Simultaneous determination of some trace metal impurities in high-purity sodium tungstate using coprecipitation and inductively coupled plasma atomic emission spectrometry

A method based on the combination of coprecipitation with inductively coupledplasma atomic emission spectrometry (ICP-AES) was developed for the determination of impurities inhigh-purity sodium tungstate. Six elements (Co, Cu, Fe, Mn, Ni, and Pb) were coprecipitated bylanthanum hydroxide so as to be concentrated and separated from the tungsten matrix. Effects of somefactors on the recoveries of the analytes and on the residual amount of sodium tungstate wereinvestigated, and the optimum conditions for the coprecipitation were proposed. Matrix-matchingcalibration curve method was used for the analysis. It is shown that the elements mentioned abovecan be quantitatively recovered. The detection limits for Co, Cu, Fe, Mn, Ni, and Pb are 0.07, 0.4,0.2, 0.1, 0.6, and 1.3 μg·g^(-1), respectively. The recoveries vary from 92.5% to 108%, and therelative standard deviations (RSDs) are in the range of 3.1%-5.5%.

Synthesis of Mg_2B_2O_5 whiskers via coprecipitation and sintering process

Mg2B2O5 whiskers with high aspect ratio were synthesized by coprecipitation and sintering process using MgCl2-6H2O, H3BO3, and NaOH as raw materials and KCl as a flux. Their formation process was investigated by thermogravimetry and differential scanning calo- rimetry （TG-DSC）, X-ray diffraction （XRD）, and scanning electron microcopy （SEM）. It is found that the products synthesized at 832℃ are monoclinic Mg2B205 whiskers with a diameter of 200-400 nm and a length of 50-80 μm. Transmission electron microscopy （TEM） and selected area electron diffraction （SAED） analyses show that the whiskers obtained at 832℃ are single crystalline and grow along with the [010] direction. The growth mechanism of Mg2B2O5 whiskers was also presented.

Growth of carbon nanotubes on the novel FeCo-Al_2O_3 catalyst prepared by ultrasonic coprecipitation

FeCo-Al2O3 catalyst was prepared by an ultrasonic coprecipitation （UC） method for the growth of carbon nanotubes （CNTs） from catalytic decomposition of methane.Its catalytic performance was compared with that of the FeCo-Al2O3 catalyst counterparts prepared by stepwise impregnation （I） and conventional coprecipitation （C） methods,respectively.The structure and properties of the catalysts and the CNTs as produced thereon were investigated by means of XRD,XPS,TEM and N2 adsorption techniques.It was found that the catalyst prepared by the ultrasonic coprecipitation method was more active,and the yield and purity of the synthesized CNTs were promoted evidently.The XPS results revealed that there were more active components on the surface of the catalyst prepared by the ultrasonic coprecipitation method.On the other hand,N2 adsorption demonstrated that the catalyst prepared by the ultrasonic coprecipitation method conferred larger specific surface area,which was beneficial to dispersion of active components.TEM images further confirmed its higher dispersion.These factors could be responsible for its higher activity for the growth of CNTs from catalytic decomposition of methane.

Studies on State and Structure of Noble Metals in Electrocatalyst Made by Coprecipitation Method

The electrocatalysts of Pt/C, PtRu/C and Ru/C were prepared by the impregnation method. The facet characterization, the dispersion and the particle size for the catalysts were determined by means of X ray diffraction and transmission electron microscopy. X ray photoelectron spectroscopy was also used to analyze the state and the valency of the noble metals. The results show that the particle size was in nanometer range and the binary metals have come into being an alloy. The platinum in the catalysts existed in zero valency. The valency of the ruthenium on the surface is different from that in the body, while the ruthenium on the surface existed in oxide form. PtRu/C and Pt/C are of good activity to the electrooxidation of hydrogen except Ru/C. PtRu/C is more tolerant of CO than Pt/C, and CO is only adsorbed on Pt.

Characterization of (Y,Gd)B_xV_(1-x)O_(4-x)∶Eu Phosphor Prepared by Coprecipitation Reaction

White body-color （Y, Gd）BxV1-xO4-x ：Eu^3＋ phosphors were prepared by coprecipitation reaction. Under VUV excitation at 147 nm, the red emission colorimetric purity of （Y, Gd） BxV1-xO4-x： Eu^3＋ phosphor is much better than that of commercial PDP （plasma display panels） phosphor （Y, Gd）BO3：Eu^3＋ . But its relative emission intensity is only about 90% of the commercial phosphor.

