超分散剂在莠去津颗粒表面吸附的XPS和SEM分析

用X射线光电子能谱(X-ray photoelectron spectroscopy,XPS)研究了聚羧酸型梳状共聚物超分散剂吸附于莠去津颗粒样品表面的电子状态,计算了吸附厚度。结果表明,吸附分散剂后,莠去津颗粒界面的N(1s)和Cl(2p)谱峰强度明显减弱,Cl(2s)几乎消失,C(1s),O(1s)和Na(1s)谱峰强度则明显增强,这主要是分散剂中C,O和Na的贡献,且吸附分散剂后能在莠去津颗粒界面形成良好的吸附保护膜,其厚度约为24 nm。用扫描电子显微镜(scanning electron microscope,SEM)研究了样品表面形貌,研究发现吸附分散剂后莠去津颗粒变小、分布有序,使莠去津在水中能够获得稳定的悬浮性能。本文研究结果为莠去津环保剂型悬浮剂的应用提供了重要信息。     

FTIR，XPS和SEM研究聚羧酸盐分散剂在吡唑醚菌酯颗粒表面的吸附性能

采用傅里叶变换红外光谱、X射线光电子能谱和扫描电子显微镜相结合的方式，从微观角度研究梳状聚羧酸盐分散剂在吡唑醚菌酯颗粒表面的吸附性能，为聚羧酸盐分散剂在吡唑醚菌酯悬浮剂中的应用提供理论依据。研究结果表明：吡唑醚菌酯吸附聚羧酸盐分散剂后，红外谱图未出现新的吸收峰，聚羧酸盐分散剂与吡唑醚菌酯之间主要是物理吸附，范德华力是聚羧酸盐分散剂与吡唑醚菌酯颗粒表面结合的主要作用力。吡唑醚菌酯颗粒吸附聚羧酸盐分散剂后，吡唑醚菌酯颗粒界面的N和Cl电子峰强度减弱，C和O电子峰强度明显增强，还出现了Na的电子峰，这主要是聚羧酸盐分散剂中C，O和Na的贡献，说明聚羧酸盐分散剂在吡唑醚菌酯颗粒表面形成了良好的吸附。并以Cl元素为特征元素，计算出聚羧酸盐分散剂在吡唑醚菌酯颗粒表面的吸附层厚度约为1.22 nm。用扫描电子显微镜研究了样品的形貌，吸附聚羧酸盐分散剂后，原本光滑的吡唑醚菌酯颗粒表面吸附了很多细小的颗粒，且有序分布，这是由于分散剂疏水集团对吡唑醚菌酯颗粒形成了包覆，亲水基团充分外露，从而有效阻止吡唑醚菌酯颗粒间的团聚，提高了吡唑醚菌酯悬浮剂的物理稳定性。     

二维傅里叶变换光谱实验方法简介

二维傅里叶变换光谱是近几十年来发展起来的一种先进光谱技术. 与其他超快光谱方法相比，它具有许多优点，并且为研究各种复杂系统提供了巨大的机会. 然而，二维傅里叶变换光谱的系统搭建、实验测量和理论描述仍面临许多挑战，从而限制了其广泛应用. 近年来，随着超快激光等各种相关技术的发展和革新，二维傅里叶变换光谱方法也逐渐发展成熟，进而大大降低了进行二维傅里叶变换光谱实验的技术壁垒. 对于二维傅里叶变换光谱实验装置的光学设计，目前存在许多不同的方法，每种方法都有其自身的优点和局限性. 但是目前还没有一个简单的教程可以帮助实验工作者选择搭建其第一套二维傅里叶变换光谱实验装置. 因此，本文旨在为计划搭建其第一套二维傅里叶变换光谱实验装置的初学者提供一个简短的介绍.     

