Batchwise separation of gallium by an anion exchange resin loaded with a sulphonated azo dye

Gallium(III) is sorbed by a strong base anion exchange resin loaded with a sulphonated azo-dye, T-azo-R [1-(tetrazolylazo)-2-hydroxynaphthalene-3,6-disulphonic acid], which is able to complex it in aqueous solution. As sorption takes place at acidities at which the hydrolysis of gallium is not negligible, it must be considered as conconmitant equilibrium. The distribution equilibria depend on the amount of ligand sorbed, and on the volume, acidity and ionic composition of the aqueous solution, according to the Gibbs-Donnan model. The thermodynamic complexation constant in the resin phase can be calculated from the experimental distribution coefficients; the value of log K = -1.24(0.20) is in acceptable agreement with that in aqueous solution [log K = -0.75(0.33)] which was also determined in the present investigation. Two equations deriving from the Gibbs-Donnan model are used for predicting the conditions for sorption and elution of gallium by a batch procedure, and for separating it from aluminium.     

Column chromatographic separation of gallium, indium and thallium

Distribution ratios are given for the extraction of gallium-(III), indium(III) and thallium(III) from aqueous solutions of hydrobromic acid into di-isopropy ether and isobutyl methyl ketone. Based on the results obtained, a scheme is presented for the quantitative separation of these elements from each other by liquid-liquid partition chromatography. The effect of a number of other metal ions upon the separation is also studied. The separation method has been applied to the analysis of a series of lead-indium alloys.     

Utilization of anion exchange resin Spectra/Gel for separation of arsenic from water

Arsenic in drinking water is one of the most challenging health hazards facing mankind today. Arsenic is a naturally occurring carcinogen and creates epidemiological problems through chronic ingestion from drinking water. Arsenic is present in water primarily as As(III) or As(V). Removal of both As(III) and As(V) from water by adsorption on strong base anion-chloride has been studied. Arsenic concentration was measured by Inductively Coupled Argon Plasma (ICP) analysis. The resin was regenerated and the adsorbed arsenic fractions were eluted by using 2 M NaCl. The effect of different parameters that influence adsorption process, such as relative arsenic and resin concentrations, retention time, and pH, were investigated. Results obtained revealed that As(III) was poorly adsorbed, whereas As(V) was successfully retained on the resin. The adsorption process was optimized by using 1 g resin for 16 ppm As(V) at pH 9 for 30 min. The removal efficiency of As(V) was 99.2%.     

An electrolytic system based on the anion exchange reaction between KCl and an anion exchange resin

We have developed a novel electrolytic system based on the anion exchange reaction between KCl and Amberlyst A26. It was demonstrated by preparative electrolysis experiments as well as cyclic voltammetry that the anion exchange reaction offers a unique electrolytic system for electroreduction of organic compounds. On the basis of the electrolytic system, electroreduction of aromatic carbonyl compounds was successfully achieved by using an undivided cell to provide the corresponding coupling products as pinacols in good to high yields with high diastereoselectivity.     

Spectroscopy of laser-excited indium,gallium and indium–gallium systems

The spectroscopy of dense Ga, In and In–Ga vapours is studied via resonant pulsed laser excitation at 403.4 nm (Ga) and 410.3 nm (In). Besides some known atomic Rydberg levels emission, satellite wings on the blue side of the fundamental transitions show up both in the homonuclear and heteronuclear vapours. They are due to the presence of excited homonuclear dimers that form in the collision between excited and ground-state atoms. The formation of heteronuclear dimers is inferred by the time-resolved analysis of some atomic fluorescences.     

阴离子交换树脂分离-原子荧光法测定色母粒中的镉

采用微波消解溶样,结合离子交换法对色母粒样品进行待测元素的提取及净化处理,利用原子荧光光度计进行镉含量的测定。研究了717型阴离子交换树脂对色母粒样品中镉的吸附及分离条件,解决了样品中铅、铜等元素的干扰问题。方法加标回收率在92.4%～117.4%之间,相对标准偏差小于3.0%。     

Solvent extraction and separation of gallium, indium and thallium with N-benzylaniline

A simple and rapid method is proposed for the separation of tervalent gallium, indium and thallium by solvent extraction with N-benzylaniline in chloroform from different concentrations of hydrochloric acid. Thallium and gallium are extracted from 1M and 7.0-7.5M hydrochloric acid respectively. Indium is finally extracted from hydriodic acid. These metals in the final extracts are determined complexometrically. Interference from some cations can easily be eliminated by reduction with sulphite, followed by selective oxidation of thallium(I) to thallium(III) with saturated bromine water, and from others by the use of thioglycollic acid as a masking agent in the extraction of gallium and indium. Most common anions cause no interference. Log-log plots of distribution coefficients vs. concentration of amine for gallium, indium and thallium indicate a 2:1 limiting mole ratio of amine to these metals.     

