Direct and Simultaneous Determination of Several Impurity Elements in Manganese Tetroxide using ICP-AES

A rapid method for the determination of impurity elements, such as Zn, Ni, Co, Cr, Cu, Cd and Pb in manganese tetroxide was developed, using inductively coupled plasma atomic emission spectrometry （ICP-AES）. The critical instrumental parameters such as sample flow rate and radio frequency incident were thoroughly optimized. The effect of matrix was also examined. The sensitivity was investigated using calibration curves obtained in presence of the matrix. The obtained recoveries for Ni, Co, Cr, Cu, and Cd at the μg· g^ -1 level were satisfactory and practically independent of the matrix used for the calibration standards. The recoveries of Pb and Zn were less suffwient. The method can be applied for routine analysis and quality control purposes at μg· g^-1 level of concentration.

Determination of trace impurity elements in MnZn ferrite powder by direct current glow discharge mass spectrometry

An analytical method for the determination of 26 impurity elements （such as Li, Be, Na, Mg, Al, Si, P, S, K, Ca, Sc, Ti, V, Cr, Co, Ni, Ga, Ge, Y, Nb, Mo, Ag, Cd, Sb, W and Pb） in MnZn ferrite powder by direct current glow discharge mass spectrometry （GD-MS） was established. MnZn ferrite powder was mixed with copper powder, used as a conductor, and pressed. The effects of MnZn ferrite powder preparation conditions and glow discharge parameters for the sensitivity and stability of signal analysis were investigated. By determining the choice of isotope and the application of the mass resolutions of 4000 （MR, medium resolution） and 10000 （HR, high resolution）, mass spectral interference was eliminated. The contents of impurity elements in MnZn ferrite powder was calculated by subtraction after normalizing the total signal of Mn, Zn, Fe, O and Cu. The results showed that the detection limit of 26 kinds of impurity elements was between 0.002 and 0.57 μg/g, and the relative standard deviation （RSD） was between 3.33% and 32.35%. The accuracy of this method was verified by the ICP-MS. The method was simple and practical, which is applied to the determination of impurity elements in MnZn ferrite powder.

Determination of impurity elements in MnZn ferrites by inductively coupled plasma mass spectrometry

An inductively coupled plasma mass spectrometry(ICP-MS) method was developed for the determination of Na, Mg, Al,K, Ca, Ti, Cr, Co, Ni, Cu, Ga, As, Mo, Ag, Cd and Pb in MnZn ferrites. The sample was digested by HNO3+HCl with microwave digestion followed by dilution with ultrapure water, then the above 16 impurity elements in the solution were analyzed directly by ICP-MS. The impurity elements were introduced by the helium gas or hydrogen gas into the octopole reaction system(ORS) to eliminate the polyatomic interferences caused by the high salty matrixes. The matrix effect was minimized through matrix matching,and Be, Y and Rh were used as internal standard elements. The working parameters of the instrument were optimized. The results show that the method has good precision and high accuracy. The detection limits for the investigated elements are in the range of0.9-37.5 ng/L, the relative standard deviation of each element is within 1.1%-4.8%, and the recovery of each element is 90%-108%.

DETERMINATION OF IMPURITY ELEMENTS IN ALUMINIUM

Twenty five impurity elements in aluminium applied as reactor material are determined. Titanium and nickel are determined with epithermal neutron activation analysis (NAA), magnesium and silicon by inductance coupling plasma emission spectra (ICP), other elements by thermal NAA. The fission coefficient of uraniumis given by an experiment, the interferences of uranium to Ce, Nd, Mo, Zr, La, Sin are subtracted. The detection limits of these methods to all of impurity elements in aluminium are calculated.