空间外差光谱技术与FTS的比较研究

空间外差光谱技术是一种新型的可实现超分辨的光谱技术,它综合光栅和FTS技术于一体。对空间外差光谱技术与传统的傅里叶变换光谱技术(FTS)进行比较研究,介绍了两种光谱技术的光学原理,围绕着仪器的光谱分辨率和光谱范围进行比较分析,给出了一组系统设计参数的比较例子。分析结果表明,空间外差光谱技术可以充分利用探测器的空间频率,在一窄带光谱范围内,获得超高的光谱分辨率。     

傅里叶光谱仪高精度光谱定标研究

为了提高傅里叶光谱仪光谱定标精度,减小光谱定标误差,基于风云四号大气垂直探测仪实验室气体池光谱定标数据,进行傅里叶光谱仪高精度光谱定标算法研究。首先,分析了傅里叶光谱仪的分光原理,并在对参考激光波数漂移、光线离轴、以及有限视场引起光谱波数偏移的原理进行分析后,得出傅里叶光谱仪光谱定标公式及定标参数的计算方法;接着分析了快速傅里叶变换(FFT)的栅栏效应和干涉图截断产生的sinc函数造成的光谱定标误差较大的原因;然后通过对比几种不同的光谱细化方法,选择高效的快速Chirp Z-transform(CZT)进行光谱细化,解决FFT光谱分辨率较低导致光谱误差较大的问题;通过对气体池参考气体在HITRAN数据库中的理论谱线,用Gaussian线型展宽并卷积sinc函数处理后作为光谱定标参考谱线的方式,减小由sinc函数引起的谱线间串扰造成的光谱定标误差,从而提高光谱定标精度。最后,使用实验测得的数据对该光谱定标算法进行验证,对比使用CZT细化光谱前后定标误差,和参考谱线处理前后的定标误差,证明该算法可以有效提高光谱定标精度,最高可将光谱定标误差减小10倍以上。     

FTIR光谱结合系统聚类分析鉴别松茸和姬松茸的研究

利用傅里叶变换红外光谱技术研究了松茸和姬松茸子实体,结果显示它们的傅里叶变换红外光谱主要由蛋白质和多糖的吸收带组成。对比它们的光谱发现,两者的特征吸收峰频率位置基本一致,只是在峰形上存在一定差异。利用差谱技术发现它们的红外光谱差异主要来自于1750~1000 cm-1范围内。为了快速准确的区分松茸和姬松茸的光谱,选取1750~1000 cm-1范围内的吸收带进行系统聚类分析。结果显示,系统聚类分析能准确的把松茸和姬松茸的光谱各自聚为一类,达到鉴别它们的目的。研究表明,傅里叶变换红外光谱技术结合系统聚类分析可以发展为一种快速鉴别食用菌的方法。     

健康人体乳腺傅里叶变换红外光谱特征参数分析

通过应用傅里叶变换红外光谱仪(FTIR)的中红外光导纤维并联合衰减全反射探头(ATR)对招募的200名女性健康志愿者的右侧乳腺外上限部位皮肤进行扫描采集相应的傅里叶变换红外光谱,由此共获取200条正常人体乳腺的傅里叶变换红外光谱图。进一步对所得的200条正常人体乳腺傅里叶变换红外光谱图中与脱氧核糖核酸、核糖核酸、蛋白质、脂类、糖类等生物化学成分相关的12条特征谱带进行分析研究,并对这些特征谱带的峰位(P)、峰强(I)、半高宽(F)等36个特征性红外光谱参数进行统计学分析,同时计算相应特征红外光谱参数的90%正常参考值范围、均值、标准差等数值。研究结果首次对正常人体乳腺傅里叶变换红外光谱图相关特征光谱参数的数据建立了正常参考范围,同时为傅里叶变换红外光谱技术进一步实现其在乳腺良恶性疾病诊断方面无创、快速、高效的特有临床应用价值提供相应的理论依据。     

FTIR结合主成分分析对棕榈科植物鉴别研究

采用傅里叶变换红外光谱(FTIR)结合主成分分析(PCA)对棕榈科植物2个亚科4个族的植物叶片进行了光谱研究。结果显示,棕榈科同族不同种和同科不同族的植物在红外光谱上表现出差异。用二阶导数光谱进行主成分分析,显示可以将样品进行正确分类。研究表明傅里叶变换红外光谱在鉴别分类植物方面具有应用潜力。     

