Amphoteric polystyrene latex colloids: polymerization pathway and the control of particle size and potential

Amphoteric polystyrene latex colloids were prepared by the emulsifier-free emulsion polymerization of styrene. Two co-monomers, methacrylic acid (MA) (anionic) and dimethyl aminoethyl methacrylate (DMAM) (cationic) were used to promote the amphoteric nature of the resultant surfaces. Parameters such as particle size and the isoelectric point (IEP) were measured as a function of polymerization recipe. Particle size decreased with increasing initiator concentration according to the equation: log [d _w]=–0.67 log [I] + 0.316 whered _w is the weight average particle diameter andI is the concentration of initiator (potassium persulphate).The particle size also decreased with increasing temperature, increasing pH and addition of surfactant. Particle size was unaffected by the methacrylic acid content. The isoelectric point pH was decreased on decreasing initiator concentration and on increasing methacrylic acid content.The polymerization pathway was deduced to involve the cationic DMAM during the initiation phase and to involve the anionic MA as well as styrene, during the growth stage. A full polymerization pathway involving the formation of oligomeric DMAM micelles was postulated.     

Application of HPLC to measure vanadium in environmental,biological and clinical matrices

Vanadate and vanadium compounds exist in many environmental, biological and clinical matrices, and despite the need only limited progress has been made on the analysis of vanadium compounds. The vanadium coordination chemistry of different oxidation states is known, and the result of the characterization and speciation analysis depends on the subsequent chemistry and the methods of analysis. Many studies have used a range of methods for the characterization and determination of metal ions in a variety of materials. One successful technique is high performance liquid chromatography (HPLC) that has been used mainly for measuring total vanadium level and metal speciation. Some cases have been reported where complexes of different oxidation states of vanadium have been separated by HPLC. Specifically reversed phase (RP) HPLC has frequently been used for the measurement of vanadium. Other HPLC methods such as normal phase, anion-exchange, cation-exchange, size exclusion and other RP-HPLC modes such as, ion-pair and micellar have been used to separate selected vanadium compounds. We will present a review that summarizes and critically analyzes the reported methods for analysis of vanadium salts and vanadium compounds in different sample matrices. We will compare various HPLC methods and modes including sample preparation, chelating reagents, mobile phase and detection methods. The comparison will allow us to identify the best analytical HPLC method and mode for measuring vanadium levels and what information such methods provide with regard to speciation and quantitation of the vanadium compounds.     

Selective water sorbents for multiple applications, 3. CaCl2 solution confined in micro- and mesoporous silica gels: Pore size effect on the “solidification-melting” diagram

In this communication we present a low-temperature “solidification-melting” phase diagram for CaCl₂/H₂O solutions confined in KSK and KSM silica gels. At salt concentrations of 0–48 wt. %, the diagram has been found to lie below the diagram reported for the bulk system by 15–30°C. It shows a depression of the solution melting point due to its confinment to the pores. Several other peculiarities of melting and solidification in this system are also reported and discussed. Beside fundamental interest, the data obtained could be of importance in many commercial areas such as refrigeration, accumulation of low temperature heat, frost prevention in building materials,etc.     

On the solution characterization of an all-aromatic liquid-crystalline copolyester

Solution characterization of the thermotropic liquid–crystalline copolyester synthesized from terephthalic acid, phenyl hydroquinone, and (1-phenylethyl) hydroquinone (2 : 1 : 1) has been performed. Viscometry, size exclusion chromatography, and light scattering have been carried out under the optimal conditions found for measurement: 85°C in a 50/50 mixture by weight of phenol/1,2,4-trichlorobenzene. The absolute weight-average molecular weight from light-scattering measurements served for calibration of indirect methods of charac-terization (e.g., the limiting viscosity number [η] is related to the molecular weight by [η] = 5.10 × 10^?4 M_w^0.72), and the molecular weight per unit chain length, $ \bar M_L * $, from light scattering and size exclusion chromatography (SEC) is found to be 28 Å^?1, consistent with theoretical expectations. The calculated persistence length q is 28 Å. Moreover, the meth-odology of SEC characterization enables the kinetics of solid-state postpolymerization of this liquid-crystalline copolyester to be studied. © 1993 John Wiley & Sons, Inc.     

