核桃油品质的新方法。对几种常见掺假形式(掺入大豆油、玉米油、葵花油)的核桃油样品和纯核桃油样品进行检测和评价。实验结果表明:纯核桃油和掺入不同种类食用油的掺假核桃油在主成分得分图上可以得到很好的区分,且掺假样品随掺假比例在图中呈规律性分布;采用PLSR法对CPMG数据和实际掺假率进行回归,可实现对核桃油掺假水平的准确定量测定。方法快速、无损、准确,在食用油制品的品质控制及评价方面具有很大的应用潜力。     

油脂低场核磁(LF-NMR)检测参数的优化试验

适当的低场核磁共振(LF-NMR)检测条件对于保障数据的可靠性具有重要意义.该文研究了大豆油LF-NMR检测过程中仪器参数、样品温度及体积等对检测结果稳定性及重现性的影响.结果表明,将2.5mL油脂样品置于核磁试管中,并在32℃恒温10 min,采样前稳定1min,在TR =2000 ms,τ=200μs,EchoCount=5000个,NS =4次,TD=500050,SW=250 kHz参数条件下采集信号,可保证检测结果稳定可靠.研究结果可为后期应用LF-NMR技术进行油脂品质检测提供适当的检测条件参考.     

不同品种环保橡胶填充油对乳聚丁苯橡胶性能影响研究

通过使用差示扫描量热仪(DSC)、橡胶加工分析仪(RPA)和动态压缩生热仪测试,分别研究了采用国内外不同品种的环保型橡胶填充油所制备的乳聚丁苯橡胶的热性能、动态力学性能以及动态压缩生热性能,并与非环保型丁苯橡胶SBR1712及环保型丁苯橡胶SBR1723进行了对比。结果表明,采用环保型芳烃油(TDAE)所制备的乳聚丁苯橡胶损耗因子最大,生热稍高于其它品种环保油;采用克拉玛依石化环保型环烷油(AP-10)所制备的乳聚丁苯橡胶动态压缩生热性能最好。     

Experimental Investigation of the Rheological Behavior of an Oil-Based Drilling Fluid with Rheology Modifier and Oil Wetter Additives

Drilling issues such as shale hydration, high-temperature tolerance, torque and drag are often resolved by applying an appropriate drilling fluid formulation. Oil-based drilling fluid (OBDF) formulations are usually composed of emulsifiers, lime, brine, viscosifier, fluid loss controller and weighting agent. These additives sometimes outperform in extended exposure to high pressure high temperature (HPHT) conditions encountered in deep wells, resulting in weighting material segregation, high fluid loss, poor rheology and poor emulsion stability. In this study, two additives, oil wetter and rheology modifier were incorporated into the OBDF and their performance was investigated by conducting rheology, fluid loss, zeta potential and emulsion stability tests before and after hot rolling at 16 h and 32 h. Extending the hot rolling period beyond what is commonly used in this type of experiment is necessary to ensure the fluid’s stability. It was found that HPHT hot rolling affected the properties of drilling fluids by decreasing the rheology parameters and emulsion stability with the increase in the hot rolling time to 32 h. Also, the fluid loss additive’s performance degraded as rolling temperature and time increased. Adding oil wetter and rheology modifier additives resulted in a slight loss of rheological profile after 32 h and maintained flat rheology profile. The emulsion stability was slightly decreased and stayed close to the recommended value (400 V). The fluid loss was controlled by optimizing the concentration of fluid loss additive and oil wetter. The presence of oil wetter improved the carrying capacity of drilling fluids and prevented the barite sag problem. The zeta potential test confirmed that the oil wetter converted the surface of barite from water to oil and improved its dispersion in the oil.     

Study on Nuclear Magnetic Resonance Logging T2 Spectrum Shape Correction of Sandstone Reservoirs in Oil-Based Mud Wells

The oil-based mud filtrate will invade the formation under the overbalanced pressure during drilling operations. As a result, alterations will occur to the nuclear magnetic resonance (NMR) response characteristics of the original formation, causing the relaxation time of the NMR T₂ spectrum of the free fluid part to move towards a slower relaxation time. Consequently, the subsequent interpretation and petrophysical evaluation will be heavily impacted. Therefore, the actual measured T₂ spectrum needs to be corrected for invasion. For this reason, considering the low-porosity and low-permeability of sandstone gas formations in the East China Sea as the research object, a new method to correct the incorrect shape of the NMR logging T₂ spectrum was proposed in three main steps. First, the differences in the morphology of the NMR logging T₂ spectrum between oil-based mud wells and water-based mud wells in adjacent wells were analyzed based on the NMR relaxation mechanism. Second, rocks were divided into four categories according to the pore structure, and the NMR logging T₂ spectrum was extracted using the multidimensional matrix method to establish the T₂ spectrum of water-based mud wells and oil-based mud wells. Finally, the correctness of the method was verified by two T₂ spectrum correction examples of oil-based mud wells in the study area. The results show that the corrected NMR T₂ spectrum eliminates the influence of oil-based mud filtrate and improves the accuracy of NMR logging for calculating permeability.     

Dispersion of T1 and T2 Nuclear Magnetic Resonance Relaxation in Crude Oils

Crude oils, which are complex mixtures of hydrocarbons, can be characterized by nuclear magnetic resonace diffusion and relaxation methods to yield physical properties and chemical compositions. In particular, the field dependence, or dispersion, of T₁ relaxation can be used to investigate the presence and dynamics of asphaltenes, the large molecules primarily responsible for the high viscosity in heavy crudes. However, the T₂ relaxation dispersion of crude oils, which provides additional insight when measured alongside T₁, has yet to be investigated systematically. Here we present the field dependence of T₁‐T₂ correlations of several crude oils with disparate densities. While asphaltene and resin‐containing crude oils exhibit significant T₁ dispersion, minimal T₂ dispersion is seen in all oils. This contrasting behavior between T₁ and T₂ cannot result from random molecular motions, and thus, we attribute our dispersion results to highly correlated molecular dynamics in asphaltene‐containing crude oils.     

