Determination of Trace Amounts of Lead by Modified Graphite Furnace Atomic Absorption Spectrometry after Liquid Phase Microextraction with Pyrimidine-2-thiol

The liquid phase microextraction (LPME) was combined with the modified Graphite furnace atomic absorption spectrometry (GF-AAS) for determination of lead in the water and solid samples. In a preconcentration step, lead was extracted from a 2 ml of its aqueous sample in the pH = 5 as lead-Pyrimidine-2-thiol cationic complex into a 4 μl drop of 1,2 dichloroethane and ammonium tetraphenylborate as counter ion immersed in the solution. In the drop, the lead-Pyrimidine-2-thiol ammonium tetraphenylborate ion associated complex was formed. After extraction, the microdrop was retracted and directly transferred into a graphite tube modified by [W.Pd.Mg] (c). Some effective parameters on extraction and complex formation, such as type and volume of organic solvent, pH, concentration of chelating agent and counter ion, extraction time, stirring rate and effect of salt were optimized. Under the optimum conditions, the enrichment factor and recovery were 525% and 94%, respectively. The calibration graph was linear in the range of 0.01 - 12 μg?L–1 with correlation coefficient of 0.9975 under the optimum conditions of the recommended procedure. The detection limit based on the 3Sb criterion was 0.0072 μg?L–1 and relative standard deviation (RSD) for ten replicate measurement of 0.1 μg?L–1 and 0.4 μg?L–1 lead was 4.5% and 3.8% respectively. The characteristic concentration was 0.0065 μg?L–1 equivalent to a characteristic mass of 26 fg. The results for determination of lead in reference materials, spiked tap water and seawater demonstrated the accuracy, recovery and applicability of the presented method.

Microstructure,crystalline phase and electrical properties of Li_(0.06)(Na_(0.5)K_(0.5))_(0.94)Nb_(1-2x/5)Mg_xO_3 lead-free piezoelectric ceramics

MgO-modified Li0.06（Na0.5K0.5）0.94NbO3O3 （L6NKN） lead-free piezoelectric ceramics were synthesized by normal sintering at a rela- tively low temperature of 1000℃. The crystalline phase, microstructure, and electrical properties of the ceramics were investigated with a special emphasis on the influence of MgO content. The addition of MgO effectively improves the sintembility of the L6NKN ceramics. X-my diffr cfion analysis indicates that the morphotropic phase boundary （MPB） separating orthorhombic and tetragonal phases for the ceramics lies in the range of Mg doping content （x） from 0.3at% to 0.7at%. High electrical properties of the piezoelectric constant （d33=238 pC/N）, planar electromechanical coupling coefficient （kp=41.5%）, relative dielectric constant （εr=905）, and remanent polarization （Pr=38.3 μC/cm2） are obtained from the specimen with x=0.5at%, which suggests that the Li0.06（Na0.5K0.5）0.94Nb（1-2x/5）MgxO3 （x=0.5at%） ceramic is a promising lead-free piezoelectric material.

Modified phase transition and electrical properties of [Li_(0.05)(Na_(0.535)K_(0.48))_(0.95)]- (Nb_(0.94)Sb_(0.06))O_3 lead-free piezoelectric ceramic by sintering temperature

Li/Sb-doped (Na,K)NbO3 with a nominal composition of [Li0.05(Na0.535K0.48)0.95](Nb0.94Sb0.06)O3 ceramic was synthesized by normal sintering. The phase structure, microstructure, and electrical properties were investigated with a special emphasis on the influence of the sintering temperature. A polymorphic phase transition (PPT) from orthorhombic to tetragonal symmetry was observed when the sintering temperature was raised from 1040 to 1050 ℃, whereby the piezoelectric coefficient d33 and the electromechanical coupling coefficient kp reached the peak values of 245 pC·N-1 and 41.2%, respectively. The PPT induced by varying the sintering temperature is due to the different volatilization extents of alkali metals and appears to a lower sintering temperature with increasing Li content. The trace modifying of alkali metal content is more effective than doping B site element to enhance the d33 value.

THERMODYNAMIC EXPLANATION OF LEADING PHASE IN PEARLITE TRANSFORMATION

In this paper a concept of 'leading probability' is presented. The difference in the leading probability between ferrite and cementite depends mainly upon the difference between their driving forces at the beginning of precipitation. The results of theromdynamic calculations showed that the leading probability of cementite increased with the increase of carbon concentration of austenite, and the decrease in transformation temperature was favourable to cementite's being the leading nucleus during pearlite transformation.

