Chromatographic Zinc Isotope Separation by Chelating Exchange Resin

Zinc isotope separations were studied by displacement chromatography using the chelating properties of malate, citrate and lactate exchange resin and EDTA as ligands. After each chromatographic operation, the heavier zinc isotopes were found to preferentially fractionated into the carboxylate complex solution phase. The separation coefficients (ε) for zinc isotope separation had the largest value and were obtained for the isotopic pairs ⁶⁸Zn/⁶⁴Zn (7.16 × 10^?4) and ⁶⁶Zn/⁶⁴Zn (3.08 × 10^?4), respectively, at 298 ± 1 K. The separation coefficient per unit mass differences (ε/ΔM) for the isotopic pair of ⁶⁸Zn/⁶⁴Zn was found to range around 1.55 × 10^?4.     

Rapid Separation of Plutonium in Environmental Samples Using an Anion Exchange Resin Disk

A rapid analytical method of Pu in environmental samples by alpha-ray spectrometry and high-resolution inductively coupled plasma mass spectrometer (HR-ICP-MS) using a 3M Empore anion exchange resin disk for solid phase extraction has been developed. A trace amount of Pu was quantitatively adsorbed with an Empore anion exchange resin disk (47 mm diam.) at a flow rate of 150–200 ml/min from 8M HNO₃ sample solution. The disk was washed with 10 ml of 8M HNO₃ and 12 ml of 9M HCl and then the Pu was quantitatively eluted with 15 ml of 1M HNO₃/0.03M ascorbic acid solution. The time needed to separate Pu from the sample solution with the present method was about 20 minutes. The separated Pu was determined with alpha-ray spectrometry and HR-ICP-MS. The present method was applied to the determination of Pu in the certified reference material (IAEA-135) and the environmental soil sample. The analytical results were almost in good agreement with the literature values.     

Hydrogen Isotope Exchange Reactions in an Electrical Discharge

Hydrogen isotope exchange reactions occurring in (H₂O, D₂)or (D₂O, H₂) reacting system under a DC electricaldischarge were investigated using spectroscopic methods such asFourier-transform infrared (FTIR) and plasma emission spectroscopy(PES). The progress of the reactions was determined by real-time measurementof the IR absorbance of HDO molecule, a major product of the reaction. Theprogress of the reaction was studied as a function of the temperature, thecurrent density, and the composition of the reactants, while the pressure ofthe system was maintained at approximately 67 mbar. The results revealedthat the discharge method was far more effective in facilating the exchangereaction than was the conventional catalytic method. The (H₂O, D₂)system also generated a significant amount of D₂O besides HDO andHD as the ratio of D₂ to H₂O was increased. Thetransient species of the system, such as H or D atoms, were monitored duringthe discharge using emission spectroscopy. The analysis of the final products by mass spectroscopy confirmed that neither H₂ nor O₂was among the major products of the system in the discharge.     

阳离子交换树脂对钙拮抗剂的吸附及控释特性

离子交换树脂是一类功能高分子材料．长期以来应用于分析化学、蛋白质化学、纯水制备等领域．近年来 ,离子交换树脂也逐渐应用于ＤＲＳ的研究和开发 ,即口服药物树脂复合物缓释给药系统 (ＯｒａｌＤｒｕｇ ＲｅｓｉｎＣｏｎｔｒｏｌｌｅｄＲｅｌｅａｓｅＳｙｓｔｅｍ,ＯＤＲＣＲＳ)．与其他的给药系统相比,ＯＲＣＲＳ的最主要的优点是能制成稳定性良好的液体控释制剂,供儿童及有吞咽困难的老年人服用［１ ３］．中枢镇咳药美沙芬药物树脂复合物液体控释制剂（Ｄｅｌｓｙｍ）的上市被认为是药物控释技术的一大突破［４］．盐酸维拉帕米 (…     

Microwave Assisted Benign Method of Chelating Resin Synthesis Having Different Thermal and Ion Exchange Properties