模糊K-Harmonic-Kohonen网络的FTIR光谱数据聚类分析

食品的品种不同则其含有营养成分和功效存在差异,得到的傅里叶变换红外光谱也存在差异。为了准确的实现品种分类,设计了一种将傅里叶变换红外光谱与模糊聚类分析方法相结合的品种鉴别方法。在模糊Kohonen聚类网络(FKCN)基础上将模糊K调和聚类(FKHM)引入到Kohonen聚类网络的学习速率和更新策略中,提出了模糊K-Harmonic-Kohonen网络(FKHKCN)算法。FKHKCN利用模糊C均值(FCM)聚类的模糊隶属度计算其学习速率,以FKHM的聚类中心为基础通过推导计算得到FKHKCN的聚类中心,可以解决模糊Kohonen聚类网络方法对于初始类中心敏感而导致聚类结果不稳定的问题。FKHKCN作为一种模糊聚类算法,可实现傅里叶变换红外光谱数据的聚类分析。采用三种数据集：(1)采集产自四川的三种茶叶(优质和劣质的乐山竹叶青以及峨眉山毛峰)作为实验样本,样本总数为96。(2)两个品种(robusta和arabica)的咖啡样本。(3)三个品种(鸡肉、猪肉和火鸡)的肉类样本。首先对三个光谱数据集进行预处理,利用多元散射校正降低茶叶样本原始光谱数据集的散射影响,使用Savitzky-Gol...     

原位漫反射FTIR研究Fe改性的Cu-Mn/ZrO2催化剂上CO的吸附行为

利用原位漫反射傅里叶变换红外光谱(FTIR)技术，研究了Fe改性的Cu—Mn／ZrO2催化剂的CO吸附行为。通过测定单组元及其不同组合催化剂的CO吸附以及催化剂的CO-TPD-IR特征、不同温度CO吸附的红外光谱，研究了Fe助剂对催化剂上CO吸附行为的影响，发现Fe通过提高铜的分散度，改变铜的化学环境，影响催化剂上CO线式吸附的特征，而且形成CO桥式吸附中心，从而提供了低碳醇合成的催化剂表面，并探讨了催化剂上CO吸附形式变化的规律。     

Analysis of Anionic Polymer Dispersant Behavior in Dense Silicon Nitride and Carbide Suspensions Using an AFM

The paper focuses on the interaction mechanism caused by anionic polymer dispersants in dense silicon nitride and silicon carbide suspensions. An atomic force microscope (AFM) was used to determine the relationship between the macroscopic suspension viscosity and the microscopic structure adsorbing of a polymer dispersant at the solid/liquid interface. The surface interactions within the suspensions were analyzed under various dispersant pH values and additive conditions. The addition of an anionic polymer dispersant decreased the viscosity of silicon nitride and silicon carbide suspension and increased the electrosteric repulsive force on the non-oxide surface in solution at pH > 6, which was the isoelectric point of the materials. Based on the above results, we estimated the adsorption mechanism of anionic polymer dispersants on each solid surface in solution under relatively high pH conditions.     

噻菌灵在纳米银胶表面吸附的表面增强拉曼光谱研究

噻菌灵(TBZ)属苯并咪唑类杀菌剂,容易在水果、蔬菜及相应的果蔬饮品中形成有毒残留。基于密度泛函理论(DFT)的量子化学计算方法和表面增强拉曼光谱(SERS)技术,从理论和实验角度系统研究了噻菌灵在纳米银胶粒子表面的吸附行为和增强效应。采用柠檬酸钠还原法制备了具有表面增强拉曼散射活性的银纳米溶胶,并对水相的噻菌灵进行了SERS光谱研究。利用TBZ-Ag₄四种吸附模型对噻菌灵与银纳米溶胶的相互作用进行了理论分析。结合FT-Raman光谱和B3LYP/6-311G(d)理论计算的结果,借助Gaussian View5.0程序的图形化功能,对噻菌灵分子的振动模式、FT-Raman振动光谱和SERS光谱进行了系统的指认。研究结果表明：噻菌灵分子的所有原子在同一平面上,属于Cs对称性;其在银纳米溶胶表面具有十分显著的表面增强拉曼活性;分子中的S原子与银胶粒子发生吸附作用,并通过该分子的长轴方向垂直于银纳米银胶表面;可利用SERS光谱方法对痕量的噻菌灵进行快速检测。为研究噻菌灵的特性以及其快速检测提供了理论和实验依据。     