Large phase shift of spatial soliton in lead glass by cross-phase modulation in pump-signal geometry

We investigate the co-propagation of a strong pump beam and a weak signal beam in lead glass, and find that the large phase shift of the strongly nonlocal spatial optical soliton （SNSOS） can be realized via cross-phase modulation. The theoretical study suggests a synchronous propagation of the pump SNSOS and the signal SNSOS under the required initial condition. A π-phase shift of the signal SNSOS is experimentally obtained by changing the power of the pump SNSOS by about 13 mW around the soliton critical power, which agrees qualitatively with our theoretical prediction. The ratio of the phase shift rate of the signal SNSOS to that of the pump SNSOS shows a close match to the reciprocal of the ratio between their wavelengths.

Fractional-order L_βC_a filter circuit network

In this paper we introduce the new fundamentals of the conventional LC filter circuit network in the fractional domain.First, we derive the general formulae of the impedances for the conventional and fractional-order filter circuit network.Based on this, the impedance characteristics and phase characteristics with respect to the system variables of the filter circuit network are studied in detail, which shows the greater flexibility of the fractional-order filter circuit network in design.Moreover, from the point of view of the filtering property, we systematically study the effects of the filter units and fractional orders on the amplitude–frequency characteristics and phase–frequency characteristics. In addition, numerical tables of the cut-off frequency are presented. Finally, two typical examples are presented to promote the industrial applications of the fractional-order filter circuit network. Numerical simulations are presented to verify the theoretical results introduced in this paper.

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.

Effects of Na/K ratio on the phase structure and electrical properties of Na_xK_(1-x)NbO_3 lead-free piezoelectric ceramics

Lead-free piezoelectric NaxK1-xNbO3（x = 0.3-0.8）（NKN） ceramics were fabricated by normal sintering at 1060°C for 2 h.Microstructures and electrical properties of the ceramics were investigated with a special emphasis on the influence of Na content.The grain size of the produced dense ceramic was decreased by increasing Na content.A discontinuous change in the space distance was found at the composition close to Na0.7K0.3NbO3 ceramic, which indicates the presence of a transitional composition between two different orthorhombic phases, which is similar to the behavior of morphotropic phase boundary（MPB） in NaxK1-xNbO3 ceramics.Such MPB-like behavior contributes to the enhanced piezoelectric coefficient d33 of 122 pC/N, planar-mode electromechanical coupling coefficient kP of 28.6%, and dielectric constant εr of 703, respectively for the Na0.7K0.3NbO3 ceramic.Cubic temperature TC and the transitional temperature TO-T from orthorhombic to tetragonal phase are observed at around 420°C and 200°C, respectively.

The Implementation and Lateral Control Optimization of a UAV Based on Phase Lead Compensator and Signal Constraint Controller

Unmanned Aero Vehicles (UAV) has become a useful entity for quite a good number of industries and facilities. It is an agile, cost effective and reliable solution for communication, defense, security, delivery, surveillance and surveying etc. However, their reliability is dependent on the resilient and stabilizes performance based on control systems embedded behind the body. Therefore, the UAV is majorly dependent upon controller design and the requirement of particular performance parameters. Nevertheless, in modern technologies there is always a room for improvement. In the similar manner a UAV lateral control system was implemented and researched in this study, which has been optimized using Proportional, Integral and Derivative (PID) controller, phase lead compensator and signal constraint controller. The significance of this study is the optimization of the existing UAV controller plant for improving lateral performance and stability. With this UAV community will benefit from designing robust controls using the optimized method utilized in this paper and moreover this will provide sophisticated control to operate in unpredictable environments. It is observed that results obtained for optimized lateral control dynamics using phase lead compensator (PLC) are efficacious than the simple PID feedback gains. However, for optimizing unwanted signals of lateral velocity, yaw rate, and yaw angle modes, PLC were integrated with PID to achieve dynamical stability.

Observations and modelling of the travel time delay and leading negative phase of the 16 September 2015 Illapel,Chile tsunami

