铋膜电极阳极溶出伏安法检测痕量Cd金属

镉氧化产生的溶出电流与样品中Cd²⁺的浓度有关。本研究通过方波阳极溶出伏安法(SWASV)在活化铋膜电极(Activated BFE)上对低浓度μg/L水平的Cd(II)进行测定。通过电化学方法对电极进行初步改性, 然后电沉积制备铋膜再次对电极进行改进, 从而增强了对痕量目标Cd²⁺的敏感性。对改性前后的玻碳电极(GCE)表面进行SEM、CV、EIS和SWV的表征。为了将这种伏安法传感器应用于含有低浓度Cd²⁺的实际样品中, 对检测Cd²⁺的实验参数进行了研究。使用选定的条件, 在10 min的预富集条件下Cd²⁺的检测限为1 μg/L。     

Further study on different dopings into PbWO4 single crystals to increase the scintillation light yield

Since we presented our preliminary result (Nucl. Instr. and Meth. A 486 (2002) 170) at SCINT2001, we have continued our efforts to increase the light yield (LY) of PbWO₄ scintillators by extending different dopings with an aim to find a possibility of using PbWO₄ successfully in Positron Emission Tomography (PET). Overall result obtained for single doping as well as double and tripple co-dopings are summarized, including decay characteristics and radiation hardness. The LY in non-doped PbWO₄ crystals with a size of 10×10×(20–30) mm³ is 25–35 photolectrons/MeV (phe/MeV) corresponding to 3–4% of the LY in BGO, when measured with a bialkali photomultiplier during a gate of 1 μs. The maximum LY increased to 49 phe/MeV for single doping with Mo⁶⁺, 80 phe/MeV for double co-doping of Mo⁶⁺+Sb⁵⁺, and 85 phe/MeV for tripple co-doping of Mo⁶⁺+Cd²⁺+Sb⁵⁺. The radiation hardness is larger than 10⁵ Gy for each of the samples co-doped with Mo⁶⁺+Sb⁵⁺ and Mo⁶⁺+Cd²⁺+Sb⁵⁺, while it is much poorer in PWO:Mo⁶⁺. In each of these co-doped samples, a medium-speed green emission in the microsecond range is created besides the fundamental fast (a few nanoseconds range) blue one, giving a peak at 500 nm in the radioluminescence spectrum similarly as in PWO:Mo⁶⁺.     

One pot synthesis of monodispersed L-glutathione stabilized gold nanoparticles for the detection of Pb2+ ions

Direct mixture of Au³⁺ with glutathione (GSH), which act as both reduction agents and stabilizers, in aqueous solution gave rise to production of gold nanoparticles (Au NPs) with uniform sizes of around 21 nm. The GSH stabilizer Au NPs in solution show immediate aggregation after addition of 1 mol/L NaCl aqueous solution containing Pb²⁺ ions. The Pb²⁺-induced aggregation in Au NP solution is monitored by both colorimetric response and UV-vis spectroscopy. A rather broad linear range (from 0.1 to 30 μmol/L) and low detection limit (0.1 μmol/L) are explored for Au NP sensors used for detection of Pb²⁺ ions. Furthermore, the response of GSH-stabilized Au NPs toward Pb²⁺ ions is specific compared with other possible interferants (Hg²⁺, Mg²⁺, Zn²⁺, Ni²⁺, Cu²⁺, Co²⁺, Ca²⁺, Mn²⁺, Cd²⁺, and Ba²⁺).     

Enhancing foam drainage using foam fractionation column with spiral internal for separation of sodium dodecyl sulfate

A new type of foam fractionation column with spiral internal had been designed for enhancing the foam drainage and thus for the removal of minute hazardous materials. The column without spiral internal was served as the comparison column, and an anionic surfactant sodium dodecyl sulfate (SDS) was used as the foaming solution. Effects of liquid loading volume, initial SDS concentration and superficial gas velocity on enrichment ratio and recovery percentage of SDS were investigated. The experimental results showed that the spiral column successfully enhanced the enrichment ratio of SDS by reducing countercurrent resistance between the rising bubbles and the entrained liquid of reflux. Enrichment ratio of SDS obtained by using the spiral column was 15.7, which was 2.5 times of that obtained by using the comparison column under the suitable operating conditions of liquid loading volume 0.4 L, initial SDS concentration 0.2g/L and superficial gas velocity 1.7 mm/s.     