3种聚酰亚胺分子的核磁共振碳谱及氢谱的分析

本文报道了３种高性能聚酰亚胺的核磁共振定量碳谱及氢谱。利用这３种样品化学结构的相似性，根据ＰＥＩ和ＤＥＰＴ谱，ＰＥＩ和ＰＯＩ的二维同核化学位移相关谱，碳氢自旋晶格驰豫时间以及化学位移的理论计算，详细分析并归属了３种聚酰亚胺的碳谱峰和氢谱峰，同时验证了其重复单元结构的正确性。     

小檗碱与牛血清白蛋白相互作用的核磁共振研究

采用核磁共振波谱技术(NMR)研究小檗碱与牛血清白蛋白(BSA)的相互结合作用.比较不同浓度小檗碱在一定浓度的BSA溶液中的化学位移、弛豫时间和扩散系数的变化情况.研究表明,小檗碱环上芳香质子与BSA的结合作用较强,其它烷基质子与BSA结合作用较弱;BSA的结合使得小檗碱各个质子的1HT1弛豫时间明显减少,质子在溶液中...     

Stacking interaction study of trans-resveratrol (trans-3,5,4'-trihydroxystilbene) in solution by Nuclear Magnetic Resonance and Fourier Transform Infrared Spectroscopy

Interactions between aromatic rings or other unsaturated systems, including pi-stacking and face-to-edge complexes, are the origin of many phenomena in both organic and biological chemistry. It is well known that these interactions play an important role in the stabilization of the stereo-structure of DNA and the tertiary structure of many proteins.Trans-resveratrol (trans-3,5,4'-trihydroxystilbene, trans-RSV) is a phytoalexin found in Vitis sp. and in many other plants and food products and has received much attention because of its possible positive health benefits. In this work, the pi-stacking interaction of trans-RSV was studied by nuclear magnetic resonance (NMR) and Fourier transform infrared (FTIR) spectroscopy. In particular, the proton chemical shift dependence of the RSV concentration in the range 2 x 10(-2) - 1 x 10(-5) M and temperature were analysed. Moreover, the dynamics of the supramolecular aggregates were studied by nuclear spin relaxation data.     

Cos-7细胞胞内pH的31 P核磁共振测定

生物细胞内pH的测定对于细胞内代谢、游离离子及离子通道的研究有重要的意义,而且一些酶的活性也与细胞内pH密切相关。猴的肾细胞cos-7细胞常用于外源基因的转染表达,研究这一细胞株细胞内的pH,可为基因转染提供可靠的依据。本文采用^31P核磁共振对cos-7细胞胞内的pH进行了分析测定。     

三氟乙酸溶液中尼龙6链凝聚缠结的NMR弛豫研究

采用1D和2DNMR技术,归属了三氟乙酸(TFA)溶液中尼龙6链上的主要¹HNMR共振信号.不同温度下测定的自旋-自旋弛豫时间(t2)提供了大分子主链间凝聚缠结及TFA溶液中尼龙6链随温度变化的动力学信息.结果表明,尼龙6主链上亚甲基基团有不同程度的凝聚缠结,距离CO和NH基团越远,凝聚缠结越明显.与CO和NH基团相连的亚甲基基团的缠结不很明显,主要是因为尼龙6链间氢键的存在.升高温度,热运动加快,这些凝聚缠结逐渐减弱.NH质子的t2H值几乎不随温度变化,TFA质子的t2H值随温度升高而快速下降,表明尼龙6链间氢键随温度升高而破坏,TFA质子又与因温度升高而从尼龙6中释放出来的自由NH和CO基团形成新的氢键.     

钆-二乙三胺五乙酸与牛血清白蛋白作用的核磁共振研究

采用核磁共振弛豫分析法研究了造影剂母体化合物钆-二乙三胺五乙酸（Gd-DTPA）在水溶液和牛血清白蛋白溶液中的诱导弛像增强性质。Gd-DTPA络合物在水溶液中弛豫效率为5．25mmol-1·L·s-1,并发现牛血清白蛋白分子可非共价地结合Gd－DTPA络合物,这种非共价结合体的旋转相关时间明显长于自由络合物,使Gd-DTPA在蛋白质溶液中弛豫效率增高。本文结果表明该方法可以用来研究顺磁性金属络合物与蛋白质之间的相互作用情况。     

Mechanism of Water Dynamics in Hyaluronic Dermal Fillers Revealed by Nuclear Magnetic Resonance Relaxometry

¹H spin−lattice nuclear magnetic resonance relaxation experiments were performed for five kinds of dermal fillers based on hyaluronic acid. The relaxation data were collected over a broad frequency range between 4 kHz and 40 MHz, at body temperature. Thanks to the frequency range encompassing four orders of magnitude, the dynamics of water confined in the polymeric matrix was revealed. It is demonstrated that translation diffusion of the confined water molecules exhibits a two-dimensional character and the diffusion process is slower than diffusion in bulk water by 3–4 orders of magnitude. As far as rotational dynamics of the confined water is concerned, it is shown that in all cases there is a water pool characterized by a rotational correlation time of about 4×10⁻⁹ s. In some of the dermal fillers a fraction of the confined water (about 10 %) forms a pool that exhibits considerably slower (by an order of magnitude) rotational dynamics. In addition, the water binding capacity of the dermal fillers was quantitatively compared.