A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.     

Preparation of porous nano-calcium titanate microspheres and its adsorption behavior for heavy metal ion in water

Using D311 resin as a template, porous nano-calcium titanate microspheres (PCTOM) were prepared by a citric acid complex sol-gel method and characterized by X-ray diffraction (XRD), SEM and FTIR. The method's adsorption capabilities for heavy metal ions such as lead, cadmium and zinc were studied and adsorption and elution conditions were investigated. Moreover, taking the cadmium ion as an example, the thermodynamics and kinetics of the adsorption were studied. The results show that the microspheres were porous and were made of perovskite nano-calcium titanate. The lead, cadmium and zinc ions studied could be quantitatively retained at a pH value range of 5-8. The adsorption capacities of PCTOM for lead, cadmium and zinc were found to be 141.8 mg g(-1), 18.0 mg g(-1) and 24.4 mg g(-1) respectively. The adsorption behavior followed a Langmuir adsorption isotherm and a pseudo-second-order kinetic model, where adsorption was an endothermic and spontaneous physical process. The adsorbed metal ions could be completely eluted using 2 mol L(-1) HNO(3) with preconcentration factors over 100 for all studied heavy metal ions. The method has also been applied to the preconcentration and FAAS determination of trace lead, cadmium and zinc ion in water samples with satisfactory results.     

Novel analytical reagent for the application of cloud-point preconcentration and flame atomic absorption spectrometric determination of nickel in natural water samples

Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 degrees C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ngml(-1). The extraction efficiency was investigated at different nickel concentrations (20-80 ngml(-1)) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence level.     

甘蔗渣制备生物形态分级多孔木质陶瓷

采用甘蔗渣为生物质原料,浸渍环氧树脂后(两者质量比为2.5∶1)高温烧结制备了分级多孔木质陶瓷。使用XRD、SEM、TG等手段研究了木质陶瓷的物相组成、微观形貌和热稳定性,通过压汞法和氮吸附法分析了木质陶瓷从微米到纳米范围的分级多孔结构。研究结果表明,木质陶瓷主要由非石墨化碳层和微量的磷石英组成。木质陶瓷保留了甘蔗渣的管状孔洞,具有从宏孔到介孔分布的分级多孔结构。木质陶瓷的宏孔孔径分布主要在0.4～6μm之间,BET表面积最高达39.7m2/g。随着烧结温度的升高,木质陶瓷的BET表面积、介孔体积和平均孔径都降低。     

Preparation and characterization of biomorphic nickel oxide microtubes templated from cotton

Biomorphic nickel oxide microtubes with mesoporous structure were successfully prepared from cotton templates. By the infiltration of nickel nitrate solution into cotton, followed by calcination at 673 K in oxygen for 1 h, the product was obtained. The sample was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy and nitrogen absorption-desorption. Compared with regular nickel oxide prepared without using cotton, biomorphic nickel oxide exhibited an enhanced antimicrobial activities, ferromagnetic behavior and photocatalytic activities due to the formed special microstructure.     

多孔镍载体材料的制备

试验在常规粉末冶金方法基础上通过添加造孔剂的办法制备出高孔率(70%以上)、小孔径(最大冒泡孔径＜5 μ m)、高透过量,通孔率(通孔率可达97%以上)的多孔镍载体材料.主要进行了粉末粒度及形貌的分析选择研究,造孔剂的添加量与多孔镍载体性能关系的研究、烧结工艺对材料性能影响的研究.主要从孔率、最大冒泡孔径、透气系数、通孔率等方面着手,研究了造孔剂加入量及烧结工艺对该性能的影响,同时对不同条件下样品的性能进行了测试.     

Determination of trace nickel in water samples by cloud point extraction preconcentration coupled with graphite furnace atomic absorption spectrometry

A new method based on the cloud point extraction (CPE) preconcentration and graphite furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of trace nickel in water samples. When the micelle solution temperature is higher than the cloud point of surfactant p-octylpolyethyleneglycolphenyether (Triton X-100), the complex of Ni2+ with 1-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) could enter surfactant-rich phase and be concentrated, then determined by GFAAS. The main factors affecting the cloud point extraction were investigated in detail. An enrichment factor of 27 was obtained for the preconcentration of Ni2+ with 10 mL solution. Under the optimal conditions, the detection limit of Ni2+ is 0.12 ng mL(-1) with R.S.D. of 4.3% (n = 10, c = 100 ng mL(-1)). The proposed method was applied to determination of trace nickel in water samples with satisfactory results.     