Summary: Microwave irradiation method was used for synthesis of chelating ion exchange resin derived fom Salicylicacid-Formaldehyde-Resorcinol (SFR-M). The resin was characterized by Elemental analysis, FTIR, TGA and SEM. The Broido and Horowitz-Metzger method were used to calculate the energy of activation (Ea) from TGA. The microwave assisted chelating resin has different thermal behaviour as compared to conventional resin (SFR-C). The sorption capacities of microwave SFR resin for transition metal ions are higher than conventional SFR resin. The separation of binary mixtures [Cu (II) and Zn (II)] in brass and [Ni (II) and Cd (II)] were successfully carried out using Kd value.     

碱熔-阳离子交换树脂分离-离子色谱法/电感耦合等离子体质谱法测定地球化学调查样品中卤素

地质样品中的卤素具有中度不相容性、较强的挥发性和流体迁移能力,作为示踪元素对反演流体和挥发分相关的地球化学过程具有重要意义。由于地球化学调查样品中的卤素含量低以及具有较强挥发性,测定难度较大。F、Cl、Br、I主要采用单独或分组熔矿的方法进行制备和测定,操作难度大、消耗时间长、分析效率低。本文采用Na2O2和NaOH混合试剂碱熔后分取溶液,加入阳离子交换树脂,静态交换2～3小时,除去溶液中大量的阳离子,减少基体干扰,利用离子色谱测定F、Cl,利用电感耦合等离子质谱法测定Br、I。结果表明：该方法测定F、Cl、Br、I 的检出限分别为6.9、10.2、0.87、0.27μg/g,相对标准偏差（RSD%,n=12）在2.8～8.5之间,均小于10%。该方法具有结果准确、简单、快速、经济的特点,在地球化学调查样品分析中具有良好的应用前景。     

Bromate Exchange Resin as an Oxidizing Agent in Organic Synthesis

Bromate exchange resin has been prepared by a simple elution technique and used for the oxidation of aromatic aldehydes to the carboxylic acids. Oxidation is carried out under biphasic condition. Work up is simple. Resin immobilized bromate ions have been used for the first time as an oxidizing agent in organic synthesis.     

Kinetics of Exchange of Chloride Ions in an Anion-Exchange Resin

The kinetics of the exchange of chloride ions in an anion-exchange resin has been studied. The rate measurements were carried out by a potentiometric technique, and thus both the kinetic and the activation parameters of the reaction were determined. The results concerning the influence of the stirring velocity upon the fractional attainment of equilibrium prove that the diffusion of the C1[sbnd] species into the resin beads plays an important role in the mechanism of the exchange reaction, although the exchange rate is chemical in its ultimate mechanism.     

电感耦合等离子体原子发射光谱法测定铜合金中磷

在pH 3～4的微酸性介质中,铜合金试样溶液通过装有强酸性聚苯乙烯型阳离子交换树脂的离子交换柱,分离除去其基体金属阳离子.交换柱流出液(包括洗液)经酸化,蒸发浓缩并定容为25 mL后,用电感耦合等离子体原子发射光谱法测定此溶液中磷(以PO3-4形态存在)的含量.方法的检出限(3σ)为0.026 mg·L-1,用标准加入法测得方法的平均回收率为101.9%.     

Hydrodynamic Effect on Secondary Phase Separation in an Epoxy Resin Modified with Polyethersulfone

Summary: The evolution of the morphologies in blends of epoxy/4,4′‐methylenebis(2,6‐dimethylaniline)/polyethersulfone was followed by time‐resolved light scattering, optical microscopy and scanning electron microscopy. The results suggest that, once the diffusion of epoxy molecules cannot follow the geometrical growth, a secondary phase separation occurs, even in the droplet morphology, in which the size of the epoxy‐rich domain grows as usual. The viscoelastic effect of polyethersulfone is also discussed.