The systematic discrepancies in both tsunami arrival time and leading negative phase(LNP)were identified for the recent transoceanic tsunami on 16 September 2015 in Illapel,Chile by examining the wave characteristics from the tsunami records at 21 Deep-ocean Assessment and Reporting of Tsunami(DART)sites and 29 coastal tide gauge stations.The results revealed systematic travel time delay of as much as 22 min(approximately 1.7%of the total travel time)relative to the simulated long waves from the 2015 Chilean tsunami.The delay discrepancy was found to increase with travel time.It was difficult to identify the LNP from the near-shore observation system due to the strong background noise,but the initial negative phase feature became more obvious as the tsunami propagated away from the source area in the deep ocean.We determined that the LNP for the Chilean tsunami had an average duration of 33 min,which was close to the dominant period of the tsunami source.Most of the amplitude ratios to the first elevation phase were approximately 40%,with the largest equivalent to the first positive phase amplitude.We performed numerical analyses by applying the corrected long wave model,which accounted for the effects of seawater density stratification due to compressibility,self-attraction and loading(SAL)of the earth,and wave dispersion compared with observed tsunami waveforms.We attempted to accurately calculate the arrival time and LNP,and to understand how much of a role the physical mechanism played in the discrepancies for the moderate transoceanic tsunami event.The mainly focus of the study is to quantitatively evaluate the contribution of each secondary physical effect to the systematic discrepancies using the corrected shallow water model.Taking all of these effects into consideration,our results demonstrated good agreement between the observed and simulated waveforms.We can conclude that the corrected shallow water model can reduce the tsunami propagation speed and reproduce the LNP,which is observed for tsunamis that have propagated over long distances frequently.The travel time delay between the observed and corrected simulated waveforms is reduced to<8 min and the amplitude discrepancy between them was also markedly diminished.The incorporated effects amounted to approximately 78%of the travel time delay correction,with seawater density stratification,SAL,and Boussinesq dispersion contributing approximately 39%,21%,and 18%,respectively.The simulated results showed that the elastic loading and Boussinesq dispersion not only affected travel time but also changed the simulated waveforms for this event.In contrast,the seawater stratification only reduced the tsunami speed,whereas the earth’s elasticity loading was responsible for LNP due to the depression of the seafloor surrounding additional tsunami loading at far-field stations.This study revealed that the traditional shallow water model has inherent defects in estimating tsunami arrival,and the leading negative phase of a tsunami is a typical recognizable feature of a moderately strong transoceanic tsunami.These results also support previous theory and can help to explain the observed discrepancies.

Identification of Rare Earth Phase in the Deformed High Lead-Brasses

Deformed high lead-brasses have excellent machining characteristics and good mechanical and physicalproperties.They are widely used in mechanical,clock-watch and pen-making field.Especially,they are suit-able for deep-hole machining.Because of their worse hot-working characteristics,there exists trouble inproduction process.It is reported that the rare earth metals could improve the hot-rolling property,but themechanism is still unclear.

基于石墨烯/硫化铅量子点异质结的窄带光电探测器

纳米材料硫化铅量子点(PbS QD)以其高光吸收率和尺寸可调的带隙,被视为短波红外(SWIR)光电探测器的重要候选材料。将卤素配体置换的PbS QD薄膜与单层石墨烯结合制备了石墨烯/硫化铅量子点异质结光电探测器。采用液相配体交换技术结合单步旋涂工艺,实现了PbS QD薄膜的均匀沉积。该技术不仅减少了缺陷态的产生,而且通过单步旋涂工艺能够实现所需薄膜厚度的快速沉积,简化了器件制备流程,满足工业化生产要求。测试了器件在SWIR波段的性能,结果显示该光电探测器在1550 nm处响应度为1.26×10^(4)A/W,显著高于其他波段,证实器件在1550 nm波段附近具有窄带探测的能力。此外,在1550 nm处比探测率高达1.49×10^(12)Jones。该结果表明器件在SWIR波段具备高探测灵敏度和实际应用的潜力。

Novel thermal expansion of lead titanate

Lattice parameters of lead titanate were precisely re-determined in thetemperature range of-150-950 deg C by high precision XRPD measurements. It was clarified that therewas no any evidence for a new phase transition at low tempera-lures. Tetragonal distortion straindecreases with temperature increasing. A novel thermal expansion was observed, positive thermalexpansion from -150 deg C to room temperature (RT) and above 490 deg C, and the negative thermalexpansion in the temperature range of RT-490 deg C. A big jump of thermal expansion coefficient isattributed to the tetragonal-cubic phase transition. A rationalization for the negative thermalexpansion of PbTiO_3 is due to the decrease of anion-anion repulsion as polyhedra become moreregular at heating. The mechanisms of positive and negative thermal expansions were elucidated asthe same nature in the homogenous tetragonal phase at present case.

Effect of CaO/SiO_2 and Fe/SiO_2 ratios on phase equilibria in PbO-ZnO-CaO-SiO_2-“Fe_2O_3” system in air

Experimental studies on phase equilibria and liquidus temperature in the PbO-ZnO-CaO-SiO2-＂Fe2O3＂ system,with the mass ratios of CaO/SiO2=1-1.6 and Fe/SiO2= 1.3-1.7,and 40% PbO and 8% ZnO,were carried out between 1273 and 1573 K.Slags were equilibrated at 1273 to 1573 K and cooled rapidly by quenching.The XRD and SEM-EDS results showed that the slag compositions are in the franklinite primary phase field.Calcium and lead silicates are formed between 1373 and 1473 K.The Ca/Pb silicate and magnetoplumbite phases are partially formed by an incongruent reaction.The experimental and thermodynamical results showed that the liquidus increased by increasing CaO/SiO2 mass ratio and decreasing Fe/SiO2 mass ratio.