Simultaneous Determination of Trace Rare Earth Elements and Other Elements in High Purity Terbium Oxide (Tb_4O_7) by ICP-AES After HPLC Separation Using P507 Resin

This article describes a new method for the simultaneous determination of trace rare earth elements (REEs) and non rare earth elements (NREEs) in high purity terbium oxide by ICP-AES after HPLC separation using P507 resin. The chromatographic separation of the analytes from the matrix using dilute nitric acid as mobile phase was studied. The experimental results showed that a favorable separation of trace metals (Cu and Gd) from the matrix (Tb) can easily be achieved by elution with dilute nitric acid within 25 min. The proposed method was applied to the determination of trace metals (Ca, Cu, Mg, Mn, Ni, Si, La, Ce, Pr, Nd, Sm, Eu and Gd) in high purity terbium oxide. The detection limits (DLs) for the analytes ranged from 0.4-4.0 μg\5g -1, and the recoveries are from 78%-105%.

Features of rare earth elements geochemistry in coals of Central Kazakhstan

This research presents the results of a comprehensive study of mineralogical and geochemical features of REE distribution in coals of Central Kazakhstan deposits—Karaganda coal basin and Shubarkol deposit,which have large hard coal reserves and are industrially important for the coal industry of Kazakhstan;the research is based on 205 samples of clayey interlayers and coal seams.It shows basic patterns of distribution and features of concentration for impurity elements,gives an estimate of the impurity elements concentration,including REE,defines conditions and factors of their accumulation,and studies features of their forms in coal and coal-bearing rocks,which allows estimating the mechanisms of their migration and conditions of accumulation.According to the results of geochemical indicators,the article establishes the factors of REE dislocation,reveals the composition of margin rocks that have influenced REE concentration in coal seams,and the presented latest data on mineralogy allowed to establish the ways of their transportation to the paleobasin during the synand epigenetic periods of formation of the coal deposits of Central Kazakhstan being researched.It was found that the coals are insignificantly enriched with heavy lanthanides from Ho to Lu.The distribution curves of UCC normalized REE values in the coals are similar and coincide,but they are less than the average value for world coal,and amount to only one-third of the UCC.It was found that the highest concentrations of all REE are characteristic of clayey interlayers and oxidized coals.The La/Yb ratio in this case increases upwards along the section,indicating mainly clastogenic mechanism of REE delivery to the coals.In coal and clay samples,the predominant mineral form of REE is light lanthanide phosphates.Identified particles of REE from minerals and their composition peculiarities suppose autigene nature of their formation.The formation of the bulk of autigene minerals occurred during the maturation of brown coals and their transformation into hard ones.

Determination of Trace Impurities of Rare Earth Elements in High Purity Yttrium Oxide by ICPMS

Determination of trace rare earth elements(REEs)in 99. 999% purity yttrium oxide using the inductively coupled plasma mass spectrometric technique (ICPMS) has been developed. Instrumental parameters and factors affecitng analytical results have been studied and then optimized.Samples are analyzed directly following an acid digestion without separation or preconcentration and with limit of detection of 0. 003～0. 02 ng/ml, precision of ±5. 4%(cofficient of variation)and recovery of 90～115%. Correction for isobaric interferences from oxide ions and hydroxide ions is made mathematically. Special internal standard procedures are used to compensate drift in metal:metal oxide ratios and sensitivity. The analytical results of several samples are accurate as compared with inductively coupled plasma atomic emission spectrometry (ICPAES) and spark source mass spectrometry (SSMS).

Progress of Separation and Determination Methods for Rare Earth Elements

This review covers the developments in rare earth elements analysis over the period from 2003 to 2005. Some novel separation and determination methods and their applications in rare earth elements analysis were presented and discussed in detail. Some new materials, such as ionic liquids, nanometer materials and ion-imprinted polymers, and some new technologies, such as cloud point extraction, membrane extraction and capillary electrophoresis were successful used in rare earth elements analysis. The determination methods of NAA, ICP-OES and ICP-MS were also discussed in detail.

Recent Development in Simultaneous Multi-Element Determination of the Platinum Group Elements and Gold in Geological and Environmental Samples

In recent years, the modern methods of multi-element analysis of precious metals have attracted wide attention in scientific research and industry. The application and development in the decomposition of samples, separation and enrichment, and modern instrumental analysis of the platinum-group elements (PGEs) and gold in geological and environmental samples have been reviewed. Finally, the tendency of analysis of precious metals is also prospected.

