Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

A An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of 24 elements （Be, Mg, A1, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn Sb, Ba, Pt, Au, and Pb） in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCI. The matrix effects because of the presence of excess HCI and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 ].tg·g^-1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.

Quantification of Trace Amounts of Impurities in High Purity Cobalt by High Resolution Inductively Coupled Plasma Mass Spectrometry

An analytical method using high resolution inductively coupled plasma mass spectrometry （HR-ICP-MS） for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.

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).

Direct Determination of Trace Impurities in High Purity Zinc Oxide by High Resolution Inductively Coupled Plasma Mass Spectrometry

The determination of trace impurities in high purity zinc oxide by high resolution inductively coupled plasma mass spectrometry （ HR-ICP-MS ） was investigated. To overcome some poteutially problematic spectral iuterference, measurements were acquired in both middle and high resolution modes. The matrix effects due to the presence of excess HCl and zinc were evaluated. The optimum conditions for the determination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits ranged from 0.02μg/ g to 6 μg/ g depending on the elements. The experimental resalts for the determination of Na, Mg, Ca, Cr, Mn, Fe, Co, Ni, Cu, Mo, Cd, Sb and Pb in several high purity zinc oxide powders were presented.

Simultaneous determination of seven impurities in high-purity cobalt oxide by ICP-AES after matrix separation using 1-nitroso-2-naphthol as a precipitant

A method was developed for the simultaneous determination of seven trace impurities (Cd, Mn, Pb, Zn, Cu, Fe and Ni) in high purity cobalt oxide by ICP AES. The matrix effect was eliminated by preci pitation with 1 nitroso 2 naphthol. The matrix effect of cobalt on the absorptions of trace impurities, the effects of reaction time, pH value, dosage of precipitant on the formation of cobalt 1 nitroso 2 naphthol complex, the effects of hydrochloric acid on the stability of this complex and masking of elements were studied. Recoveries of the impurities in spiked sample are from 90% to 110% with a precision of 1.1% 5.0% RSD. The detection limits of the seven elements are in the range of 0.01 0.24μg/g. The method can be applied to the analysis of high purity cobalt metal, cobalt oxide and other cobalt compounds.

OAM mode purity improvement based on antenna array

Orbital Angular Momentum(OAM)waves are characterized by helical wave fronts and orthogonality between different modes.Therefore,OAM waves have huge potential in improving wireless communications'channel capacity and radar imaging's resolution.Consequently,the generation and application of OAM waves have attracted a lot of attention.And many methods are proposed to generate OAM waves.Although antenna array is the most popular method of generating OAM waves,OAM waves generated by antenna array have redundant modes.However,all advantages of OAM waves are closely related to infinite OAM modes.Thus,to better apply OAM waves to wireless communications and radar,it is very important to reduce unnecessary OAM modes and improve the OAM mode purity.In order to improve the OAM mode purity,two combined antenna arrays composed of X direction antenna and Y direction antenna array are proposed in this paper.The X direction antenna array and the Y direction antenna array are supplied by the excitations with the same amplitude and fixed phase shift.The overall phase shift of the X direction antenna array isπ/2 more or less than that of the Y direction antenna array.The results of formulas and antenna models in CST show that the combined antenna arrays can generate OAM waves with less redundant modes in x component,y component and z component.Besides,the z component carries pure OAM modes.

Preparation of High－purity Sodium Tungstate from Low－grade Tung－sten－concentrate with a High Content of Calcium and Other Impurities

A new technological process for production of talium tungstate from low-grade tungsten-concentrate witha high content of calcium and other impurities has been studied. The experiments showed that average tungstenleaching efficiency of more than 96. 92 % can be obtained with a low NaOH consumption by using the mechani-cal activating caustic decomposition , and the content of main impurities (P, As, Si) in Na_2WO_4 solution ob-tained is competitive with that from standard wolframite concentrate by traditional caustic decomposition. Afterrecovering caustic liquor by first crystallization, molylxlenum is removed from Na_2WO_4 solution by ion ex-change method. High-purity sodium tungstate is obtained by second crystallization of Na_2WO_4 solution. Thistechnology has the advantages of good adaptability for raw materials, high removing efficiency of impurities,high tungsten recovery and high economic benefit.

