糠醛水溶液的液-液萃取分离

糠醛是重要的化工溶剂和中间体,传统生产过程流程复杂[1],能耗高。近年已提出用不同溶剂萃取分离糠醛和水[2]。本文在前文基础上[3]选择醋酸丁酯为萃取剂测定糖醛-水-醋酸丁酯体系的LLE数据,由二组二元体系和三元体系液液平衡数据确定UNIQUAC模型中三对模型参数,并采用UNIQUAC模型模拟计算糖醛水溶液萃取分离结果,以便为错流和逆流萃取试验提供依据。1　实验部分糠醛水溶液和醋酸丁酯加入液液平衡釜[4],磁力搅拌器搅拌30分钟,待温度稳定后,静置40分钟,取上相和下相分析。平衡釜采用CS501型超级恒温水浴控温,平衡结果由SP-6800…     

氯乙酸甲酯为萃取剂的液\|液半微萃取与胶束电动色谱耦联富集分离中性化合物

报道了采用氯乙酸甲酯作为液-液半微萃取溶剂与胶束电动色谱耦联,通过萃取剂柱上分解来富集分离中性化合物的方法。选取烷基苯酮类（C8, C10 和C11）作为模型化合物,将水中的烷基苯酮类化合物通过液-液半微萃取进入氯乙酸甲酯相中,氯乙酸甲酯相直接进入胶束电动色谱中分离。对于苯乙酮、苯丁酮和苯戊酮的检出限分别为50,50和100 μg/L（S/N≥3）,三者的富集因子达到63～151。本方法只需要有一个毛细管电泳仪而无须特殊设备,省时且操作简便。因此,有很大的潜力用于实际环境样品分析。     

分散液液微萃取技术的研究进展

分散液液微萃取是一种基于传统液液萃取的新型样品前处理技术。该文以分散液液微萃取技术中萃取剂的筛选为出发点,综述了低密度萃取剂、辅助萃取剂、反萃取剂和离子液体等低毒性萃取剂在该技术中的应用,以及应用自制装置、溶剂去乳化、悬浮萃取剂固化,辅助萃取,反萃取和离子液体-分散液液微萃取等萃取模式;并简要评述了该技术与液液萃取、固相萃取、固相微萃取、分散固相萃取、基质固相分散萃取、超临界流体萃取、超声辅助萃取等其他样品前处理技术的联用特性。     

一种固液,液液连续萃取新装置

根据联通管原理,作者设计了一套固液,液液连续萃取装置(图1)。可封闭,可开放;可热萃,亦可冷萃,还可用磁力搅拌器搅拌。装置说明:图1的装置由两个三颈瓶A、B组成。“1”、“2”为温度计,若不需控温可改为磨口塞。“3”为冷凝管。“4”为带三通活塞的联通管。在固液萃取及萃取剂比重大的液液     

基于冷冻熔炼的液-液萃取样品富集技术研究

本文通过对区域熔炼原理及液-液萃取技术的探讨,发展了一种简单高效的基于冷冻熔炼的液-液萃取样品富集新技术.通过理论分析,探讨了冷冻熔炼、常温液-液萃取以及冷冻熔炼液-液萃取中溶质浓度的分布特征,通过富集效率的探讨证明冷冻熔炼液-液萃取技术是液-液萃取与区域熔炼技术的结合.通过葡萄汁样品的分析,对该技术进行了评价.理论计算求得冷冻熔炼液-液萃取中相应组分的富集效率为4.5,而试验测得富集效率为4.8,两者结果一致,说明冷冻熔炼液-液萃取是一种简单高效的样品富集技术.     

微流控液液萃取-液液波导集成化分析系统

利用溴化1-丁基-3-甲基咪唑离子液体/碳酸钠溶液双水相体系,实现了多相层流液液萃取.以具有较高折射率的离子液体为液芯,较低折射率的盐溶液为包层,实现了液液波导吸光度检测.据此建立了一种液液萃取与液液波导检测集成化的微流控分析系统.该系统对甲酚红试样的萃取率在93%以上,对甲酚红试样检测的线性范围为0.01~0.40 mg/m L,相对标准偏差为3.4%(n=11),检出限为3.8μg/m L(3σ).该系统将萃取分离与液液波导长光程吸光度检测集成在一起,为拓展吸光度检测在微流控系统中的应用提供了新思路.     

