Preconcentration of copper with multi-walled carbon nanotubes pretreated by potassium permanganate cartridge for solid phase extraction prior to flame atomic absorption spectrometry

A procedure for the preconcentration of copper was described in this paper using multi-walled carbon nanotubes (MWCNTs) oxidized by potassium permanganate as the adsorbent for the enrichment of trace copper in water samples. Important parameters, such as the sample pH, the concentration and volume of eluent, sample flow rate and volume, and interference of coexisting ions, were investigated. The obtained results indicated that proposed method possessed an excellent analytical performance. The linear range, the detection limit, and precison (RSD) were 1–100 ng/mL (R(2) = 0.9993), 0.32 ng/mL and 2.88%, respectively. The results showed that copper could be adsorbed quantitatively on the pretreated MWCNTs with potassium permanganate, and proposed method was very useful in the monitoring of copper in the environment.

Atomic origins of solid helium bubbles in tungsten

Solid helium bubbles were directly observed in the helium ion implanted tungsten（W）, by different transmission electron microscopy（TEM） techniques at room temperature. The diameters of these solid helium bubbles range from1 nm to 8 nm in diameter with the mean bubble size about 3 nm. The selected area electron diffraction（SAED） and fast Fourier transform（FFT） images revealed that solid helium bubbles possess body-centered cubic（bcc） structure with a lattice constant of 0.447 nm. High-angle annular dark-field scanning transmission electron microscopy（HAADF-STEM）images further confirmed the existence of helium bubble in tungsten. The present findings provide an atomic level view of the microstructure evolution of helium in the materials, and revealed the existence of solid helium bubbles in materials.

Analysis of trace mercury in water by solid phase extraction using dithizone modified nanometer titanium dioxide and cold vapor atomic absorption spectrometry

A new method for analysis of trace mercury in water samples was developed, based on the combination of preconcentration/separation using dithizone-modified nanometer titanium dioxide （TiO2） as a solid phase extractant and determination by cold vapor atomic adsorption spectrometry （CVAAS）. Dithizone was dissolved with alcohol and loaded on the surface of nano-sized TiO2 powders by stirring. The static adsorption behavior of Hg^2＋on the dithizone-modified nanoparficles was investigated in detail. It was found that excellent adsorption ratio for Hg^2＋ could be obtained in the pH range of 7-8 with an oscillation time of 15 rain, and a 5 mL of 3.5 mol·L^-1 HCI solution could quantitatively elute Hg^2＋ from nanometer TiO2 powder. Common coexisting ions caused no obvious influence on the determination of mercury. The mechanisms for the adsorption and desorption were discussed. The detection limit （30） for Hg^2＋ was calculated to be 5 ng·L^-1. The proposed method was applied to the determination of Hg^2＋ in a mineral water sample and a Zhujiang River water sample. By the standard addition method, the average recoveries were found to be 94.4%-108.3% with RSD （n = 5） of 2.9%-3.5%.

Qualitative Analysis of Relationship between Refractive Index and Atomic Parameters of Solid Materials

The refractive index is one of the important parameters describing the optical properties of solid materials. However, it is difficult to obtain a quantitative relation between the refractive index and the structure and composition of materials. A qualitative relation between the refractive index and some atomic parameters of materials was proposed and demonstrated by some oxide optical crystals. A parameter P=r~-/F=r~-/(r~+ΔxD) is defined, in which Δx is the difference of the electronegativities between cations and anions in the materials and r~+ and r~- are the radii of cations and anions respectively. On the other hand, the factor D was introduced to describe the effect of mass difference of the ions. It is demonstrated by both theoretical discussion and experimental data that refractive index is a decreasing function of parameter P. The relation may be useful for the investigation of optical materials.

Preconcentration of Lead in Sugar Samples by Solid Phase Extraction and Its Determination by Flame Atomic Absorption Spectrometry

A simple and sensitive solid phase extraction utilizing C18 filled cartridges incorporated with dithizone for preconcentration of lead and its subsequent determination by flame atomic absorption spectrometry (FAAS) was developed. Several parameters such as type, concentration and volume of eluent, pH of the sample solution, flow rate of extraction and volume of the sample were evaluated. The effect of a variety of ions on preconcentration and recovery was also investigated. At pH = 7.4 and 1.0 mol?L–1 HCl eluting them, lead ions were recovered quantitatively. The limit of detection (LOD) defined as 3Sbl was determined to be 8.1 μg L–1 for 500 mL of sample solution and eluted with 5 mL of 1.0 mol?L–1 HCl under optimum conditions. The accuracy and precision (RSD %) of the method were >90% and <10%, respectively. In the end, the proposed method was applied to a number of real sugar samples and the amount of lead was determined by spiking a known concentration of lead into the solution.