食品工业中的双极膜技术

双极膜是近年来国际上研究比较活跃的一种新型膜．基于双极膜的水解离技术乒逐渐成为一种通用的目标单元操作，可用于多种工业过程，如化工生产、湿法冶金、环境保护和资源回收等领域，并大大地改变了这些领域的面貌．本文针对食品工业领域，介绍了双极膜在食品化工中的应用和研究现状．     

Preparation and adsorbing performance of calcium titanate with template method

In this paper, using furfural residue as a template, porous calcium titanate (FPCT) was prepared by a sol-gel method and characterized by XRD, SEM, and nitrogen adsorption method. The conditions of preparation were investigated. The adsorption capabilities of FPCT for heavy metal ions were studied, and the adsorption mechanism was investigated. The results show that the calcium titanate was porous, and material is composed of crystals in nanoparticle size with a small amount of calcium sulfate impurities, while the sulfuric acid in furfural residue is fixed as the calcium sulfate in the material. The adsorbed quantity is affected by the pH value of medium and time. When the pH value of medium is 5, and oscillating adsorption lasts for 30?min, the adsorbed quantities of Cd, Pb, Zn, Cu, and Ni are 118.04, 197.96, 64.98, 56.85, and 47.91?mg/g, respectively. The adsorption conforms to the Langmuir adsorption isothermal model and pseudo-second-order kinetic equation, and is a spontaneous endothermic process driven by entropy. After adsorption, adsorbents can be regenerated with 1?mol/L nitrate solution. It is used for eliminating Cd, Pb, Zn, Cu, and Ni in wastewater and the results are satisfactory.     

聚硅氧烷型交联剂的制备及其在聚合物多孔材料中的应用

为了获得性能优异的聚合物多孔材料,首先,在封端剂六甲基二硅氧烷(MM)的存在下,通过硅酸钠与甲基丙烯酰氧基丙基三甲氧基硅烷(MPS)的水解缩聚反应制备了含甲基丙烯酰氧基丙基官能基团的MTQ有机硅树脂;然后,以MTQ硅树脂为交联剂,丙烯酸异辛酯(EHA)为单体,利用高内相比乳液模板法制备了MTQ硅树脂/聚丙烯酸异辛酯(PEHA)聚合物多孔材料;最后,对该多孔材料的孔结构、压缩性能和热稳定性进行了研究。结果表明:采用MTQ硅树脂作为交联剂制备得到的MTQ硅树脂/PEHA聚合物多孔材料的泡孔孔径介于4~10μm范围内,毛孔孔径分布于0.3~2.0μm区间内;泡孔之间紧密相连,毛孔均匀分布且通道较窄。MTQ硅树脂含量对MTQ硅树脂/PEHA聚合物多孔材料的比表面积和孔容的影响较小,但可显著提高聚合物多孔材料的热稳定性和压缩强度;在氮气氛围下,聚合物多孔材料的最大热分解速率温度可达411.5℃。     

海藻酸钙多孔支架的制备研究

利用冷冻干燥法制备海藻酸钙组织工程多孔支架,对支架的形貌进行分析,同时考察了支架的吸水性能.结果表明,冷冻干燥法制备的海藻酸钙多孔支架具有开放、贯通的多孔结构,孔径范围在100～300μm之间,利于细胞生长和物质传输.2%海藻酸钠经-5℃预冻所得支架结构最为规整,对蒸馏水和生理盐水的吸水率分别为985%和1088%.     

Flow injection preconcentration system using a new functionalized resin for determination of cadmium and nickel in tobacco samples

A solid-phase extraction method combined with flow injection (FI) on-line flame atomic absorption spectrometry (FAAS) for the determination of cadmium and nickel in tobacco samples is presented. The 2-aminothiophenol functionalized Amberlite XAD-4 (AT-XAD) resin was synthesized by covalent coupling of the ligand with the copolymer through a methylene group. A minicolumn packed with AT-XAD was connected into the automated on-line preconcentration system. Elution of metal ions from minicolumn can be made with 0.50 mol L⁻¹ hydrochloric acid solution. With a consumption of 21.0 mL of sample solution, detection limits (3 s) of 0.3 (Cd) and 0.8 μg L⁻¹ (Ni) were achieved at a sample throughput of 18 h⁻¹. Enrichment factors (EF) of 99 (cadmium) and 43 (nickel) were obtained compared with the slope of the linear portion of the calibration curves before and after preconcentration. The contents of Cd and Ni in a certified reference material (NIST 1570a, spinach leaves) determined by the present method was in good agreement with the certified value. The developed procedure was also successfully applied to the determination of Cd and Ni in local tobacco samples.     

Development of a cloud-point extraction method for copper and nickel determination in food samples

A new, simple and versatile cloud-point extraction (CPE) methodology has been developed for the separation and preconcentration of copper and nickel. The metals in the initial aqueous solution were complexed with 2-(2'-benzothiazolylazo)-5-(N,N-diethyl)aminophenol (BDAP) and Triton X-114 was added as surfactant. Dilution of the surfactant-rich phase with acidified methanol was performed after phase separation, and the copper and nickel contents were measured by flame atomic absorption spectrometry. The variables affecting the cloud-point extraction were optimized using a Box-Behnken design. Under the optimum experimental conditions, enrichment factors of 29 and 25 were achieved for copper and nickel, respectively. The accuracy of the method was evaluated and confirmed by analysis of the followings certified reference materials: Apple Leaves, Spinach Leaves and Tomato Leaves. The limits of detection expressed to solid sample analysis were 0.1 microg g(-1) (Cu) and 0.4 microg g(-1) (Ni). The precision for 10 replicate measurements of 75 microg L(-1) Cu or Ni was 6.4 and 1.0, respectively. The method has been successfully applied to the analysis of food samples.     