Comparison of the Sol-gel Method with the Coprecipitation Technique for Preparation of Hexagonal Barium Ferrite

Hexagonal barium ferrite BaFe12O19 particles were prepared by sol-gel and coprecipitation methods, respectively. The composition of the so-obtained materials was investigated by means of XRD. By the sol-gel method, non-anticipated intermediate crystalline phases, such as γ-Fe2O3, α-Fe2O3, BaCO3, and BaFe2O4 etc., were formed with the delay of the formation of BaFe12O19. The formation of single phase BaFe12O19 required calcination at 850 oC for 4 h. On the other hand, using coprecipitation technique, amorphous hydroxide precursor was directly transferred into BaFe12O19 almost without the formation of intermediate crystalline phases. BaFe12O19 was prepared by calcining at 700 oC for 3 h. The results were confirmed by ESEM and VSM analyses. Based on the already reported results and the observed results in this study, it can be concluded that the coprecipitaion technique is easier to control than the sol-gel method for preparation of BaFe12O19 at a low temperature.

A Coprecipitation Coating Synthesis of SiC/YAG Composites

The α-SiC in 0.5μm size powders were coated with Al_2O_3 and Y_2O_3 by a coprecipitation coating (CPC) method forfabrication of SiC/YAG composites. The same powder preparation was carried out by conventional mechanical mixing(MM) method for comparison. Two kinds of SiC/YAG composites were manufactured by pressureless sintering usingthe different powders, named CPC composite and MM composite thereafter respectively. It is shown that the CPCcomposite has the advantages of homogeneous distribution of YAG phase and of being sintered to high density ata low temperature, 100℃ lower than that of MM composite. The strength (573 MPa) and hardness (23.3 GPa) ofthe CPC composite are significantly higher than those (323 MPa and 13.5 GPa) of the MM composite, respectively.

COPRECIPITATION PREPARATION AND VOLTAGE SENSITIVE CHARACTERISTICS OF DOPED ZnO VARISTOR

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Coprecipitation of metal ions into calcite: an estimation of partition coefficients based on field investigation

Trace elements(and their isotopes)in carbonates are commonly used to reconstruct paleoenvironment and paleoclimate.Understanding the processes and mechanisms of element incorporation into carbonates is thus crucial for using such geochemical parameters as paleoclimate proxies.In contrast to laboratory-based experimental results,the partitioning of trace metals between solid and solution phases in natural carbonate precipitation systems has rarely been reported.In this study,we investigated the partition coefficients of metal ions between solid and solution in the channel of the natural Baishuitai travertine system,Yunnan,China.Our results show that the partition coefficients of Li+,Na+,Mg2+,Sr2+and Ba2+are<1,that of Ni2+is approximately 1,and those of Co2+,Mn2+,Zn2+and Cu2+are>1,consistent with the results found in previous experimental studies.Although the substitution for Ca2+is likely the main uptake process of these metals into calcite,depending on their ionic radius and charge,trace elements may also be incorporated by adsorption or physical entrapment.Our study shows that unlike laboratory experiments performed under specific conditions,the partitioning of metals between two phases in the natural travertine system could be controlled by several,even multiple,environmental factors(e.g.,carbonate deposition rate,temperature,and pH),which should be taken into account when using trace metals(and their isotopes)in carbonate archives as a paleoclimate proxy.