Zn和Cu对纯镁的微观组织与导电性能的影响研究

本文研究了Zn和Cu元素的添加对纯Mg微观组织和导电性能的影响。结果表明,Zn和Cu能明显细化纯Mg的铸态组织,且元素添加量越多,晶粒尺寸越细小。铸态Mg-Zn和Mg-Cu合金的导电率均随着元素添加量的增加而不断降低。Mg-Zn合金中,固溶在基体中的溶质原子是影响导电率的主要因素;Mg-Cu合金中,第二相是影响导电率的主要因素。当元素添加量相同时,Zn对导电率的降低作用比Cu要更加显著。分别选取Mg-2.5%Zn合金和Mg-4%Cu合金在不同挤压温度下(200℃、300℃、400℃)进行挤压变形。Mg-2.5%Zn合金随着挤压温度提高,晶粒尺寸增大,第二相数量减少,导电率先降低再升高,但均低于其铸态合金的导电率。Mg-4%Cu合金随着挤压温度提高,晶粒尺寸增大,第二相数量无明显变化,导电率不断升高,均高于其铸态合金的导电率。

探索微纳尺度润湿动力学:长针式原子力显微镜的应用与进展

“如何在微观层面测量界面现象”是微纳尺度实验流体力学的关键科学问题,被列入世界前沿125个科学问题名单(Sanders S,Science,2021).由于光学衍射极限的限制,传统光学手段很难直接测量微纳尺度下的流动与界面现象.利用原子力显微镜的精准操控和小尺度力学测量等优势,结合长针式探针组装成的微流变计可以直接测量气-液-固三相接触线上的毛细力,并监测探针在垂直方向运动中力的动态变化.通过该技术手段,可以实现对流体界面的动力学行为以及各类材料在液体环境中力学性质在微纳尺度的精确表征.文章将系统介绍长针式原子力显微镜技术的实验原理和方法,及其在微纳尺度非理想界面润湿动力学中的最新研究进展,包括低能垒表面毛细力的速度依赖性与非对称性、无序粗糙表面接触线黏滑运动的统计学规律、柔性表面接触线动力学的状态与速度定律、以及离子液体-金属界面处电场对接触角迟滞的调控等,最后展望了该技术在新兴领域中的应用.该实验手段为检验各类理论模型与数值模拟提供了可信数据,为探究界面上复杂现象的物理本质提供参考.

原子荧光光度法测定固体废物中砷的方法验证

为对我国环境保护与控制提供技术支持,进一步完善固体废物中重点参数,本文对HJ 702—2014《固体废物砷、汞、硒、铋、锑的测定微波消解/原子荧光法》中砷的测定进行6个方面的验证:线性关系、方法检出限、测定下限、精密度、准确度和实际样品加标回收率。结果表明,线性关系达到0.9998;当称取0.5 g固体废物样品验证砷(全量)时,测得0.009μg/g检出限、0.036μg/g的测定下限,当移取40 m L固体废物浸出液验证砷(浸出液)时,测得0.08μg/L的检出限、0.32μg/L的测定下限;砷(全量)、砷(浸出液)的相对标准偏差分别为0.35%~1.0%、1.2%~2.9%;实验室砷(全量)有证标准物质相对误差分别为-4.6%~0.85%,砷(浸出液)标准浓度的相对误差分别为0.25%~3.0%;固体废物砷(全量)加标回收率分别为93.7%~97.5%,固体废物砷(浸出液)加标回收率分别为96.0%~98.1%。各项指标均满足标准方法要求,证实实验室具备原子荧光光度法测定固体废物中砷的试验条件和技术能力。

无机-有机复合材料沸石@聚丙烯酰胺的制备及对Pb^(2+)的吸附研究

重金属污染会引起严峻的环境问题。因此,必须对重金属离子进行测定,但由于重金属离子的含量低并受基体效应影响,检测前需要先将其分离富集。利用一锅法制备沸石@聚丙烯酰胺复合材料,将其作为分离富集材料,结合火焰原子吸收光谱仪,研究对Pb^(2+)的吸附性能。为了得到最佳的吸附性能,对制备条件中的沸石用量进行了优化,并对优化后的复合材料进行了扫描电镜、热重分析和比表面积表征。利用单一变量法,对固相萃取条件中的溶液pH值和振荡时间进行了优化。研究了复合材料在吸附Pb^(2+)过程中的动力学模型、等温线模型和热力学参数。结果表明:在沸石用量为333 mg/g,溶液pH值为5和振荡时间为80 min时,复合材料的吸附效率最佳;沸石@聚丙烯酰胺复合材料吸附Pb^(2+)的过程符合二级动力学和Freundlich模型,且在298.15 K时,热力学参数ΔH=15614.18 J/mol、ΔS=65.2 J/(mol·K)、ΔG=-1878.059 J/mol,是一个吸热且熵增的自发过程;此外,复合材料经过连续三次吸附和解吸实验,对Pb^(2+)的吸附量基本不变,且解吸率保持在89.7%以上,说明沸石@聚丙烯酰胺复合材料具有较好的再生性能。