The role of poly(methacrylic acid) conformation on dispersion behavior of nano TiO2 powder

To exploit the advantages of nanoparticles for various applications, controlling the dispersion and agglomeration is of paramount importance. Agglomeration and dispersion behavior of titanium dioxide (TiO₂) nanoparticles was investigated using electrokinetic and surface chemical properties. Nanoparticles are generally stabilized by the adsorption of a dispersant (polyelectrolyte) layer around the particle surface and in this connection ammonium salt of polymethacrylic acid (Darvan C) was used as dispersant to stabilize the suspension. The dosages of polyelectrolyte were optimized to get best dispersion stability by techniques namely particle charge detector (13.75 mg/g) and adsorption (14.57 mg/g). The surface charge of TiO₂ particles changed significantly in presence of dispersant Darvan C and isoelectric point (iep) shifted significantly towards lower pH from 5.99 to 3.37. The shift in iep has been quantified in terms of free energy of interaction between the surface sites of TiO₂ and the adsorbing dispersant Darvan C. Free energies of adsorption were calculated by electrokinetic data (−9.8 RT unit) and adsorption isotherms (−10.56 RT unit), which corroborated well. The adsorption isotherms are of typical Langmuir type and employed for calculation of free energy. The results indicated that adsorption occurs mainly through electrostatic interactions between the dispersant molecule and the TiO₂ surface apart from hydrophobic interactions.     

Dispersion of nano-silicon carbide (SiC) powder in aqueous suspensions

The dispersion characteristics of nanosize silicon carbide (SiC) suspension were investigated in terms of surface charge, particle size, rheological measurement and adsorption study. Ammonium polycarboxylate has been used as dispersant to stabilize the suspension. It was found that the isoelectric point (iep) of SiC powder was pH_iep (4.9). The surface charge of powder changed significantly in presence of the ammonium polycarboxylate dispersant and iep shifted significantly towards lower acidic pH (3.6). The shift in iep has been quantified in terms of ΔG ⁰ _SP, the specific free energy of adsorption between the surface sites and the adsorbing polyelectrolyte (APC). The values of ΔG ⁰ _SP (−10.85 RT unit) estimated by the electro kinetic data compare well with those obtained from adsorption isotherms (−9.521 RT unit). The experimentally determined optimum concentration of dispersant required for maximizing the dispersion was found to be 2.4 mg/g of SiC (corresponding to an adsorbed amount of 1.10 mg/g), at pH 7.5. This is much below the full monolayer coverage (corresponding to adsorbed amount of 1.75 mg/g) of the particles surface by the dispersant. The surface charge quantity, rheological, pH, electro kinetic and adsorption isotherm results were used to explain and correlate the stability of the nanosize silicon carbide in aqueous media. At pH 7.5, where both SiC surface and APC are negatively charged, the adsorption of APC was low because of limited availability of favourable adsorption sites. In addition, the brush-like configuration of the adsorbed polymer prevented close approach of any additional dispersant; hence stabilization of the slurry happens at a comparatively lower concentration than the monolayer coverage.     