一种新型膦酸锆孔材料的合成及其对金属离子的吸附性质

骨架含强配位基的有机无机杂化多级孔材料合成是目前吸附研究的一个重要领域。以bis (hexamethylene) triamino-N, N-bisacetyl-phosphonic acid和ZrOCl₂·8H₂O为原料、应用水热合成技术合成了一种新型膦酸锆多级孔材料ZrPTA, 并通过FT-IR、TGA、XRD、XPS、SEM以及元素分析等手段对制备产物进行了表征。研究结果表明, ZrPTA具有棒状微形貌, 其内部存在大量直径为1.38 nm和1.93 nm的微孔以及直径为2.99 nm的介孔, 其表面积为112.2 m²/g。ZrPTA对水溶液中Pb²⁺、Cu²⁺和Cd²⁺三种金属离子具有良好的吸附作用, 最大吸附量分别为742.7、689.8和627.0 mg/g, 远远高于文献报道值。这一性质使ZrPTA具有潜在的废水处理功效, 显示出诱人的应用前景。     

Cadmium Selective PVC-Membranes Sensor Based on 1, 2-Bis (Quinoline-2-Carboxamido) -4-Chlorobenzene as a Neutral Carrier

The 1, 2-bis(quinoline-2-Carboxamido)-4-chlorobenzene (H₂Clbqb) was used as an excellent ionophore in the construction of a cadmium(II)-selective PVC-based membrane sensor. The influences of membrane compositions on the potentiometric response of the electrodes have been found to substantially improve the performance characteristics. The best performance was obtained with a membrane composition of (H₂Clbqb) (5%): PVC (31%): DBP (61%): NaTPB (3%). The sensor shows a Nernestian response for cadmium ions over a wide concentration range (1.0times10⁶ to 1.0 times 10^-1 mol.L^-1) with slope of 30.3 plusmn0.4 mV decade¹. The limit of detection was 8.0 times10^-7 mol.L^-1. It illustrates a relatively fast response time in the whole concentration range (< 10 s) and it can be used for at least 8 weeks without any divergence in potential. The electrode can be used in the pH range from 2.4 to 9.0. The selectivity coefficient of some alkali, alkaline earth, transition and heavy metal ions towards Cd²⁺ion have been determined. The results show proposed Cd sensor is selective over a number of mono, bi- and trivalent cations such as Pb²⁺, Fe³⁺, Ni²⁺, K⁺, and Mg²⁺. The analytical usefulness of the proposed electrode has been evaluated by its application in the determination of cadmium in real samples. It was successfully applied for the direct determination of Cd²⁺ in standard and real sample solutions.     

聚天冬氨酸/木质纤维素水凝胶的制备及吸附性能

采用水溶液聚合法合成聚天冬氨酸（PASP）/木质纤维素（LNC）水凝胶;考察了预处理时间、预处理温度、KMnO₄浓度、戊二醛用量、PASP的用量、反应时间以及反应温度对PASP/LNC水凝胶吸附Pb2+、Cd2+性能的影响;运用Langmuir吸附等温线计算PASP/LNC水凝胶最大吸附量;使用HNO₃对PASP/LNC水凝胶进行脱附再生实验;采用SEM和FTIR对水凝胶的结构进行表征。吸附结果表明:预处理时间15 min,预处理温度50 ℃、KMnO₄浓度0.06 mol·L-1、戊二醛用量1.00 g、PASP用量11 g、反应时间3.5 h且反应温度70 ℃时,对Pb2+、Cd2+的平衡吸附容量分别为980.39 mg·g-1、813.01 mg·g-1。 吸附/脱附循环实验表明:循环吸附脱附4次后PASP/LNC水凝胶吸附量仍较高,PASP/LNC水凝胶是一种可循环利用的吸附剂。表征结果表明:PASP/LNC水凝胶的表面有大小不等的孔隙,PASP的—COOH与LNC的O—H发生缩聚反应,形成具有三维网络结构的水凝胶。      

A useful approach towards solid–liquid extraction of metal cations with unsupported calixarenes

This article describes a convenient and effective method to study the extraction properties of unsupported calixarenes used as solid extracting agents. The solid–liquid extraction properties of different functionalized calixarene derivatives were studied. This method was compared to classic liquid–liquid extractions. The reproducibility of the solid–liquid extractions was studied among with the calixarene recycling. Results obtained for Cu²⁺, Cd²⁺and Pb²⁺extractions using both methods have revealed the interest to use calixarenes as solid extracting agents. Moreover, a study of selective extraction has been carried out.     