原子荧光光度法测定固体废弃物中总锡量的研究

建立以氢氟酸—盐酸—硝酸为消解体系,运用原子荧光光度计测定固体废弃物中总锡质量分数的分析方法。比较不同酸介质、还原剂及掩蔽剂的试验效果,得出最佳的工作条件下,该方法锡元素校准曲线的相关系数稳定在0.9998,检出限为0.06 mg/kg。对GSS-4a平行测定8次计算得RSD=3.58%;选取从低到高4种不同锡质量分数的标准样品测得结果的相对误差为-3.85%~4.11%;在8、4和2μg/L 3种加标量下,方法的加标回收率在93.7%~107.0%之间。该方法检出限低、稳定性高、操作性强,可满足实验室检测固体废弃物中总锡的质量分数,提高检测效率,适用于日常大批量分析样品的要求。

bcc结构下二元合金Fe-X(X=Cr,Co,Mo,W)低温低浓度下固溶软化行为的机制

采用第一性原理计算研究了体心立方(bcc)Fe的4种二元合金Fe-X(X=Cr,Co,Mo,W)低温低浓度下固溶软化行为的机制,发现低温低浓度下的固溶软化行为由双扭结形核控制,由溶质原子直接引起双扭结形核势垒降低为固溶软化的本征机制,而由溶质原子对间隙原子清除减少双扭结形核为固溶软化的外部机制.分别计算了bcc Fe的4种二元合金Fe-X(X=Cr,Co,Mo,W)中反映双扭结形核势垒的原子行位移(ARD)能和堆垛层错(GSF)能.计算结果表明,仅Cr可微弱降低ARD和GSF能,而Co,Mo,W均引起ARD和GSF能升高,因此,依据固溶软化的本征机制,仅Cr引起固溶软化,而Co,Mo,W均引起固溶强化.Cr,Mo,W与周围Fe原子均为反铁磁相互作用,Co与Fe为铁磁相互作用.尽管铁磁/反铁磁相互作用与价电子数(电子构型)具有一定相关性,双扭结形核势垒并不与价电子数(电子构型)明显相关.进一步的计算表明,双扭结形核势垒与其结合能呈现正相关关系,Cr与Fe结合能减弱,因此双扭结形核势垒降低,而Co,Mo,W与Fe结合能增强,因此双扭结形核势垒升高.而结合能并未表现出与原子半径、电子数(电子构型)的明显相关性,因此,双扭结形核势垒并不与原子半径、电子数(电子构型)明显相关.依据本征机制,Co,Mo,W与Fe的结合能增强引起双扭结形核势垒升高,因此为固溶强化,其二元合金低温低浓度下的固溶软化行为无法用本征机制解释,需要考虑外部机制(如间隙C原子的作用),而Cr二元合金的固溶软化行为可能为本征机制.

Determination of Trace Amounts of Zinc, Iron and Copper by Flame Atomic Absorption after Their Preconcentration Using Sodium Dodecyl Sulfate (SDS) Coated Alumina Nanoparticles Modified with 3-Mercapto-D-Valin from Environmental Samples

A sensitive and simple solid phase extraction method for the simultaneous determination of trace and toxic metals in environmental samples has been reported. The method is based on the adsorption of Zinc, Iron and Copper on SDS-coated alumina nanoparticles, which is also modified with 3-mercapto-D-valine. The retained analyte ions on modified solid phase were eluted using 5 mL of 4 mol·L﹣1 HNO3. The analyte determination was carried out by flame atomic absorption spectrometry. The influences of some metal ion and anions on the recoveries of understudy analyte ion were investigated. The influences of the analytical parameters including pH, ligand and SDS amount, eluting solution (type and concentrations) and sample volume on metal ions recoveries were investigated. The extraction efficiency was > 98% with relative standard deviation lower than 3% the method has been successfully applied for the extraction and determination of these ions content in some real samples. Prepared adsorbent was characterized by SEM and FT-IR measurements.

四种稻米中镉检测方法比较研究

采用石墨炉原子吸收法、固体直接进样电热蒸发原子吸收光谱法、电化学阳极溶出伏安法和X射线荧光光谱法测定稻米中镉含量,对4种定量检测方法的准确度、精密度以及相对误差进行了比较分析。研究结果表明,固体直接进样电热蒸发原子吸收光谱法操作简单,无需化学前处理,单样检测时间在3 min左右,快速高效,精密度良好,可信度高。通过4种检测方法对比,固体直接进样电热蒸发原子吸收光谱法的测试结果准确度高,与国家标准方法相比相对误差多数在±10%以内,重复6次测定的RSD为3.9%,可作为一种新型快速检测稻米中镉的方法,具备方便快速、准确度高、重复性好等优点,在基层可广泛应用。

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes （MWCNTs） and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry. The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing. Parameters influencing the recoveries of target analytes were optimized. Under optimal conditions, the target analyte exhibited a good linearity （R^2=0.9992） over the concentration range 0.5-50 ng/ml. The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively. The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%. All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.