Assessment of the conventional molybdenum-blue and magnesium-induced coprecipitation procedures in phosphorus measurement in various aquatic environments

Phosphorus （P） is an essential nutrient utilized by all organisms for energy transport and growth. Both the conventional molybdenum-blue method and the magnesium-induced coprecipitation （MAGIC） procedures were applied for the measurement of dissolved inorganic phosphorus （DIP） and total dissolved phosphorus （TDP） in more than 840 water samples collected between 2003 and 2005, including seawater （the Huanghai Sea, the East China Sea, and the northern South China Sea）, water from rivers and estuaries （the Changjiang, the Huanghe, and the major rivers emptying into the Jiaozhou Bay）, groundwater （in the drainage basin surrounding the Jiaozhou Bay）, rain-water, and aquaculture water samples. The MAGIC method allows the investigation of phosphorus distributions and cycling for systems in which DIP is below the detection limits of conventional methods. Comparison between the two methods demonstrated that the concentrations obtained with both methods were significantly correlated. The differences of DIP and TDP concentrations measured with the two methods were higher when the concentrations of DIP and TDP were lower, implying the lower reproducibility at low concentrations. The concentration differences increase with the increase in the proportion of DOP in TDP, which indicates that the discrepancy of DIP concentrations measured with the two methods increases when the DOP concentration is high. The discrepancies indicated that the composition of P compounds differs depending on sample sources and water type; it would be useful to infer the presence of different phosphorus compound pools from differences between the two methods. This study indicates the potential presence of a pool of alkaline-labile compounds for samples from rainwater and rivers and estuaries surrounding the Jiaozhou Bay; the potential presence of acid-labile compounds that were adsorbed by Mg（OH）2 for samples from the Changjiang Estuary, Huanghai Sea, East China Sea, and groundwater; the potential presence of a substantial pool of acid-labile compounds that were not adsorbed by Mg（OH）2 for samples from the Huanghe Estuary, aquaculture water, the East China Sea algal bloom water, and the northern South China Sea.

Synthesis of (1-x)Pb[(Mg,Zn)_(1/3)Nb_(2/3)] O_3-PbTiO_3 DielectricCeramic Powder by a Coprecipitation Process

A coprecipitation method was used for preparation of 0.95Pb[(Mg0.8,Zn0.2) 1/ 3 Nb2 /3]O3-0.05PbTiO3(PMZN-PT),dielectric ceramic powder. X-ray powder diffraction and electron probe energy dispersive, X-ray analyzer revealed that the powder calcinated at 800℃ for 2 h is the PMZN-PT with 100% single perovskite phase, and the order of magnitude of atomic proportion of Mg to Zn reaches approximately 10: 1. In addition, the influence of Zn and Ti content on the perovskite phase and pyrochlore phase formation namely : 0.95Pb[(Mg1-x Znx) 1 /3Nb,2/3]O3 -0.05PbTiO3, (1-y)Pb[(Mg0.7Zn0.3) 1 /3Nb2 /3] O3-yPbTiO3 was also analysed.

Determination of Trace Amount of Vanadium in High Purity Y_2O_3 by Electrothermal Vaporization－ICP－AES With Bi（PDC）_3 Coprecipitation

A new method for the determination of vanadium in high purity Y2O3 by fluorination assisted electrothermal vaporization-ICP-AES is presented in this paper. After the sample dissolved,the vanadium in the sample solution was coprecipitated with Bi(PDC)_3 at pH 3. 7. The precipitates were made into a slurry with the fluorinating agent PTFE and directly introduced into the graphite furnace for determination. The analytical results were obtained by aqueous calibration curve method. The detection limit of the method is 1. 1 ng/mL, the RSD is 2. 8% (n=10,1 5 ng/mL vanadium solution), and the recovery of vanadium added to real sample is more than 96%.

Synthesis and Tribological Properties of Copper-alumina Nanocomposites Prepared by Coprecipitation Technique

The objective of this work is to study the synthesis of copper-alumina nanocomposites using the coprecipitation process and hot-pressing method, and investigate their mechanical properties. The effects of calcination temperature on the average size of composite particles and chemical composition after calcination were also analyzed. The sintering parameters including sintering temperature, hot pressure and packing time were optimized to fabricate the alumina nanoparticles reinforced copper matrix composites（CMCs）. The density, microhardness and tribological properties of the CMCs reinforced with 1 wt%, 2 wt%, 3 wt%, 4 wt% and 5 wt% of alumina nanoparticles were investigated correspondingly. The results showed that the optimum preparation parameters for the CMCs were 900 ℃ of hot pressing temperature, 27.5 MPa of hot pressure and 2 hrs of packing time. The CMC reinforced with 2 wt% of alumina nanoparticles had the lowest wear rate, with the relative wear resistance of 3.13.