Growth kinetic study of ionic liquid mediated synthesis of gold nanoparticles using Elaeis guineensis (oil palm) kernels extract under microwave irradiation

Gold nanoparticles (AuNPs) are the most studied nanomaterials due to their promising applications. However, surface capping of AuNPs is essential to protect aggregation for enhanced colloidal stability. In this study, a single step method was established to synthesize stable AuNPs using oil palm kernel (OPK) extract prepared in IL[EMIM][OAc] (1-ethyl-3-methylimidazolium acetate). Ionic liquids were used for phytochemicals extraction along with capping and stabilizing of AuNPs after their synthesis. The OPK extract reduced the gold precursor, and UV–vis spectroscopy revealed a sharp surface plasmon (SPR) peaks in the region of 524–529 nm, which confirmed the formation of AuNPs. UV–vis and TEM analysis indicated that microwave assisted synthesis was rapid to synthesize well dispersed and small sized AuNPs in comparison with conventional heating. FTIR analysis of kernels extract before and after its reaction with gold precursor identified the involvement of CH aromatic groups, polyphenolic OH groups, and carbonyl amide groups that are responsible for reduction of trivalent gold ions to AuNPs. EDAX and XPS analysis were performed to identify the elemental gold and its surface interaction with ILs and other organic moieties. Colloidal AuNPs kept at room temperature for periods of six months were remained stable. The change of pristine nanostructure arises due to involvement of different driving forces during growth of nanoparticles. Thermodynamically instability of nanomaterials may leads to Ostwald Repining (OR) or adopt complex pattern of growth and undergo coalesce and orientation attachment (OA). These models were fitted to compare the theoretically growth of particles along with actual increase of particles size. Experimental results suggested that OA growth was originated in early phase, however, it substituted and mainly controlled by OR growth pattern over time.     

Curing of a maleimide model compound

A monofunctional maleimide-ended model compound was synthesized and purified. The thermal curing of this compound was followed by size exclusion chromatography and the molecular masses of the oligomers formed during the curing reaction were determined by mass spectroscopy. It was found that high molecular mass species were not thermally stable. At high temperature and after enough time, a strong decrease in the polydispersity of the oligomers and a significantly preferential formation of trimer were observed. From ¹³C-NMR characterization, a five membered ring structure was found for the trimer, which explains the thermal stability of this species. © 1995 John Wiley & Sons, Inc.     

灰化消解-极谱法测定油料中五个重金属元素

建立了灰化消解-极谱法测定油样中镉、铅、铜、镍、钴等5种微量重金属元素的含量.油料样品通过灰化法消解后,用极谱法在乙酸-乙酸盐缓冲溶液和磺基水杨酸-磷酸-氨水体系中测定5种重金属元素的含量.5种微量重金属元素的检出限为1.3×10-4～9.8×10-4 g·L-1,加标回收率为90%～106%,相对标准偏差为0.22%～3.16%.     

自组装单层保护金纳米团簇的量子化电容充电

本文研究自组装单层保护金纳米团簇(C12Au MPC)在常温下二氯甲烷溶液中的量子化电容充电效应.示差脉冲伏安曲线显示金核平均直径为2.0 nm的C12Au MPC在-0.6~0.6 V电位区间内有9个明显的量子化电容充电峰,其双电层电容总的变化趋势为在零电荷电位附近最小,随着电位正移或负移电容变大.而且随着该金核尺寸的增大,MPC双电层电容值也变大.     

信息时代的铌酸锂晶体:进展与展望

铌酸锂晶体具有非线性效应、电光效应、声光效应、光折变效应、压电效应与热释电效应等多种物理特性,在表面声波器件、光电器件、声光器件等方面获得广泛的应用.经历了六十多年的发展,铌酸锂晶体历久弥新,随着材料特性的不断开发,新功能、新器件、新应用层出不穷,尤其是铌酸锂单晶薄膜在薄膜滤波器、集成光电器件等领域的性能具有明显优势,...