中空纤维液-液-液微萃取/HPLC分析人尿液中麻黄碱及伪麻黄碱

建立了中空纤维液-液-液微萃取高效液相色谱对人尿液中的麻黄碱和伪麻黄碱进行纯化、分离、富集以及测定的方法。采用中空纤维三相微萃取装置,考察了影响萃取的因素,确定了萃取条件:中空纤维壁上的有机相为正辛醇,以50μL盐酸溶液(pH 2.0)为接受相,在室温下萃取60 min。该条件下麻黄碱和伪麻黄碱的富集倍数分别为180倍和220倍,两者的线性范围分别为0.01～5 mg/L和0.005～0.75 mg/L,相关系数(r)分别为0.998 2、0.997 8,定量下限分别为0.01、0.005 mg/L。该方法使用极少量的有机溶剂,便可有效地对尿样中麻黄碱和伪麻黄碱进行纯化、分离和富集,萃取效率高,可用于尿液中麻黄碱和伪麻黄碱的同时测定。     

离子液体-分散液液微萃取-比色法测定水样中痕量铁

建立了基于分散液液微萃取(DLLME)-数字成像比色(DIC)法测定水样中Fe的方法。在乙酸-乙酸钠缓冲溶液中,Fe(Ⅲ)被盐酸羟胺还原成Fe(Ⅱ)后与邻菲罗啉作用生成橙红色络合物。以离子液体[C6M IM][PF6]为萃取剂,乙腈为分散剂,采用涡旋辅助的分散液液微萃取方法对该络合物进行萃取和富集后,直接通过手机比色装置对Fe进行测定。优化了手机比色装置参数和分散液液微萃取的萃取剂种类及用量、分散剂种类及用量等条件。结果表明,在最佳条件下,方法的线性范围为24～200μg/L,相关系数(r~2)为0.9973,检出限为3μg/L,加标回收率为90.0%～108.0%,相对标准偏差(RSD)为0.8%～1.8%。该方法可用于测定环境水样中痕量Fe。     

分散液液微萃取技术及其在生物样品分析中的研究进展

分散液液微萃取是一种新型微萃取技术,具有易操作、低成本、耗时短、环境友好、萃取效率高等优点。该文着眼于分散液液微萃取技术中萃取剂的性质及辅助分散方式,综述了常规分散液液微萃取、离子液体分散液液微萃取、超声辅助分散液液微萃取等多种萃取模式,并重点归纳总结了近5年分散液液微萃取技术在生物样品分析领域的应用进展。     

分散液液微萃取-反相液液微萃取-扫集-胶束电动色谱法测定红酒中的3种氯酚类物质

建立了分散液液微萃取（DLLME）-反相液液微萃取（RP-LLME）-扫集-胶束电动色谱富集模型,并用于红酒中五氯酚（PCP）、2,4,6-三氯酚（TCP）和2,4-二氯酚（DCP）3种氯酚的测定。实验考察了两步微萃取的萃取参数对氯酚萃取率的影响和样品分离富集的电泳条件。最佳萃取条件DLLME为：3.5 mL红酒（pH 3.0,120 g/L NaCl）,300 μL正己烷（萃取剂）;RP-LLME为：25 μL 0.16 mol/L NaOH（萃取剂）。最佳电泳条件：25 mmol/L NaH₂PO₄,100 mmol/L十二烷基硫酸钠（SDS）,30%（v/v）乙腈,pH 2.3;分离电压-15 kV;样品基质为80 mmol/L NaH₂PO₄;压力进样20 s×20.67 kPa（3 psi）。PCP和TCP的线性范围为0.5~100 μg/L（r≥0.9910）,DCP的线性范围为1.5~80 μg/L（r=0.9851）。3种分析物的检出限（S/N=3）为0.035~0.114 μg/L,加标回收率为75.2%~104.7%,相对标准偏差≤6.17%。该方法富集倍数高、灵敏度高、重现性好、分析速度快,可为不同样品基质中痕量氯酚污染物及某些弱酸性有机污染物测定提供参考。     

Polyarylates. III. Kinetic studies of interfacial polycondensation

The kinetics of interfacial polycondensation of bisphenol A with isophthaloyl chloride and terephthaloyl chloride in dichloromethane with triethylbenzylammonium chloride (TEBAC) as the catalyst was investigated via measurements of bisphenolate concentration by UV. The reaction was found to be second order with respect to bisphenolate. The dependence of the rate constant on stirring speed, amount of TEBAC, and reaction temperature was studied. The rate constant was increased with an increase of stirring speed, quantity of TEBAC added, as well as the reaction temperature. The activation energy was found to be 7.7 kcal/mol at a stirring speed of 700 rpm in the presence of 0.160 of TEBAC. The role of TEBAC was found to be interesting. It did not alter the equilibrium (the partition coefficient remained the same in the presence of TEBAC), but it did enhance the transfer rate of bisphenolate.     