Development of morphologies followed by OM: bicontinuous phase separation in the PES‐15.9 blend cured at 140 °C after 80 s.     

树脂快速静态分离-石墨炉原子吸收光谱法测定砷的形态化合物

用离子交换树脂静态吸附和溶剂萃取相结合的分离技术,结合塞曼GFAAS测定方法,分析了砷的四种形态化合物:As(Ⅲ)、As(Ⅴ)、MMA和DMA。文中的静态吸附分离是指采用少量树脂,对小体积溶液室温下用电磁搅拌数分钟,经短时间的相对静态的吸附或解吸过程,达到分离的目的。分离和测定全过程约为30～40min。方法对As(Ⅲ)、As(Ⅴ)、MMA和DMA和总As的检出限分别是0.94、0.89、0.94、0.26(富集4倍)和0.90μg/L。可应用于河水、植物中砷形态分析。     

聚苯乙烯型离子交换树脂的研究进展

介绍了聚苯乙烯型离子交换树脂的合成方法;综述了近年来在氯甲基化反应、Mannich反应以及磺化反应上的新进展、新理论：从结构上对聚苯乙烯型离子交换树脂的强度和热稳定性进行了分析。聚苯乙烯型离子交换树脂具有稳定的物理化学性质、吸附选择独特、再生容易、操作简便、使用周期长等优良性能,大大促进了化工企业、制药工业、环保、医疗、分析等行业的发展,具有广阔的发展前景。     

Hydrogen Isotope Exchange Reactions in an Atmospheric Pressure Discharge Utilizing Water as Carrier Gas

Allowing water/hydrogen or water/hydrogen/He gas mixture to flow through micro- hollow type of electrodes and applying 60 Hz AC power between the electrodes made it possible to sustain large area and atmospheric pressure discharge. The electrode assembly was constructed by sandwiching a dielectric spacer with two thin metal sheets and boring an array of micro holes through them. Another variation of the assembly was prepared by stacking thin metallic sheets so that the stack functions as an electrode through which the gas mixture flows for generating dielectric barrier discharge. A large volume of the gas mixture, while producing plasma, underwent instantaneous hydrogen isotope exchange reactions between H₂O and D₂O or between D₂O and H₂ gas molecules. The efficiency of the atmospheric pressure discharge was assessed by measuring the extent of the exchange reactions at a given flow rate of the gas mixture.     

阳离子树脂交换分离-电感耦合等离子体质谱(ICP-MS)法测定地质石膏样品中硼

硼石膏近些年在水泥、沥青混合材料等领域应用广泛,其主要成分为CaSO4·2H2O和B2O3以及其他杂质,因此准确、快速测定石膏样品中的硼元素对石膏的应用、资源综合利用等方面具有重要意义。而国家标准GB/T 5484-2012《石膏分析方法》中并没有硼元素的化学分析方法,且相关文献报道也很少。目前测定硼元素主要采用电感耦合等离子体质谱法（ICP-MS）,样品前处理多采用酸溶法,而碱熔法应用不多,主要原因是碱熔后溶液中产生大量盐分影响等离子体焰的稳定性,而732型阳离子交换树脂能吸附大量的钠离子,同时吸附了钙、镍、铁及稀土等阳离子,减少盐分干扰。基于此原理,本文采用氢氧化钠碱熔-732型阳离子交换树脂交换分离,在线加入铑内标的方式,建立了ICP-MS法测定石膏中硼的方法,同时由于石膏国家标准物质不包含硼元素的含量,采用高纯硫酸钙分别与岩石标准物质、水系沉积物国家标准物质和土壤国家标准物质混合配置成人工标准物质,并讨论了熔矿体系、阳离子加入量与吸附时间、清洗液、同位素的选择等实验条件。本方法的检出限为0.76μg/g,精密度（RSD,n=7）为0.9%~1.7%,相对误差为1.56%~3.96%,加标回收率在97.5%~102%,该方法快速、准确,记忆效应小,适合石膏中硼元素的测定。     

Photochemical Transformations with Iodine Azide after Release from an Ion‐Exchange Resin

This report discloses the photochemical homolytic cleavage of iodine azide after its formation following release from polymer‐bound bisazido iodate(I) anions. A series of radical reactions are reported including the 1,2‐functionlization of alkenes and the unprecedented chemoselective oxidation of secondary alcohols in the presence of primary alcohols.     