Order of sphalerite and galena precipitation: A case study from lead-zinc deposits in southwest China

Most of the lead and zinc deposits in Southwest China, are characterized by mineral zoning, which is especially true for the Huize and Zhaotong deposits. The mineral assemblage zoning is consistent for both horizontal and vertical zoning, from the base(center) of the ore body to the top(outermost), the mineral zones are as follows. I-1: coarse-grained pyrite and a little puce sphalerite;I-2: brown sphalerite, galena, and ferro-dolomite;I-3: galena, sandy beige and pale yellow sphalerite, and calcite;and I-4: fine-grained pyrite, dolomite, and calcite. Among them, sphalerite is the landmark mineral of different zoning. From I-1 to I-3, the color of sphalerite changes from dark to light, its crystalline size changes from coarse to fine, and its structure changes from disseminated to veinlet. This mineral zoning is seen not only on a microscopic scale, but is also clear on a mesoscopic and macroscopic scale. It is caused by the order of the sphalerite and galena precipitation. We studied the metallic minerals and fluid inclusions using a thermodynamic phase diagram method, such as lgfO2–lgfS2, pH–lgfO2, pH–lg[Pb^2+] and pH–lg[HS^-], discussed the constraints on the order of the sphalerite and galena precipitation in the migration and precipitation process of lead and zinc under different pH values, oxygen fugacity, sulfur fugacity, and ionic activity. We also explain the formation mechanism and propose that the main controlling factor of the order of the sphalerite and galena precipitation is sulfur fugacity.

Lead Iodide Crystals as Input Material for Radiation Detectors

Lead iodide is an important inorganic solid for fundamental research and possible technological applications and is considered to be a potential room temperature nuclear radiation detector. In lead iodide the phenomenon of polytypism is posing an interesting problem of phase transformations amongst its various polytypic modifications. The transformations have also been observed even when the crystals are stored for few months. It causes deterioration in functioning of PbI2 devices. Taking into account the known structures of PbI2 and the data available on the mode of growth and storage of crystals, it has been concluded that purified melt grown crystals of PbI2 are the best suited for nuclear radiation detectors.

Effect of Pb Addition on Melting Behavior ofBi-Sr-CuO System 2201 Phase

The effect of Pb on the melting of the 2201 phase was studied by DTA and XRD. The results indicate that as the mole ratio of Pb/(Pb+Bi) is up to 20%, the tetragonal 2201 phase will transform into the orthorhombic 2201 and that the melting point Tm of the tetragonal 2201 decreases with increasing Pb-content, however, Tm of the orthorhombic 2201 remains 883°C.

Effect of Pb Content on Phase Composition and Property of Bi-Pb-Sr-Ca-Cu-O System Superconductors

The addition of Pb in the superconductors of BiSrCaCuO system is very helpful for growth of the high-Tc phase (Tc 110K). We prepared a series of samples with nominal composition of Bi2-xPbxSr2Ca2Cu3Oy (0.1&lex&le2). The zero resistance transition temperature Tc of 106K and the critical transport current density Jc of 1 × 103A/cm2 at 77K have been obtained for the samples of Bi2-xPbxSr2Ca2Cu3Oy (x=0.2 and 0.3). The X-ray diffraction analysis and measurement of AC magnetic susceptibility confirmed that the material is comprised of single high-Tc phase. We also report the magnetic properties of this material as well as the results of TEM observation.

Effectively Inhibit Phase Separation to Improve Efficiency and Stability of All-Inorganic Planar CsPbIBr2 Perovskite Solar Cells

The advancement in a power conversion efficiency(PCE)to reach 25%,the inorganic perovskites are being explored intensively as promising optoelectronic materials due to their excellent photovoltaic performance,i.e.,thermal stability and efficiency.Lately,the inorganic cesium lead halide perovskite is studied to show enhanced light absorption,however,it suffers from the phase separate into I-rich and Br-rich phase which leads to poor film quality due to difference of electronegativity.Herein,we propose a unique solution of controlling the rate of solvent volatilization followed by gel method to inhibit phase separation effectively to obtain the homogenous and pinhole-free CsPbIBr2 films with high crystalline quality.In this study,an inverted planar device based on a light absorber of CsPbIBr2 is prepared to achieve a power conversion efficiency of 8.8%(maintain a stabilized value of 8%in ambient air conditions).Surprisingly,the optimized cell without encapsulation shows excellent long-term stability,as it maintained 90%initial efficiency over 500 h and controlled storage at around 45%relative humidity and 25℃.