Understanding the wetting properties of nanostructured strontium titanate and its application for recyclable oil/water separation

In the present work, we have investigated the oil and water wetting properties of strontium titanate nanoparticles. The as-synthesized nanoparticles were coated on the stainless steel mesh to investigate wetting properties. The coated mesh was found to have superhydrophilic and superoleophilic behavior with a contact angle value of nearly zero degree for both water as well as oil. Further underwater oil contact angle was measured, showing underwater superoleophobic behavior of the coated mesh. The underlying mechanism was studied for the wetting behavior of strontium titanate coated mesh. The coated mesh was then utilized for the gravity-driven separation of different oil/water mixtures. The separation mesh can be used multiple times showing its antifouling property along with recyclability. Further, a capillary pressure based model was developed to explain the wettability contrast for water and oil as well as separation of the two liquid phases on passing through the separation device. The approach here used for fabrication is applicable for large-area fabrication making it convenient and cost-effective towards oil/water separation at large scale.     

固体超强酸于多孔高硅氧纤维的负载及其在酯化中的应用

以溶胶浸渍法,将SO42-/ZrO2固体超强酸负载到由酸沥滤工艺制备的多孔高硅氧纤维上,并用于催化合成乙酸正丁酯。研究结果表明,该催化剂具有用量少,酯收率较高,产物易于分离等优点;而且使用寿命长,重复用于5次合成后,酯化率仍高于70%。     

纤维素-海藻酸钠-海泡石多孔微球的制备及其对亚甲基蓝吸附性能

以微晶纤维素(Microcrystalline cellulose,MCC)和海藻酸钠(Sodium alginate,SA)为网络框架,海泡石(Sepiolite,SEP)为功能单元,采用悬浮液滴法构建纤维素-海藻酸钠-海泡石(MCC-SA-SEP)双网络多孔复合微球。通过SEM和TG对复合微球结构和热稳定性能进行表征,并研究该微球对亚甲基蓝(Methylene blue,MB)水溶液的吸附性能。结果表明,MCC-SA-SEP复合微球呈现三维网络多孔结构,且随着SEP含量的增加热稳定性逐渐提高。吸附结果显示MCC-SA-SEP符合准二级动力学模型和Langmuir等温线,对MB的饱和吸附容量高达333.3 mg/g。经过五次再生循环后,对MB吸附能力仍能维持85.4%,表明该多孔复合微球可以作为一种高效可再生的有机-无机复合吸附剂用于染料废水处理。      

Reaction-based fluorescent probe for selective discrimination of thiophenols over aliphaticthiols and its application in water samples

The development of highly sensitive and selective detection techniques for the discrimination of relevant toxic benzenethiols and biologically active aliphatic thiols is of considerable importance in the fields of chemical, biological, and environmental sciences. In this article, we describe a new design of reaction-based fluorescent probe for discrimination of thiophenols over aliphaticthiols through intramolecular charge transfer pathways using N-butyl-4-amino-1,8-naphthalimide as a fluorophore, the strongly electron-withdrawing 2,4-dinitrobenzenesulfonamide group as a recognition unit, and 2,3-dihydroimidazo-[1,2-a] pyridine moiety as a linker. This rational design not only affords finely tunable spectroscopic properties by adding 2,3-dihydroimidazo-[1,2-a] pyridine moiety but also provides the chance to regulate the selectivity and sensitivity of the probe due to the formation of a new type of potentially reversible sulfonamide bond through 4-dimethylaminopyridine-like resonance. The developed probe displayed high off/on signal ratios, good selectivity, and sensitivity with a detection limit of 20 nM and a relative standard deviation of 1.7% for 11 replicate detections of 0.33 μM thiophenol and was successfully applied to the determination of thiophenols in water samples with quantitative recovery (from 94% to 97%) demonstrating its application prospect for thiophenols sensing in environmental and biological sciences.     

多孔无机膜的制备和应用

对目前较常见的多孔无机膜的制备方法及其在各个领域的应用进行了概述 ,并比较了各种制备方法的优缺点     

Kinetic dissociation of nickel titanate and nickel tungstate in oxygen potential gradients

Nickel titanate (NiTiO₃) and nickel tungstate (NiWO₄) were exposed to oxygen potential gradients at 1400 and 1100° C, and they were found to dissociate into their constituent oxides, namely, NiO and TiO₂, and WO₃ and NiO, respectively. This is consistent with the non-equilibrium phenomenon of kinetic decomposition. In the case of nickel titanate, at the low-oxygen-potential side, TiO₂ was formed as sharp needle-like structures within the titanate matrix, while at the high-oxygen-potential side, NiO was formed. In contrast, NiO was formed at the lower-oxygen-potential side in the case of nickel tungstate, while WO₃ volatized off from the high-oxygen-potential side. This indicated that W diffuses faster than Ni in tungstates. In both cases, there were significant macroscopic shifts of the oxide with respect to the original position, established with Pt markers, towards the high-oxygen-potential side.