Applications of Raman and Surface-Enhanced Raman Scattering Techniques to Humic Substances

This paper highlights the use of Raman, FT-Raman and surface-enhanced Raman scattering (SERS) techniques for the study of humic substances. In contrast to other technologies which reveal information only about the average compositions and the kinds of functional groups present in humic substances, Raman and especially FT-Raman spectroscopies characterize the building blocks of humic substances and their changes in derivation and separation processes. Furthermore, surface-enhanced Raman scattering (SERS) techniques are able to readily detect humic substances and co-existing organic species at low concentrations typically found in natural environments and reveal definitive information about the specific groups in humic substances that bind on metal electrodes. Further applications of both Raman and SERS techniques can be extended to complicated systems as well as real environmental samples. Experiments have demonstrated: (1). the backbones of humic substances are structurally disordered carbon networks in most cases; (2). The backbones of humic substances from different sources and types are similar to each other; (3). Normal Raman spectroscopic study of humic substances should concentrate on the use of near-IR laser(s) resulting from strong fluorescence background and self-adsorption under the excitation with visible laser irradiation; (4). FT-Raman spectroscopy is the required analytical method to assess the effectivity of fractionation methods; (5). SERS spectra of humic substances on metal colloids and films are in most aces very similar to the corresponding Raman spectra of neutralized samples; (6). SERS techniques are very sensitive and highly selective, also both visible lasers and near-IR lasers can be used for SERS study; (7). SERS spectra on metal electrodes may provide additional information about the binding sites and adsorption mechanisms of humic substances on metal surfaces.     

利用多重光散射技术研究吡虫啉悬浮剂的物理稳定性

Turbiscan Lab稳定性分析仪利用多重光散射技术,能够准确测量乳状液、悬浮液等沉淀层、浮油层或澄清层厚度以及粒子平均粒径随时间的变化情况,定性定量分析体系不稳定性发生的机理和速率。本文利用Turbiscan Lab稳定性分析仪测定了不同萘磺酸盐分散剂GY-D10,NNO,Morwet D-425,TERSPERSE 2425制备的350 g·L-1吡虫啉悬浮剂及其悬浮液背散射光强度随时间的变化情况以及颗粒平均粒径的聚结增大速率,同时利用激光粒度分析仪测定加速试验前后颗粒平均粒径的变化情况,结果表明：添加分散剂GY-D10,用量为4 Wt%时悬浮液的稳定性最好,对应的吡虫啉悬浮剂的稳定性也最好。     

An Electroacoustic Investigation of Concentrated Aqueous Suspensions of Calcium Pyrophosphate

The zeta potential of concentrated suspensions of calcium pyrophosphate were investigated using electroacoustics. The particles were negatively charged over the entire pH range studied. It proved impossible to reduce the pH of the suspension below 1.8, but the iso electric point could be estimated to occur at approximately pH 1. Two commercially available dispersants (one cationic and one anionic) were then added in small increments to the suspension in order to follow the change in zeta potential as the dispersants adsorbed onto the particles. From the shape of the curve it was possible to estimate the optimum adsorbed amount of dispersant required to fully coat the particles. The cationic dispersant adsorbed strongly and the optimum dosage was estimated at 2.5 ml of active polymer/kg of powder. Anionic dispersants are known to adsorb onto negatively charged ceramic oxide particles, but the anionic dispersant used in this study did not adsorb onto the negatively charged calcium pyrophosphate particles.     

SMA-g-MPEG comb-like polymer as a dispersant for Al2O3 suspensions

SMA-g-MPEG comb-like polymer is first employed as the dispersant of Al₂O₃ suspensions in this paper. The comb-like polymer has anionic polycarboxylate backbone, which makes the polymer easily absorbed on the cationic surface of Al₂O₃ particles; on the other hand, the comb-like polymer has hydrophilic MPEG side chains, which extend into the solution to provide steric repulsion after the comb-like polymer is absorbed on the surface of Al₂O₃ particles. The adsorption behavior, zeta potential, apparent viscosity, granularity and TEM images of the Al₂O₃ suspensions using SMA-g-MPEG as dispersant are investigated. The addition of SMA-g-MPEG improves the dispersibility and decreases the apparent viscosity of the Al₂O₃ suspension observably. The impacts of the length of side chains on the dispersion of Al₂O₃ suspensions are particularly discussed. The adsorbed molecular number of the dispersant decreased by increasing the length of side chains. The zeta potential of Al₂O₃ suspension is more negative by using comb-like polymer with shorter side chains. Based on the steric repulsion and adsorbed molecular number, SMA-g-MPEG with moderate length of side chain is found to have the best dispersibility for Al₂O₃ suspension.