Improved optical photoluminescence by charge compensation in the phosphor system CaMoO4:Eu

It has been found that charge compensated CaMoO₄:Eu³⁺ phosphors show greatly enhanced red emission under 393 and 467 nm-excitation, compared with CaMoO₄:Eu³⁺ without charge compensation. Two approaches to charge compensation, (a) 2Ca²⁺ → Eu³⁺ + M⁺, where M⁺ is a monovalent cation like Li⁺, Na⁺ and K⁺ acting as a charge compensator; (b) 3Ca²⁺ → 2Eu³⁺ + vacancy, are investigated. The influence of sintering temperature and Eu³⁺ concentration on the luminescent property of phosphor samples is also discussed.     

两种不锈钢在单相流和液/固两相流中冲刷与腐蚀的交互作用

用质量损失法研究了65Mn和316L及其Ni-P镀层的冲刷腐蚀行为.结果表明:在试样表面与流体间相对运动距离相同的条件下,65Mn和316L在单相流和两相流中的冲刷腐蚀速率随着介质温度的升高和理论流速的减小而增大.在20%H2sO4单相流和20%H2S04+20 g/L黄砂两相流(50℃,L88 m/s)中,冲刷与腐蚀...     

Laser microwave double-resonance experiment on trapped 113Cd+ ions

The possibility of using Cd⁺ ions as a microwave frequency standard whose light source is an all-solid state UV laser system is presented. The ground-state hyperfine splitting of trapped ¹¹³Cd⁺ ions is measured using an RF trap technique. The transition is detected using a laser microwave double-resonance method in the presence of He buffer gas. The splitting is determined to be 15 199 862 858(2) Hz. The preciseness of the value was improved over that in previous data by seven orders of magnitude. A light source of 214.5 nm is being developed by the authors for optical pumping and laser-cooling of Cd⁺ ions whose fundamental oscillator is based on diode lasers     

Optically active Er–Yb codoped Y2O3 films produced by pulsed laser deposition

Optically active Er³⁺:Yb³⁺ codoped Y₂O₃ films have been produced on c-cut sapphire substrates by pulsed laser deposition from ceramic Er:Yb:Y₂O₃ targets having different rare-earth concentrations. Stoichiometic films with very high rare-earth concentrations (up to 5.5 × 10²¹ at cm^− 3) have been achieved by using a low oxygen pressure (1 Pa) during deposition whereas higher pressures lead to films having excess of oxygen. The crystalline structure of such stoichiometric films was found to worsen the thicker the films are. Their luminescence at 1.53 μm and up-conversion effects have been studied by pumping the Yb³⁺ at 0.974 μm. The highest lifetime value (up to 4.6 ms) is achieved in films having Er concentrations of ≈ 3.5 × 10²⁰ at cm^− 3 and total rare-earth concentration ≈ 1.8 × 10²¹ at cm^− 3. All the stoichiometric films irrespective of their rare-earth concentration or crystalline quality have shown no significant up-conversion.     

Properties of Al heavy-doped ZnO thin films by RF magnetron sputtering

Al-doped ZnO films were deposited by RF magnetron sputtering. From the X-ray diffraction and scanning electron spectrometer studies, wurtzite structure with (0 0 2) orientation ZnO thin films were obtained at Al concentration below 15 atomic percent (at.%). As the Al concentration above 15 at.%, the thin films did not fully crystallize. Two new emission peaks occurred at 351 nm and 313 nm when the Al doping above 15 at.% from the photoluminescence spectrum, and the peaks shift towards the shorter wavelengths with increasing the Al concentration. X-ray photonic spectra of O 1s conformed the amount of oxygen captured by Al³⁺ increasing as the Al³⁺ concentration increasing due to the dominant Al³⁺ possess high charge in competition with Zn²⁺ in the matrix of ZnO.     