Method to Study the Primary Nucleation for Solid Solution: Application to Uranium-Neodymium Oxalate Coprecipitation

Actinides co-precipitation is currently investigated in order to synthesize solid solutions of actinides mixed oxalates. This paper deals with the thermodynamic and kinetic study of the precipitation of uranium-neodymium oxalate system. Based on an analysis of the theories developed in the literature, a new expression for the determination of the supersaturation ratio for the solid solutions is presented. An experimental study of the nucleation kinetics was performed on the mixed uranium-neodymium oxalates. Homogeneous and heterogeneous primary nucleation laws are obtained using a specific stopped flow apparatus. The experimental results are consistent with the classical behaviour of nucleation phenomena. The values of the kinetic parameters for the solid solution point out that the formation of the uraniumneodymium mixed oxalates is kinetically favoured compared with the simple uranium and neodymium oxalates.

Enhanced thermal stability of Ce_(0.33)Zr_(0.55)(LaNdY)_(0.12)O_(2) mixed oxides prepared by sulfate-aided coprecipitation method

Ceria-zirconia based mixed oxides(CZs)have been applied in three-way catalysts(TWCs)for their high surface area and oxygen storage capacity(OSC).In this work,enhanced thermal stability of Ce_(0.33)Zr_(0.55)(LaNdY)_(0.12)O_(2)mixed oxides was realized via a facile and scalable approach,namely,sulfateaided coprecipitation method was labelled as CZ-S.Sulfate ion(SO_(4)^(2-))was added into raw solution in the form of sulfuric acid and acted as coordination agent.The control sample was prepared by conventional coprecipitation method without sulfuric acid added and labelled as CZ.The promotion effect of sulfate ion was analyzed systematically by X-ray diffraction(XRD),transmission electron microscopy(TEM),scanning electron microscopy(SEM),N_(2)adsorption-desorption,Fourier transform infrared spectroscopy(FT-IR),X-ray photoelectron spectroscopy(XPS),OSC and hydrogen temperatureprogrammed reduction(H_(2)-TPR)analysis.XRD and high resolution TEM results reveal that CZ-S have homogeneous distributions of elements.TEM and SEM images show that fresh samples of CZ-S have narrower distributions of grain sizes and larger pore sizes than those of CZ.Through cross analysis of structure and morphology of CZ and CZ-S,we find that the introduction of sulfate ions results in uniform distributions of elements,narrows distributions of grain sizes,and enables the formation of secondary loose packing of sub-particles,which lead to enhanced thermal stability of the samples of CZ-S upon aging process at high temperature.After aging treatment at 1100℃for 10 h,aged samples of CZ-S present larger specific surface areas and pore volumes than the aged sample prepared by conventional coprecipitation method without sulfate ions added.Furthermore,the aged sample of CZ-S2(SO_(4)^(2-)/Zr=1)possesses the highest specific surface area of 21.9 m2/g and the biggest pore volume of 0.035 mL/g among all aged samples.

Modified coprecipitation process of synthesizing Bi-system superconductor precursor powder and its stoichiometry

A modified coprecipitation process is presented based on the stoichiometry study of oxalate coprecipitation process in water medium to synthesize Bi-Pb-Sr-Ca-Cu-O multi-component powder.Its characteristic is that the coprecipitation reaction takes place in a mixed solution medium composed of water and a kind of organic solvent (volume percentage 】90%).Thus,it overcomes the serious shortcoming of inability to maintain stoichiometry in Bi-system superconductor powder synthesized by water-medium coprecipitation.The effects of pH value,oxalic acid concentration and aging time on stoichiometry maintenance in precipitate are systematically studied.Bulk material made from the powder prepared by the new modified coprecipitation also shows the success of the new process.