Determination of Non-Rare Earth Impurities in High Purity Lanthanum Oxide by Inductively Coupled Plasma Atomic Emission Spectrometry after HPLC Separation Using P507 Resin

A new method for the determination of trace non-rare earth elements (NREEs) impurities in high-purity lanthanum oxide by HPLC combined with ICP-AES is proposed. The chromatographic retention behaviors of matrix (La) and NREEs were studied using 2-ethylhexyl hydrogen 2-ethylhexyl phosphonate (P507) chelating resin as the stationary phase and dilute nitric acid as the mobile phase. It is found that the use of pH 1.7 nitric acid enables effective elution of NREEs from HPLC column, but the lanthanum remains on the column. The experimental results show that a favorable separation between matrix lanthanum and NREEs can be obtained within 15 min. The method proposed is applied to the determination of 8 NREEs impurities in high-purity La2O3. The recoveries of 8 NREEs are in the range of 90 % similar to 110 %.

Structure uniformity and limits of grain refinement of high purity aluminum during multi-directional forging process at room temperature

The effect of forging passes on the refinement of high purity aluminum during multi-forging was investigated. The attention was focused on the structure uniformity due to deformation uniformity and the grain refinement limitation with very high strains. The results show that the fine grain zone in the center of sample expands gradually with the increase of forging passes. When the forging passes reach 6, an X-shape fine grain zone is initially formed. With a further increase of the passes, this X-shape zone tends to spread the whole sample. Limitation in the structural refinement is observed with increasing strains during multi-forging process at the room temperature. The grains size in the center is refined to a certain size （110 μm as forging passes reach 12, and there is no further grain refinement in the center with increasing the forging passes to 24. However, the size of the coarse grains near the surface is continuously decreased with increasing the forging passes to 24.

Signal-purity-spectrum-based colored deconvolution

Signal to noise ratio （SNR） and resolution are two important but contradictory characteristics used to evaluate the quality of seismic data. For relatively preserving SNR while enhancing resolution, the signal purity spectrum is introduced, estimated, and used to define the desired output amplitude spectrum after deconvolution. Since a real reflectivity series is blue rather than white, the effects of white reflectivity hypothesis on wavelets are experimentally analyzed and color compensation is applied after spectrum whitening. Experiments on real seismic data indicate that the cascade of the two processing stages can improve the ability of seismic data to delineate the geological details.

Screening of SSR Core Primers for Purity Identification of Pepper(Capsicum) Hybrids

[Objective] This study aimed to screen a set of SSR core primers suitable for purity identification of pepper （Capsicum） hybrids. [Method] DNA fingerprint of 100 pepper hybrids was analyzed using 17 SSR primers. [Result] According to the polymorphism and heterozygosity, Hpms1-214, Es395 and Hpmsl-5 were determined as three preferred core primers for purity identification of pepper hybrids. By using these three preferred core primers, 97 pepper hybrids （accounting for 97%） had heterozygous band pattern with at least one primer. Es330, Es363, Epms923, Es120 and Es64 were determined as candidate core primers for purity identification of pepper hybrids. Specific primers of 14 varieties were obtained, which could be used to further screen parent-complementary primers of each pepper hybrid. [Con- clusion] This study laid the foundation for constructing standard DNA fingerprints for purity identification of pepper hybrids.