Spectroscopic evidence of inhomogeneous distribution of Nd in YVO4, YPO4 and YAsO4 crystals

Nd³⁺ : YVO₄ is one of the most interesting laser hosts for micro and diode-pumped solid state lasers. We have studied magnetic and optical properties of Nd³⁺ in three zircon type crystals YMO₄ (M=V, As, P). In particular, Nd³⁺ ions exhibit in the three hosts a multisite character observed in the absorption and emission spectra. However, the emission and its dynamics are strongly dependant on the reabsorption mechanisms. In Nd : YVO₄, single crystals containing 7 ± 1 × 10¹⁸ Nd³⁺ ions/cm³, the lifetime is 95 ± 2 μs in good agreement with the calculated radiative lifetime. Electron Paramagnetic Resonance (EPR) measurements are performed to identify the nature of the different substitution sites for Nd³⁺ ions. Nd³⁺ ions are found to be inhomogeneously distributed in tetragonal D_2d symmetry sites, in isolated ions, “shallow clusters” and pairs. Proportions of the different local environments depend on the total neodymium concentration. For instance, 15% of the Nd³⁺ ions are gathered in Nd³⁺–Nd³⁺ pairs for 7.2 ± 0.2 × 10¹⁹ Nd³⁺ ions/cm³.     

Frequency upconversion of Tm and Yb codoped YLiF4 synthesized by hydrothermal method

In this paper, YLiF₄ codoped with Tm³⁺ and Yb³⁺ ions was synthesized by hydrothermal method. Yb³⁺ concentration is fixed at 1.5%, and Tm³⁺ concentration is changed from 0.1 to 0.4%. Intense upconversion luminescence is observed when the samples are excited by 980 nm. The dependence of upconversion luminescence on Tm³⁺ concentrations is presented. The results show that upconversion luminescence increases with the Tm⁺ concentration and gets its peak at 0.3 mol%. Under the excitation of 980 nm, the blue emission of 479 nm and the red emission of 647 nm are both duo to two photons process, and the UV emission of 361 nm is attributed to the three photons process. We also analyse the upconversion mechanism and process.     

Cloud point extraction for the determination of copper, nickel and cobalt ions in environmental samples by flame atomic absorption spectrometry

A cloud point extraction procedure was presented for the preconcentration of copper, nickel and cobalt ions in various samples. After complexation with methyl-2-pyridylketone oxime (MPKO) in basic medium, analyte ions are quantitatively extracted to the phase rich in Triton X-114 following centrifugation. 1.0 mol L⁻¹ HNO₃ nitric acid in methanol was added to the surfactant-rich phase prior to its analysis by flame atomic absorption spectrometry (FAAS). The adopted concentrations for MPKO, Triton X-114 and HNO₃, bath temperature, centrifuge rate and time were optimized. Detection limits (3 SDb/m) of 1.6, 2.1 and 1.9 ng mL⁻¹ for Cu²⁺, Co²⁺ and Ni²⁺ along with preconcentration factors of 30 and for these ions and enrichment factor of 65, 58 and 67 for Cu²⁺, Ni²⁺ and Co²⁺, respectively. The high efficiency of cloud point extraction to carry out the determination of analytes in complex matrices was demonstrated. The proposed procedure was applied to the analysis of biological, natural and wastewater, soil and blood samples.     

Static energy transfer for Mn : Pr system in Phosphate glasses

The process of energy transfer from divalent manganese to trivalent praseodymium ions is studied with the help of Forster–Dexter theory. Some of the important energy transfer parameters such as transfer probability (P_SA), quantum yield of energy transfer (μ), critical radius (R₀) and critical concentration of the acceptor (C_A) are evaluated for the energy transfer pairs Mn²⁺ : Pr³⁺, Pr³⁺ : Pr³⁺ in phosphate glasses. The transfer of energy from Mn²⁺ to Pr³⁺ was confirmed by recording the fluorescence decay curves of Mn²⁺ emission corresponding to various activator concentrations which show a non-exponential behaviour. Large values of transfer probabilities and transfer efficiencies suggest that Mn²⁺ ion can act as a good sensitizer to Pr³⁺ ion in phosphate glass.     