阴离子交换树脂分离香菇多糖中蛋白质

香菇多糖是从香菇中提取分离出的一种药用活性成分,具有抗肿瘤,抗病毒,提高人体免疫力等功能,在临床上具有很好的应用前景[1~3]。多糖的药效与多糖的纯度有很大关系,要得到较纯的多糖,工艺复杂,成本很高,因此市场上大多香菇多糖产品纯度较低。香菇多糖中难分离的杂质主要是蛋白     

330阴离子交换树脂对草甘膦的吸附性能

采用静态吸附法研究了330阴离子交换树脂对水中草甘膦的吸附性能,并研究了吸附动力学;测定了溶液的pH值、温度、NaCl含量等因素对330树脂吸附草甘膦的影响.结果表明:330树脂对水中草甘膦的吸附速率快;在pH=2.69时对草甘膦的吸附性能最好;330树脂对草甘膦的吸附是放热、自发的过程,吸附等温线符合Freundli...     

On the use of anion exchange resin and acidic-organic mixtures in the separation of Na,Cs and Ba

A systematic study was carried out on the adsorption behaviour of Na, Cs and Ba on Dowex 1X8 from various concentrations of hydrochloric and nitric acid solutions. The addition of water-miscible organic solvents to the acidic solutions was found to increase the K_d values for these elements to different extents, which provides a useful method for the separation of carrier-free Ba from irradiated Cs. The effect of kind and content of the different alcohols on the adsorption of Ba was also investigated. It was found that K_d increases with the increase of the alcohol content as well as with the increase of both the dielectric constant and chain length of the alcohol. This effect was found to be more pronounced in the case of nitric acid media.     

Esterification of palmitic acid with epichlorohydrin on anion exchange resin catalyst

The esterification reaction of palmitic acid with epichlorohydrin catalyzed by an anionic macroporous resin was studied. Purolite A-500 resin proved to be a very effective catalyst in the synthesis of 3-chloro-2-hydroxypropyl palmitate. The effects of certain parameters such as speed of agitation, catalyst particle size, catalyst loading, temperature, initial molar ratio between reactants on the rate of reaction were studied. It was found that the overall rate is intrinsically kinetically controlled. The structure of synthesized ester was confirmed by FTIR and ¹H NMR analyses.      

FI-spectrophotometric determination of uranium after preconcentration on an anion exchange resin

An economical, fast, sensitive and selective method for the determination of uranium (VI) from sulfate media based on the flow injection on-line preconcentration in a minicolumn having amberlite IRA-402 (strong anion exchange) resin is described. Uranium (VI) was selectively adsorbed on the resin as uranyl trisulfate complex from aqueous solution of pH 2 in the minicolumn (2.56 mm i.d. and 7.5 cm in length) at a flow rate of 10 ml min^?1. The adsorbed uranyl trisulfate complex was eluted by HClO₄ (0.1 mol l^?1, 6.5 ml min^?1) and mixed with arsenazo-III (0.05 %, 6.5 ml min^?1), and passed through the flow through cell of spectrophotometer where its absorbance was measured at 653 nm. Various parameters affecting adsorption and elution of the uranium complex were optimized. For data analyses peak absorbance was used. For 60 and 180 s preconcentration time, enrichment factors (EF) 20 and 40, sampling frequency (SF) 45 and 18 h^?1; and detection limits (DL) (3σ) 14.2 and 8.6 μg l^?1 were obtained, respectively. To enhance the sensitivity of the system, two minicolumns (described above) were used for simultaneous preconcentration and elution purpose. For 60 and 180 s preconcentration time, EF 30 and 50, SF 42 and 17 h^?1 and DL (3σ) 4.4 and 3.44 μg l^?1 were obtained, respectively. The effect of various anions and cations was studied for single column manifold. High selectivity of this method was observed. All the anions and cations studied did not interfere up to 330 times higher mass ratio to 300 μg l^?1 U (VI) except Th(IV) which was tolerated up to 133 times by the addition of washing step in the manifold. The method based on single column manifold was applied on the spiked tap water, biological sample CRM (IAEA-V4) and synthetic leach liquor solution and good recovery was obtained. The method based on dual column manifold was validated on lake sediment SL-1 (CRM) and the results obtained were in good agreement at 95 % confidence level with the given value.     

Local structure around chloride ion in anion exchange resin

Neutron diffraction measurements on 35Cl/37Cl isotopically substituted anion exchange resins were carried out in order to obtain direct information on the local structure around the chloride ion absorbed in the resin. Structural parameters concerning the first nearest-neighbor interaction of chloride ions were determined through a least-squares fitting procedure of the observed first-order difference function, DeltaCl(Q). It has been revealed that the chloride ion is neighboring an ion exchange group (-CH2(CH3)3N+) with a Cl-...N distance of 3.10(3) A, and simultaneously bonded with 2.4(1) D2O molecules with a Cl-...D distance of 2.25(2) A. The second and third nearest water molecules around Cl- have also been observed. These results indicate that the direct ionic interaction between Cl- and -CH2(CH3)3N+ drastically reduces the number of first-neighbor water molecules around Cl- but enhances the long-distance structuring of the remaining water molecules in the environment surrounded by a hydrophobic polymer matrix.     