First-principles Investigation on Solution Hardening of Interstitial Impurity Elements (O,N) inγ-TiAl

We have calculated the electronic Structures of O-doped and N-doped r-TiAl using the firstprinciples discrete variational method (DVM) with the aim to understand the solution hardening effects of oxygen and nitrogen in r-TiAl. Our combination analysis on the electronic density, density of states (DOS) and the local environment total bond orders (LTBO) will show that, X atom (X is O or N) can strongly bind with its six surrounding atoms via electronic hybridizations of Ti-3d/X-2p and Al-3p/X-2p. As a sequence, there forms a 'hard' cohesive region around the impurity atom. A pinning model based on the calculations is proposed to explain the hardening effects. The consistent results are obtained between the present calculation and formal test experiments.

Determination of Impurity Silicon in Anticancer Drug (Ge-132) by Electrothermally Atomised Atomic Absorption Spectrometry with Optical Temperature Control Accessory

The present paper describes the ashing and atomization processes in silicon analysis by electrothermally atomised atomic absorption spectrometry(EAAAS) with an uncoat-ed graphite tube, a pyrolytically coated graphite tube and a tungsten-coated graphitetube. The sensitivity and linear range of three graphite tubes were compared. By using optical temperature control accessory, the signals are enhanced by a factor of 2 and the germanium interferences in the determination of silicon are eliminated. The effects of time constant and carrier gas flow-rate on the determination of silicon were also tested. The sample can be directly analyzed in its aqueous solution without any pretreatment. The measurements of samples containing 0. 2 μg/mL and 0. 4 μg/mL silicon were run ten times and the variation coefficient is 4. 9% and 2.6%, respectively. The recovery tests for carboxyethyl germanium sesquioxide(Ge-132) synthesized and imported were performed, and the recoveries are 97. 0% and 110%, respectively. Keywords Carboxyethyl germanium sesquioxide, Electrothermally atomised atomic absorption spectrometry, Silicon

THE USE OF CHELATING RESIN FOR THE PRE-CONCENTRATION OF TRACE RARE EARTH ELEMENTS IN BIOLOGICAL SAMPLES AND THEIR DETERMINATION

Macroporous amino-carboxvlic chelating resin of acrylic acid series may concentrate trace rare earth in the presence of 0.1 mol/l α-hydroxy-isobutyric acid at pH 4.5.With 0.10 mol/l HCl as eluant rare earth may be eluted quantitatively and separated from Ca,Mg,Fe and Cu.This method is used to determine trace amount of rare earth in human hair,stone (in kidney and bladder),peanut,grape,strawberry,cucumber,pig liver and other biological samples.

Electronic Theoretical Study of the Interaction between Rare Earth Elements and Impurities at Grain Boundaries in Steel

The model of dislocations was used to construct the model of grain boundary (GB) with pure rare earths, and rare earth elements and impurities. The influence of the interaction between rare earth elements and impurities on the cohesive properties of 5.3° low angle GB of Fe was investigated by the recursion method. The calculated results of environment sensitive embeding energy( E ESE ) show that the preferential segregation of rare earth elements towards GBs exists. Calculations of bond order integrals (BOI) show that rare earth elements increase the cohesive strength of low angle GB, and impurities such as S, P weaken the intergranular cohesion of the GB. So rare earth element of proper quantity added in steel not only cleanses other harmful impurities off the GBs, but also enhances the intergranular cohesion. This elucidates the action mechanism of rare earth elements in steel from electronic level and offers theoretical evidence for applications of rare earth elements in steels.

Impurity Profiling of Solid Oral Drug Products to Sail through GDUFA-II Requirements

Defining impurity profile is key element to ensure safe, efficacious and quality human drugs. Impurity profiling changed/transformed drastically over the years. Guidelines, specifications and requirements are evolving. Initially impurity profiling was based on simple methods later by degradation studies, then to understand drug strength and efficacy chiral impurities and stereo isomers were included followed by residual solvents, polymorphic forms, genotoxic impurity studies. Currently, elemental impurities are the latest addition. As per the GDUFA II guidelines to improve review efficiency and reduce review cycles, data requirements have changed. Based on recent guidance and review points, Impurity profiling has significant importance in ANDA filing and to ensure approval within 10 months (first cycle approval) which is an exiling aspect for industries to enter into the generic market quickly. Hence, Impurity profile is a key aspect scientifically, regulatory wise and commercially also. This is a review article on impurity profiling of Solid oral drug substances and products as per GDUFA II requirements the reference documents for the review are ICH guidance, relevant FDA GDUFA guidance and common industry practices.