Effects of adsorbent dose, its particle size and initial arsenic concentration on the removal of arsenic, iron and manganese from simulated ground water by Fe3+ impregnated activated carbon

This paper presents the observations of the study on arsenic removal from a contaminated ground water (simulated) by adsorption onto Fe³⁺ impregnated granular activated carbon (GAC-Fe). Fe²⁺, Fe³⁺ and Mn²⁺ have also been considered along with arsenic species in the water sample. Similar study has also been done with untreated granular activated carbon (GAC) for comparison. The effects of adsorbent dose, particle size of adsorbent and initial arsenic concentration on the removal of As(T), As(III), As(V), Fe²⁺, Fe³⁺ and Mn²⁺ have been discussed. Under the experimental conditions, the optimum adsorbent doses for GAC-Fe and GAC have been found to be 8 g/l and 24 g/l, respectively with an agitation time of 15 h. Particle size of the adsorbents (both GAC and GAC-Fe) has shown negligible effect on the removal of arsenic and Fe species. However, for Mn removal the effect of adsorbent particle size is comparatively more. Percentage removal of As(T), As(V) and As(III) increase with the decrease in initial arsenic concentration (As₀). However, the increase in percentage removal of all the arsenic species with decrease in As₀ are less for higher value of As₀ (3000–500 ppb) than those of the lower value of As₀ (500–10 ppb). The % removal of As(T), As(III), As(V), Fe, and Mn were 95%, 92.4%, 97.6%, 99% and 41.2%, respectively when 8 g/l GAC-Fe was used at the As₀ value of 200 ppb. However, for GAC these values were 55.5%, 44%, 71%, 98% and 97%. The pH and temperature of the study were 7 ± 0.1 and 30 ± 1 °C, respectively.     

NF/PDMA/MnO2-Co电容电极对低浓度Pb2+的电吸附特性

在泡沫镍基体上进行阳极电沉积制备了NF/PDMA/MnO₂-Co电极,使用FESEM-EDS、XPS和Raman谱、循环伏安和电容吸脱附测试等手段表征了复合电极的结构和评价其电容特性和对Pb²⁺的吸附行为。结果表明,在电流密度为1 mA/cm²、30℃和3 min条件下制备的NF/PDMA/MnO₂-Co复合电极,在Pb²⁺浓度为20 mg/L的模拟废水中有比较高的比电容值(208.8 F/g),对Pb²⁺有较高的吸附容量(59.9 mg/g);PDMA底层与Co掺杂MnO₂表层的协同作用提高了MnO₂电极电容和吸附性能;吸附动力学拟合表明,复合电极的吸附过程受物理、化学吸附混合控制,并受离子传质和孔隙内扩散的限制;电极的稳定性好,4次循环吸附后的吸附量仍达到51.7 mg/g。     

凹凸棒土负载CeO2-La2O3复合材料制备表征及催化性能

以凹凸棒土(ATP)为载体, 以Ce(NO₃)₃·6H₂O和La(NO₃)₃·6H₂O为原料, 以C₆H₁₂N₄(HMT)为沉淀剂, 采用均相沉淀法制备了不同铈镧比的CeO₂-La₂O₃/ATP(Ce:La=9:1~3:7, 摩尔比, 下同)复合材料。用TG-DSC、 TEM、 XRD和FTIR对所制备复合材料的微观结构和形貌进行表征, 并分别考察不同铈镧比和H₂O₂添加量对酸性品红模拟废水脱色降解的影响。结果表明, 当Ce:La=5:5时, CeO₂-La₂O₃固溶体颗粒均匀分布在ATP表面, 颗粒尺寸为5~10 nm。随着铈镧摩尔比的增加, 酸性品红的降解率呈先增后减的趋势, 且当Ce:La=5:5、 H₂O₂为10 mL、 酸性品红浓度为100 mg/L时, 降解效果最好, 300 min后的最大降解率达82%。