Cloud-Point Extraction and Spectrophotometric Determination of Trace Quantities of Bismuth in Environmental Water and Biological Samples

ABSTRACT

A cloud-point extraction (CPE) process using the nonionic surfactant Triton X-114 to extract bismuth from aqueous solutions was investigated. The method is based on the complexation reaction of Bi(III) with 4-(2-benzothiazolylazo)2,2′-biphenyldiol (BTABD) and micelle-mediated extraction of the complex. The optimal extraction and reaction conditions (e.g., pH, reagent concentration, surfactant concentration, and effect of time) were studied. The analytical characteristics of the method (e.g., linear range, molar absorptivity, Sandell sensitivity, optimum Ringbom concentration ranges, limits of detection and quantification, preconcentration factor, and improvement factors) were obtained. Linearity was obeyed in the range of 2.50–85.0 ng mL^?1 of Bi(III) ion. The detection limit of the method was 0.75 ng mL^?1 of Bi(III) ion. The interference effect of some anions and cations was also tested. The method was applied to the determination of bismuth in environmental water, human hair, and urine samples.     

Preconcentration and Separation of Gold(III) from Ore Samples by Solid-Phase Extraction Prior to Its Catalytic Fluorescent Determination

ABSTRACT

A new catalytic kinetic fluorescent quenching method for the determination of trace gold(III) was investigated. The method was based on the catalytic effect of gold on oxidation of 3-(3′-methylphenyl)-5- (2′-arsenoxylphenylazo) rhodanine by hydrogen peroxide in potassium hydrogen phthalate–hydrochloric acid (pH = 3.4). Under the optimum conditions, the great decrease of fluorescence intensity has a linear relationship against the concentration of gold in the range of 0 to 12.0 µg·L^?1 with a detection limit of 6.0 × 10^?10g·L^?1. The coexistent metal ions can be separated, and gold can be enriched by TBP resin of solid-phase extraction, which greatly improves the selectivity and sensitivity of the system. The method can be used to determine trace amounts of gold in ore samples successfully with satisfactory results.     

基于苯基功能化纤维状Fe3O4@SiO2@KCC-1的磁性固相萃取-高效液相色谱测定环境水样中的邻苯二甲酸酯

本文采用共聚法制备了一种新型苯基功能化纤维状Fe₃O₄@SiO₂@KCC-1(Fe₃O₄@SiO₂@KCC-1-phenyl)材料,用于环境水样中邻苯二甲酸酯的磁性萃取. 制备的Fe₃O₄@SiO₂@KCC-1-phenyl展现了单分散的球形纤维状、较强的磁性(29 emu/g)和一个丰富的π电子体系. 研究和优化了洗脱溶剂的种类、吸附剂的用量、萃取时间和可重复使用性等因素对分析物萃取效率的影响. 在最佳条件下,用高效液相色谱方法,采用Fe₃O₄@SiO₂@KCC-1-phenyl萃取分离及测定环境水样中的邻苯二甲酸酯类化合物. 结果表明,本方法具有良好的线性(0.1∽20 ng/mL)、低的检测限(7.5∽29 μg/L, S/N=3). 将该方法应用于不同环境水样中邻苯二甲酸酯类化合物的测定,回收率为93%∽103.4%,相对标准偏差为0.8%∽8.3%.     

2-(2-喹啉偶氮)-5-二甲氨基苯酚固相萃取光度法测定铀的研究

合成了新试剂2-(2-喹啉偶氮)-5-二甲氨基苯酚(QADMAP),用红外光谱、核磁共振氢谱、质谱、可见吸收光谱和元素分析鉴定了其结构。研究了QADMAP与铀的显色反应,在pH 7.8的三乙醇胺-盐酸缓冲介质中,Triton X-100和氟离子存在下,QADMAP与铀(Ⅵ)和氟离子反应生成1∶1∶1紫色三元稳定络合物,络合物的λ_max＝590 nm,ε＝1.05×105 L·mol-1·cm-1,铀含量在0～20 μg·10 mL-1内符合比尔定律。环境水样中的铀用TBP萃淋树脂固相萃取柱分离和富集后用该方法测定,方法相对标准偏差在2.2%～3.6%之间,标准回收率在94%～105%。     