DETERMINATION OF CREEP PARAMETERS FROM INDENTATION CREEP EXPERIMENTS

The possibilities of determining creep parameters for a simple Norton law material are explored from indentation creep testing. Using creep finite element analysis the creep indentation test technique is analyzed in terms of indentation rates at constant loads. Emphasis is placed on the relationships between the steady creep behavior of indentation systems and the creep property of the indented materials. The role of indenter geometry, size effects and macroscopic constraints is explicitly considered on indentation creep experiments. The influence of macroscopic constraints from the material systems becomes important when the size of the indenter is of the same order of magnitude as the size of the testing material. Two methods have been presented to assess the creep property of the indented material from the indentation experimental results on the single-phase-material and two-phase-material systems. The results contribute to a better mechanical understanding and extending the application of indentation creep testing.

Magnetic property improvement of niobium doped with rare earth elements

A new idea is proposed by the PKU group to improve the magnetic properties of the Type-Ⅱ superconductor niobium. Rare earth elements like scandium and yttrium are doped into ingot niobium during the smelting processes. A series of experiments have been done since 2010. The preliminary testing results show that the magnetic properties of niobium materials have changed with different doping elements and proportions while the superconductive transition temperature does not change very much. This method may increase the superheating magnetic field of niobium so as to improve the performance of the niobium cavity, which is a key component of SRF accelerators. A Tesla-type single-cell cavity made of scandium-doped niobium is being fabricated.

DETERMINATION OF CREEP PROPERTIES OF THERMAL BARRIER COATING(TBC)SYSTEMS FROM THE INDENTATION CREEP TESTING WITH ROUND FLAT INDENTERS

Indentation creep behavior with cylindrical flat indenters on the thermal barrier coating (TBC) was studied by finite element method (FEM). On ike constant applied indentation creep stress, there is a steady creep rate for each case studied for different creep properties of the TBC system. The steady creep depth rate depends on the applied indentation creep stress and size of the indenters as well as the creep properties of the bond coat of the TBC and the substrate. The possibilities to determine the creep properties of a thermal barrier system from indention creep testing were discussed. As an example, with two different size indenters, the creep properties of bond coat of the TBC system can be derived by an inverse FEM method. This study not only provides a numerical method to obtain the creep properties of the TBC system, but also extends the application of indentation creep method with cylindrical flat indenters.

A Determinant Criterion of Invertible Elements in Group Algebras

An embedding from a group algebra to a matrix algebra is given in this paper. By using it, a criterion for an invertible element in a group algebra is proven.

Recombination of repeat elements generates somatic complexity in human genomes

Non-allelic recombination between homologous repetitive elements contributes to evolution and human genetic disorders.Here,we combine short-and long-DNA read sequencing of repeat elements with a new bioinformatics pipeline to show that somatic recombination of Alu and L1 elements is widespread in the human genome.Our analysis uncovers tissue-specific non-allelic homologous recombination hallmarks;moreover,we find that centromeres and cancer-associated genes are enriched for retroelements that may act as recombination hotspots.We compare recombination profiles in human-induced pluripotent stem cells and differentiated neurons and find that the neuron-specific recombination of repeat elements accompanies chromatin changes during cell-fate determination.

熔炼温度对含钼渣冶炼MoFe中杂质元素含量的影响

采用低温冶炼工艺,利用氨浸渣和钼酸钙渣两种含钼工业废渣直接还原冶炼钼铁。研究了熔炼温度对MoFe合金中C、P、S、Si、Cu等杂质元素含量的影响。结果表明,熔炼温度为1 500℃时,MoFe合金中杂质元素含量均符合国标GB/T 3649—2008要求。