Calcium-strontium separation by means of mixed solvent anion exchange

The separation of strontium and yttrium from calcium on the anion exchanger column with alcohol solution of nitric acid as eluent may be described by Glueckauf's model of elution chromatography. Experimental and theoretical results have shown that this separation is characterized by a small number of theoretical plates of the separation column. This model may also be applied for the simulation of the separation of strontium and yttrium from calcium in the strontium isolation from natural samples. The model parameters may be used for the assessment of the optimum column dimension and the optimum working conditions for the isolation of radioactive strontium and yttrium from natural samples.     

Spectrophotometric determination of titanium after separation by anion exchange

A method is outlined for separation of titanium by anion exchange and subsequent spectrophotometric determination. Titanium fluoride is adsorbed quantitatively on a column of strongly basic anion exchanger and thus separated from ions which would normally interfere. The spectrophotometric measurement is achieved by formation of the intensely yellow and stable titanium ascorbate complex which has a maximum absorbance at 355 mμ.     

Weak anion and cation exchange mixed-bed microcolumn for protein separation

To separate proteins with a wide distribution of pIs under the conditions compatible to online tryptic digestion (with preferable pH=8.0), weak anion and cation exchange chromatography (WAX/WCX) mixed‐bed microcolumn has been developed. With a mixture of five proteins with pIs ranging from 4.2 to 11.4, the effect of WAX/WCX ratio on the separation performance was investigated, and an optimum packing ratio of 1:1 w/w was obtained. Moreover, the undesirable hydrophobic interaction between the proteins and the stationary phase was suppressed with 10% ACN v/v added in the mobile phases. Under the optimized conditions compatible to tryptic digestion, basic and acidic proteins were resolved simultaneously, with RSDs of relative retention time on six columns less than 6%, indicating the good resolution and packing reproducibility. Furthermore, one RPLC fraction of proteins extracted from rat middle brain and the whole protein mixture extracted from rat liver were analyzed, respectively. The results demonstrated better separation performance on WAX/WCX microcolumns than that on both weak anion exchange chromatography and weak cation exchange chromatography at pH ～8. We anticipate that WAX/WCX microcolumns are promising for the integration of protein separation and tryptic digestion aiming at high‐throughput proteome study.     

Solid-state high-resoluction NMR studies on gallium arsenide and indium gallium arsenide semiconductors

Chemical shifts of GaAs and InGaAs were observed by solid-state high-resolution NMR. The spectrum of GaAs appeared as a single peak but that of InGaAs consisted of an intense narrow peak and a weak broad one which appeared at ≈10–15 ppm slightly higher field from the former.     

一种表面共聚氢氧根选择性阴离子色谱固定相

报道了一种基于聚(苯乙烯-二乙烯基苯)微球(PS-DVB)的表面共聚氢氧根选择性阴离子固定相。它以烯丙基缩水甘油醚(AGE)为功能单体、通过自由基引发直接与PS-DVB微球表面残留的悬挂双键共聚,再通过醇胺开环得到。考察了两种醇胺试剂对分离的影响;扫描电镜、红外光谱、元素分析表征结果表明:表面共聚反应成功在微球表面引入季胺基团,且对微球理化性质无显著影响;所得固定相表现氢氧根淋洗液的高选择性,对常规无机阴离子表现出良好的分离性能(分离度>1.5)和运行稳定性(保留时间的相对标准偏差<1.13%),其实用性通过分析茶叶样品中无机阴离子进行了展示。     

Synthesis and characterization of pyridyl anion exchange resin for 99Tc removal

Journal of Radioanalytical and Nuclear Chemistry - A new pyridyl anion exchange resin (PS-N) was synthesized by chloroacetylation and quaternization on the polystyrene-divinylbenzene microspheres...     

Extraction and separation of gallium, indium and thallium with several carboxylic acids from chloride media

A method is proposed for the extraction and individual separation of trivalent gallium, indium and thallium with sec-octylphenoxy acetic acid (CA-12), sec-nonylphenoxy acetic acid (CA-100) and naphthenic acid (NA) from chloride media. The distribution equilibria of gallium (III), indium (III), thallium (III) and thallium (I) between carboxylic acids (CA-12, CA-100 and NA) dissolved in kerosene and acidic aqueous chloride media has been investigated as a function of the concentration of extractants and the concentration of hydrogen ion in aqueous phase. A possible mechanism of the extraction is discussed. The method permits rapid and precise individual separation of gallium (III), indium (III) and thallium (III), and is applicable to the analysis of alloy samples.