Extraction of Uranium(VI) by Triphenylarsine and Triphenylphosphine Oxides from Nitric Acid Medium

The extraction of UO²⁺ ₂ from nitric acid solutions by two neutral donors ligands (L), triphenylarsine oxide (Ph₃AsO) and triphenylphosphine oxide (Ph₃PO), in chloroform is investigated. At low HNO₃ acid concentrations (<2 M), UO₂ ²⁺ is highly extracted as simple cation by Ph₃AsO and slightly extracted by Ph₃PO. The extraction constant of UO₂ ²⁺ from low nitric acid medium is found to equal 1212 ± 120. At higher HNO₃ concentration (>2 M), UO₂ ²⁺ is extracted by ion association mechanism as UO₂ (NO₃)₂- 2L, and the distribution ratio of UO₂ ²⁺ using Ph₃PO is found to be higher than that of Ph₃AsO. This is interpreted by the extraction competition of HNO₃ for Ph₃AsO. Spectroscopic investigations in the visible and IR regions supported the results obtained.     

氯磺酚偶氮硫代若丹宁固相萃取光度法测定水中的汞

研究了氯磺酚偶氮硫代若丹宁(HSCT)与汞的显色反应,在pH 3.6的HAc-NaAc缓冲介质中,HSCT与汞反应生成2∶1稳定络合物,该络合物可被C₁₈ 固相萃取小柱定量萃取富集,富集倍数达80倍,小柱上保留的络合物用DMF洗脱后用分光光度法测定,在洗脱液中络合物λ_max＝545 nm,ε＝6.24×104L·mol-1·cm-1。汞含量在0～1.5 μg·mL-1内符合比尔定律,方法用于水样中μg·L-1级汞含量的测定,相对标准偏差在1.8%～2.2%之间,标准回收率在93％～106％之间,结果令人满意。     

Study of (Al2O3)n(Ox) clusters with n = 16 and x = 0, 1, 2 from first principles calculations

The ionic and electronic structure of (Al₂O₃)_n(O_x) clusters with n 16 and x = 0, 1, 2 is studied by means of first principles density functional calculations, norm-conserving pseudopotentials and a numerical atomic basis set. The equilibrium geometries have been determined by total energy minimization, starting with several initial geometries for each cluster size. The trends obtained for the atomic arrangements (structural isomers, coordination numbers, disordered versus ordered structures, etc.) and the electronic properties (binding energies, Homo-Lumo gap and dipole moments) are discussed. For most of the oxidized clusters studied here we find that the Homo-Lumo gap and the magnitude of dipole moment of isomeric species can vary drastically.     

Darboux Transformation and Soliton Solutions for the (2+1)-Dimensional Generalization of Shallow Water Wave Equation with Symbolic Computation

In this paper,the (2+1)-dimensional generalization of shallow water wave equation,which may be used to describe the propagation of ocean waves,is analytically investigated.With the aid of symbolic computation,we prove that the (2+1)-dimensional generalization of shallow water wave equation possesses the Painlev property under a certain condition,and its Lax pair is constructed by applying the singular manifold method.Based on the obtained Lax representation,the Darboux transformation (DT) is constructed.The first iterated solution,second iterated solution and a special N-soliton solution with an arbitrary function are derived with the resulting DT.Relevant properties are graphically illustrated,which might be helpful to understanding the propagation processes for ocean waves in shallow water.     

Darboux Transformation and Soliton Solutions for the (2+1)-Dimensional Generalization of Shallow Water Wave Equation with Symbolic Computation

In this paper, the (2+1)-dimensional generalization of shallow water wave equation, which may be used to describe the propagation of ocean waves, is analytically investigated. With the aid of symbolic computation, we prove that the (2+1)-dimensional generalization of shallow water wave equation possesses the Painlevé property under a certain condition, and its Lax pair is constructed by applying the singular manifold method. Based on the obtained Lax representation, the Darboux transformation (DT) is constructed. The first iterated solution, second iterated solution and a special N-soliton solution with an arbitrary function are derived with the resulting DT. Relevant properties are graphically illustrated, which might be helpful to understanding the propagation processes for ocean waves in shallow water.