Effect of nano TiN/Ti refiner on as-cast and hot-working microstructure of commercial purity aluminum

A novel type nano TiN/Ti composite grain refiner （TiN/Ti refiner） was prepared by high energy ball milling, and its effect on as-cast and hot-working microstructure of commercial purity aluminum （pure Al） was investigated. The results show that TiN/Ti refiner exhibits excellent grain refining performances on pure Al. With an addition of 0.2% TiN/Ti refiner, the average grain size of pure Al decreases to 82 μm, which is smaller than that of pure Ti and Al 5Ti 1B master alloy as refiners. The microstructure of weld joint of pure Al with 0.1% TiN/Ti refiner is fine equiaxed grains and the hardness of weld joint is higher than that of the base metal. For pure Al with 40% cold deformation and recrystallization at 250 °C for 1.0 h, the grains of the sample added 0.1% Ti powder have an obvious grain growth behavior. In contrast, oriented grains caused by deformation have been eliminated, and there is no obvious grain growth in pure Al refined with 0.1% TiN/Ti refiner, indicating that nano TiN in the refiner inhibits the growth of grain during recrystallization.

Identification of Genetic Purity of Bitter Gourd Hybrid by ISSR Markers

Objective] This study was conducted to verify the feasibiIity of ISSR marker for identifying genetic purity of bitter gourd hybrid, and thus to provide an effective method for seed purity test in production practices. [Method] The DNA fin-gerprints of a bitter gourd cuItivar Xiuyu 1 and its parents were analyzed using IS-SR marker with 91 primers. [Result] Two primers ISSR-845 and ISSR-891 which ampIified two DNA bands of 510 and 300 bp respectiveIy from F1 generation and its parents were screened out from 91 primers. ISSR-845 couId distinguish the male parent from F1 hybrid and the female parent, whiIe ISSR-891 couId distinguish the female parent inbred Iine from Xiuyu 1. Seed purity test with the specific markers gave the same resuIt with fiIed trials based on morphoIogical identification. [Conclu-sion] ISSR marker is an accurate, simpIe and effective method for seed purity test bitter gourd hybrid, and thus can be used in production practices.

Detection of Purity of Thai Hom Mali Rice by RAPD

[Objective] The aim was to establish more specific, sensitive, accurate and practical method to detect purity of Thai Hom Mali rice. [Method] RAPD method cooperated with two primers of KDML105 and RD15 was established by feeling for the extraction methods of DNA, optimizing concentrations of the factors influencing the results of RAPD such as template DNA, Mg2＋, random primer, dNTPs and Taq polymerase, and screening the random primers. [Result] The optimum RAPD reaction system was 25.0 μl in total volume, containing 4.0-32.0 ng/μl of template DNA, 200.0 μg/L random primer, 2.0 mmol/L Mg2＋, 200.0 μmol/L dNTPs and 1.0 U of Taq enzyme. Then, the Thai Hom Mali rice and non-Thai Hom Mali rice can be distinguished according to the presence or absence of two DNA markers. [Conclusion] The RAPD technology can effectively cover the shortages of identifications by sense and boiling in water; in addition, it is simple, sensitive and low-cost, suitable to be used in routine tests.

A High Purity Integer-N Frequency Synthesizer in 0.35μm SiGe BiCMOS

An integer-N frequency synthesizer in 0.35μm SiGe BiCMOS is presented. By implementing different building blocks with different types of devices,a high purity frequency synthesizer with excellent spur and phase noise performance has been realized. All the building blocks are implemented with differential topology except for the off-chip loop filter. To further reduce the phase noise,bonding wires are used to form the resonator in the LC-VCO. The frequency synthesizer operates from 2.39 to 2.72GHz with output power of about 0dBm. The measured closed-loop phase noise is - 95dBc/Hz at 100kHz offset and - 116dBc/Hz at 1MHz offset from the carrier. The power level of the reference spur is less than - 72dBc. With a 3V power supply, the whole chip including the output buffers consumes 60mA.