The effect of nozzle layout on droplet ejection of a piezo-electrically actuated micro-atomizer

We study here effects of nozzle layout on the droplet ejection of a micro atomizer, which was fabricated with the arrayed nozzles by the MEMS technology and actuated by a piezoelectric disc. A theoretical model was first built for this piezoelectric-liquid-structure coupling system to characterize the acoustic wave propagation in the liquid chamber, which determined the droplet formation out of nozzles. The modal analysis was carried out numerically to predict resonant frequencies and simulate the corresponding pressure wave field. By comparing the amplitude contours of pressure wave on the liquid-solid interface at nozzle inlets with the designed nozzle layout, behaviors of the device under different vibration modes can be predicted. Experimentally, an impedance analyzer was used to measure the resonant frequencies of the system. Three types of atomizers with different nozzle layouts were fabricated for measuring the effect of nozzle distribution on the ejection performance. The visualization experiment of droplet generation was carried out and volume flow rates of these devices were measured. The good agreement between the experiment and the prediction proved that only the increase of nozzles may not enhance the droplet generation and a design of nozzle distribution from a view-point of frequency is necessary for a resonant related atomizer.

A Perspective of Laser Sampling for Inductively Coupled Plasma-Atomic Emission Spectro metry for Rock and Mineral Analysis

The development of laser sampling for optical emission spectrometry is reviewed . Advantages and limitations of pulsed laser sampling are compared with those of continuous laser sampling . A novel method of laser sampling of liquid samples for inductively coupled plasma -atomic emission spectrometry has been proposed , and its analytical performance investigated.Experimental results showed that,as a method of sample introduction , laser vaporization of liquid samples enjoyed certain advantages , e.g.,much higher sensitivity, much lower detection limit and reduced sample volume , over solution nebulization . A perspective of the application of laser sampling-inductively coupled plasma - actomic emission spectrometry for rock and mineral analysis is estimated as well.

Quantum Phase Transition of the Bosonic Atoms near the Feshbach Resonance in an Optical Lattice

The quantum phase transition from the Mott insulator to the superfluid phases of the bosonic atoms trapped in an optical lattice, in which the on-site interaction carl be tuned by a Feshbach resonance, is investigated by a variational approach within mean-field theory. We derive an extended Bos^Hubbard model to describe this ultracold atomic system. By theoretical calculation and analysis, the phase diagram is shown clearly, and we find an exciting and novel phenomenon that is the appearance of the Mort insulator-sea （MI-sea）. Meanwhile, the experimental feasibility of observing the MI-sea is discussed by analyzing the published data related to the Fashbaeh resonance at present. Finally, the potential application of the MI-sea for quantum information processing and quantum computation is also discussed in detail

Comparison between methods for predicting maximum solid solubility of transition metals in solvent metal

It is important to know the maximum solid solubility( C max ) of various transition metals in a metal when one designs multi component alloys. There have been several semi empirical approaches to qualitatively predict the C max , such as Darken Gurry(D G) theorem, Miedema Chelikowsky(M C) theorem, electron concentration rule and the bond parameter rule. However, they are not particularly valid for the prediction of C max . It was developed on the basis of energetics of alloys as a new method to predict C max of different transition metals in metal Ti, which can be described as a semi empirical equation using the atomic parameters, i e, electronegativity difference, atomic diameter and electron concentration. It shows that the present method can be used to explain and deduce D G theorem, M C theorem and electron concentration rule.

Maximum solid solubility of transition metals in vanadium solvent

Maximum solid solubility (C_ max) of different transition metals in metal solvent can be described by a semi-empirical equation using function Z_f that contains electronegativity difference, atomic diameter and electron concentration. The relation between C_ max and these parameters of transition metals in vanadium solvent was studied. It is shown that the relation of C_ max and function Z_f can be expressed as lnC_ max=Z_f= 7.3165- 2.7805(ΔX) 2- 71.278δ 2-0.85556n 2/3. The factor of atomic size parameter has the largest effect on the C_ max of the V binary alloy; followed by the factor of electronegativity difference; the electrons concentration has the smallest effect among the three bond parameters. Function Z_f is used for predicting the unknown C_ max of the transition metals in vanadium solvent. The results are compared with Darken-Gurry theorem, which can be deduced by the obtained function Z_f in this work.