Extraction and recovery of lignosulfonate from its aqueous solution using bulk liquid membrane

The paper presents an experimental study on the coupled transport of lignosulfonate (LS) through bulk liquid membrane (BLM) and thereby to identify the best set of solvent, operating conditions and mode of transport that would yield optimum performance of the BLM. Trioctylamine (TOA) is used as carrier. Among various solvents, tested for the above purpose, dichloroethane is found to be the best. The effects of operating condition, viz. pH, temperature, and carrier concentration, on the equilibrium distribution of LS are investigated. The effects of temperature, stirring of aqueous and organic phases, stirring speed, carrier concentration, initial feed and strip phase concentration on the separation of LS using BLM are also studied. It is observed that transport of LS can be enhanced by increasing the temperature and stirring speed of feed phase. Stirring of strip phase has no appreciable effects on the transport of LS. With increase in initial feed concentration the initial rate of the transport of LS is higher but continues for a longer time. Recovery of LS is much higher in co-transport mode in comparison to counter transport mode. Application of 1.25 M NaOH as stripping solution gives high recovery (70%) and high strip flux (70% of feed flux).     

磷酸可待因在安伯来特IRP-69上的离子交换平衡特性研究

采用批式离子交换法研究了磷酸可待因在安伯来特IRP-69上的离子交换平衡特性、动力学及热力学特征.结果表明,在3个温度(298K、308K和318K)及研究的浓度范围内,离子交换吸附等温方程和Freundlich方程都能够对磷酸可待因在安伯来特IRP-69上的离子交换平衡等温线进行很好的拟合,其离子交换动力学特征基本符合二级动力学方程.磷酸可待因在安伯来特IRP-69上的离子交换行为的热力学参数(ΔH、ΔG、ΔS)都小于0.在3个温度(298K、308K和318K)下,同一初始浓度(350mmol/L)的磷酸可待因在安伯来特IRP-69上的平衡交换吸附量分别为1.1295mmol/g、1.1203 mmol/g和1.1129 mmol/g.     

Optimization of various photocatalytic reaction parameters of Degussa P25 under UV irradiation

Solar photocatalysis is an Advanced Oxidation Process (AOP), used as a sustainable green technology for waste water treatment. Material engineering is one of the most widely reported strategies to develop efficient photocatalysts. However, material engineering is a time consuming and costly process. Recently it has been reported that optimization of photocatalytic reaction parameters can also enhance the photocatalytic performance substantially. In this study, an attempt was made to optimize the adsorption/desorption equilibrium and dispersion of the photocatalyst for improving the photocatalytic performance of the commercial photocatalyst Degussa P25 using Methylene Blue as the probe pollutant. The adsorption/desorption equilibrium studies were carried out under various conditions such as with and without stirring and sonication. Effect of dispersion of photocatalyst on photocatalytic performance was studied under various conditions such as stirring, sonication and with the help of homogenization. The result shows that the adsorption/desorption equilibrium was obtained under low stirring condition, within an optimal time of 20–30 min. In the study of the dispersion of photocatalysts to improve the photocatalytic performance, it is seen that dispersion under sonication showed highest photocatalytic performance under UV light irradiation. Interestingly, the use of homogenizer with higher range of rpm was not able to improve the photocatalytic performance of DP25 than stirring at lower range due to the shadow effect. Based on the above result this study gives an overview of the role of dispersion in improving the overall photocatalytic performance of the photocatalysts.     

Ultrasonication-assisted sorption of cadmium from aqueous phase by wheat bran

In the present study, the sorption of cadmium from aqueous phase by wheat bran was investigated with and without the assistance of ultrasound. Kinetic data and sorption equilibrium isotherms were carried out in batch conditions. The influence of different operating parameters such as ultrasonic power, cadmium initial concentration, sorbent mass, temperature, and the combination of ultrasound and mechanical stirring on the kinetics of cadmium removal was studied. The obtained results show that the ultrasonic irradiation significantly enhances and improves the efficiency of the removal of cadmium, especially in the combined method. The sorption kinetic data were found to be well-represented by the pseudo-second-order rate equation, both in the absence and presence of ultrasound as well as in the combined process (stirring and ultrasonication). Ultrasonic power played a key role in the removal of cadmium. Equilibrium isotherm results could be well described by the Langmuir model both with and without the assistance of ultrasound. The effect of temperature on the sorption isotherms of cadmium in the absence and presence of ultrasound has been also studied and the thermodynamic parameters DeltaG degrees, DeltaH degrees, and DeltaS degrees were determined. The monolayer sorption capacities were 51.81, 35.09, and 22.78 mg g(-1) for experiments conducted by the combined process, in the presence of ultrasound, and in passive conditions, respectively. The combination ultrasound-stirring for the sorption process was shown to be of interest for the treatment of wastewaters contaminated with cadmium.     