Properties of Co_2FeAl Heusler Alloy Nano-particles Synthesized by Coprecipitation and Thermal Deoxidization Method

Co2FeAl nanoparticles were synthesized by reducing the coprecipitated precursor of COCl2·6H2O, Fe（NO3）3·9H2O and AI2（SO4）3·18H2O under H2 atmosphere with various annealing temperatures and durations. X-ray diffraction and transmission electron microscopy were used to characterize the crystal structure and microstructure of Co2FeAl particles, respectively. The investigation indicates that the crystal structure of CO2FeAI particles tends to be B2 structure, in which atoms are partially ordered. The saturation magnetization and hyperfine field of CO2FeAI particles, which were measured under a vibrating sample magnetometer and a 57Fe Mossbauer spectroscope, are consistent with those of the bulk sample and thin films. Furthermore, the higher annealing temperature and the longer annealing time, the better crystallinity of CO2FeAI and more ordered arrangement of atoms will be. It turned out that the coprecipitation thermal deoxidization method could be an easy and high efficient way to obtain the half-metallic CO2FeAI nanoparticles.

Facile room-temperature coprecipitation of uniform barium chlorapatite nanoassemblies as a host photoluminescent material

As an emerging host phosphor material, barium chlorapatite （Bas（PO4）3CI）, is attracting growing attention. However, rare earth-doped Bas（PO4）3CI phosphors have mainly been obtained via high temperature-based, energy-consuming techniques. In this contribution, we developed a straight- forward, facile room-temperature coprecipitation method in the presence of a specific amount of ethylenediaminetetraacetic acid disodium salt that provided Bas（PO4）3CI nanoparticles self-assembled to construct uniform Bas（PO4）3CI nanoassemblies （diameter： 80-120 nm） as well as rare earth Tb3＋- doped Bas（PO4）3CI：xTb3＋ nanophosphors. The nanoassemblies were transparent within the ultraviolet and visible spectral range. The Bas（PO4）3CI：xTb3＋ nanophosphors exhibited four emission peaks under 228-nm excitation, and the optimal doping amount of Tb3＋ was 4.0%. In contrast to traditional energy-consuming, high-temperature techniques, the facile room-temperature coprecipitation method developed here represents an attractive alternative route to obtain uniform Ba5（PO4）3CI nanoassemblies and Bas（PO4）3CI：xTb3＋ nanopbosphors that are candidate luminescent hosts.

A new type-γ'/γ''coprecipitation behavior and its evolution mechanism in wrought Ni-based ATI 718Plus superalloy

In the precipitation-hardened Ni-based superalloy,typified by ATI 718 Plus,the nano-scaleγandγphase in duplet or triple coprecipitate morphology can provide superior high-temperature strength.Thus,it is of great sense to study the evolution ofγ’/γ’’coprecipitate during long term service at elevated temperature.In this study,the new-typeγ’/γ’’coprecipitates with a sandwich or compact configuration were found firstly in wrought ATI 718 Plus superalloy during long term thermal exposure at 705℃.These co-structure of theγ’/γ’’precipitates evidently inhibit the coarsening ofγ’phase.The increase of thermal exposure time evidently leads to the increase of the volume fraction ofγ’/γ’’coprecipitate and transformation of sandwich-typeγ’/γ’’coprecipitate to compact-typeγ’/γ’’coprecipitate,which is characterized asγphase precipitate at several faces of theγphase.The main evolution mechanism ofγ’/γ’’coprecipitates is element segregation,especially the composition variations of Al+Ti and Nb and their ratio of Al+Ti/Nb.In addition,the interfacial energy betweenγ’’phase andγmatrix also plays a key role on theγ’/γ’’coprecipitates evolution.The calculated results show that the longer thermal exposure time leads to the higher interfacial energy,which is beneficial for nucleation and precipitation ofγ’’phase on the faces ofγ’phase.

Catalytic properties of Cu/Co/Zn/Zr oxides prepared by various methods

The new Cu-Co based （Cu/Co/Zn/Zr） catalysts for higher-alcohol synthesis were prepared using coprecipitation method, plasma enhanced method and reverse coprecipitation method under ultrasound irradiation. The catalysts were investigated by the means of BET, SEM, XRD, H2-TPR and XPS. Catalytic properties of the catalysts prepared by various methods were examined using CO hydrogenation reaction. It was found that plasma enhanced method and reverse coprecipitation method under ultrasound irradiation were both effective in enhancing the catalytic properties of Cu/Co/Zn/Zr mixed oxides. The small particle size, high dispersion of active components, the improvement of specific surface area and surface contents of active phases could account for the excellent performance of the experimental Cu/Co/Zn/Zr catalysts.