毛细管离子交换电色谱的分离行为

在离子交换毛细管色谱柱上实施电色谱，并对其分离行为进行了研究，采用７５μｍ（ｉ．ｄ．）２０ｃｍ的毛细管强阳离子交换柱（３μｍ）以ＮａＨ２ＰＯ４－Ｈ３ＰＯ４缓冲液为淋洗剂，紫外柱上检测（２１４ｎｍ）考察了流动相的ｐＨ值，有机改性剂及分离电压等因素对分离的影响，研究表明，不同的ｐＨ溶质的流出次序发生改变，随着有机改性剂含量增加，溶质的保留时间减小，而电渗流却增大，同时，对分离的柱效和方法的重现性进行了     

Study on Adsorption and Separation of Naringin with Macroporous Resin

X-5 resin, with higher adsorption and easier desorption of naringin, was selected from five kinds of macroporous resins through static adsorption and desorption experiments. Effects of concentration, pH value, and flow rate of naringin extract on the adsorption of naringin by X-5 resin were studied. Meanwhile, the effect of these factors on the desorption of naringin from X-5 resin was also investigated. The experimental results show that the adsorption isotherm of naringin by X-5 resin can be described by the Langmuir isotherm equation. The static maximum adsorption capacity of naringin is 32.6 mg/g with naringin concentration at 2.7 g/L, while the dynamic adsorption capacity of naringin is 23.8 mg/g with naringin extract flow rate at two times that of resin volume per hour. The optimal eluant is 60% (v/v) ethanol-water with pH value of 10. The desorption ratio will rise to more than 85% when the flow rate of this optimal eluant is one to two times that of resin volume per hour. Translated from Journal of Central South University (Science and Technology)     

阳离子交换树脂分离-电感耦合等离子体发射光谱(ICP-OES)法测定盐湖卤水中偏硅酸含量

由于盐湖卤水中盐分浓度不同且盐度较高,采用常规分析方法很难准确测定。本方法采用将盐湖卤水稀释5倍,加入6g阳离子交换树脂,静态交换1.5h,除去卤水中的大量阳离子后,选择Si 251.611nm为分析谱线,以Y371.030nm谱线作为内标进行信号漂移校正,用电感耦合等离子体发射光谱仪测定卤水中偏硅酸的含量。在最佳实验条件下进行测试,该校准曲线的线性范围为0.50～200.00mg/L,所得回归方程的线性关系良好(γ≥0.9994)。本方法检出限为0.16mg/L,结果相对标准偏差(RSD,n=12)为1.79%~4.64%,加标回收率为96.3%~101.7%。同时采用紫外-可见分光光度法对偏硅酸含量进行仪器比对,两种测试结果不存在显著性差异,表明该方法具有良好的准确度。通过此方法,可以快速准确测定盐湖卤水中偏硅酸的含量,为提高盐湖资源的综合利用提供了可靠的数据支撑     

阳离子交换树脂分离-离子色谱法测定碳酸稀土和氯化稀土中硫酸根

用阳离子交换树脂柱上交换法将试样中硫酸根与稀土离子分离.交换柱上流出溶液再经AS 9阴离子分离柱(250 mm×4 mm)分离,用9.0 mmol·L-1碳酸钠溶液作流动相.定量测定中采用电导检测器和标准曲线法,该方法的检出限为0.05 mg·L-1,测定下限为0.03%.对硫酸根质量分数为3.19%的试样作精密度试验,测得相对标准偏差(n=11)为1.63%,回收率试验的结果在94.2%～112.6%之间.