影响环氧树脂E-44相反转乳化的因素

研究了乳化剂的HLB值、乳化剂浓度、乳化温度、搅拌强度对环氧树脂E-44相反转乳化中临界含水量Rf值与乳状液稳定性的影响,探讨了环氧树脂E-44相反转机理。实验结果表明环氧树脂E-44从W/O向O/W相反转的发生与乳化剂的HLB值与浓度、乳化温度、搅拌强度等因素都有关,其Rf值随着乳化条件的不同是动态变化的。     

Acridine Derivatives as Inhibitors of Copper Dissolution

Copper dissolution in an acidified chloride solution containing or not containing some acridine derivatives and potassium iodide was studied as influenced by the potential, stirring of the solution, time, and temperature.     

The controlled flocculation of submicron emulsion particles. I. A three-step synthetic route to supermicron polymer particles

The basic features of a three-step experimental process to produce supermicron polymer particles are described. First, a submicron emulsifier-free latex is prepared by a well-known technique. Second, the latex is aggregated by destabilizing with cetyl pyridinium chloride under constant stirring conditions, to yield roughly spherical clusters of 6-12 μ diameter. Third, the aggregates are stabilized with poly(vinyl alcohol) and internally coalesced by heating at or above the glass transition temperature. The final product particles have relatively smooth surfaces. Results are qualitatively interpreted in terms of a dynamic equilibrium where the aggregate size is determined by a balance between attractive interparticle potentials and stirring shear forces. Bimodal aggregate size distributions suggest the aggregate break-up mechanism may involve the erosion of individual latex particles and small fragments from the surface of aggregates. © 1996 John Wiley & Sons, Inc.     

Polymorphism in polymers. I. The equilibrium melting temperature of two crystalline modifications of trans-1,4-polyisoprene

Dilatometric, calorimetric, and dissolution studies have been made of two crystalline modifications of trans-1,4-polyisoprene in order to determine their equilibrium melting temperatures. This parameter is of fundamental importance in the formal treatment of polymorphism in crystalline polymers. A consistent set of thermodynamic parameters has been derived for both crystalline modifications. The equilibrium melting temperature of the polymorph, which was previously observed to melt from carefully crystallized bulk material at 64°C, was calculated to be at least 82.4°C. The other form, which melts from the bulk at 74°C, has an equilibrium melting temperature of 79.5 ± 0.5°C. The trans-1,4-polyisoprene, crystallized by stirring n-butyl acetate solutions at 49°C, was found by x-ray diffraction to be in the first form and melts at 81.2 ± 0.5°C when very slow heating rates are applied. This melting temperature is very close to the independently derived equilibrium melting temperature and lends support to the possibility that extended chain crystals are present in these solution crystallized crystals. Using the newly found melting temperatures of the two crystalline modifications it can be derived from the free energies of fusion that the first crystalline form is more stable at temperatures above approximately 66°C, whereas the other form is more stable below this temperature.     

Kinetics and mechanism of flocculation of bentonite and kaolin suspensions with polyelectrolytes and the strength of floccs

The effects of cationic (Zetag 7589, Zetag 8660, and SNF 528) and anionic (Magnafloc 1011) polyelectrolytes, as well as the regimes and intensity of suspension stirring, on the kinetics of formation, disruption, and subsequent regrowth of aggregates of bentonite and kaolin particles, are studied in a flow system. The optimum polymer doses and the stirring conditions providing the formation of largest and strongest floccules are found. Under comparable conditions, the effect of the adsorption of the above polymers on the electrokinetic potential and the degree of aggregation of particles is studied. It is shown that intense flocculation takes place long before the isoelectric point of particles is reached. This allows one to conclude that the formation of polymer bridges plays a significant role in the flocculation of the examined suspensions with polyelectrolytes. Different dependencies of flocculation on the dose of added polyelectrolytes have been found for diluted and concentrated suspensions. This is explained by different extents to which flocculants adsorbed on the particle surface approach the equilibrium state at different concentrations of dispersed phases.