RAPD Appraisal of Purity of the Hybrid Rice SY63

使用纯度低或真实性差的杂交种子会给农业生产造成极大损失。然而杂交种子的纯度无法单纯从种子形态上鉴别．本文首次采用ＲＡＰＤ特异扩增谱带做为分子标记对水稻杂交种纯度进行了鉴定。汕优６３杂交水稻种子由中国水稻研究所从某制种单位随机取样获得。珍汕９７Ａ不育系和明恢６３恢复系等品种由中国水稻研究所提供。在做形态观察的同时，分别取上述三种材料叶片制备ＤＮＡ作为初始模板ＤＮＡ。对３００个ＲＡＰＤ随机引物，经过三次多态性初筛复筛，发现随机引物Ｐ１８可以稳定地扩增出一条来源于父本明恢６３的０．８ｋｂ的特异条带。用Ｐ１８引物对１００株汕优６３杂交单株进行ＲＡＰＤ扩增，其中８３个获得了０．８ｋｂ特异条带（Ｆｉｇ．１ｕｐｐｅｒ）。分子杂交证明其结果是可靠的（Ｆｉｇ．１Ｌｏｗｅｒ）。以ＲＡＰＤ扩增结果为依据，对这１００株材料进行植株形态比较，发现那１７个不能扩增出特异条带的单株均为假杂种。说明该制种单位汕优６３的假种率为１７％。大大超过农业部的有关规定。应对其原因和后果进行追究。用Ｐ１８引物对１８种分别为籼粳及其中间型的常用稻种进行ＲＡＰＤ扩增鉴定，除明恢６３的亲本──圭６３０和中间型Ｐｃｃｏｓ，Ａｕｓ３７３具有０．８ｋｂ的特异条带?

Purity Identification of Xinshikui 6 Using SSR Marker Technique

[Objective] SSR molecular marker technique was used to determine the purity of sunflower seed with the aim to provide accurate, convenient method for the identification of the purity of hybrid seeds in production and processing. [Method] With the DNA of Xinshikui 6 and its parents as template, about 100 pairs of SSR molecular markers were screened after DNA extraction, PCR amplification and electrophoresis production. [Results] SSR polymorphic primer marker 532 produced a specific band of 469 bp in the female parent, and a specific band of 451 bp in the male parent; primer marker 574 produced a specific band of 364 bp in the female parent, and a specific band of 384 bp in the male parent. The indoor molecular purity identification and field purity identification were consistent with each other. The primer marker 532 and 574 could be obtained from the SSR molecular marker method to distinguish the male parent, female parent and hybrid of Xinshikui 6, and both of the 2 primer markers can effectively identify the purities of the hybrid seeds of Xinshikui 6, as well as the authenticity of the seeds. [Conclusion] The proposed method was simple, fast, accurate to operate with the advantages of high reproducibility, and it had become the major method in the identification of sunflower varieties.

Effect of indentation size and grain/sub-grain size on microhardness of high purity tungsten

Hardness of materials depends significantly on the indentation size and grain/sub-grain size via microindentation and nanoindentation tests of high-purity tungsten with different structures.The grain boundary effect and indentation size effect were explored.The indentation hardness was fitted using the Nix-Gao model by considering the scaling factor.The results show that the scaling factor is barely correlated with the grain/sub-grain size.The interaction between the plastically deformed zone（PDZ） boundary and the grain/sub-grain boundary is believed to be the reason that leads to an increase of the measured hardness at the specific depths.Results also indicate that the area of the PDZ is barely correlated with the grain/sub-grain size,and the indentation hardness starts to stabilize once the PDZ expands to the dimension of an individual grain/sub-grain.

Synthesis of High Purity SiC Powder for High-resistivity SiC Single Crystals Growth

High purity silicon carbide （SIC） powder was synthesized in-situ by chemical reaction between silicon and carbon powder. In order to ensure that the impurity concentration of the resulting SiC powder is suitable for high-resistivity SiC single crystal growth, the preparation technology of SiC powder is different from that of SiC ceramic. The influence of the shape and size of carbon particles on the morphology and phase composition of the obtained SiC powder were discussed. The phase composition and morphology of the products were investigated by X-ray diffraction, Raman microspectroscopy and scanning electron microscopy. The results show that the composition of resulting SiC by in-situ synthesis from Si/C mixture strongly depends on the nature of the carbon source, which corresponds to the particle size and shape, as well as the preparation temperature. In the experimental conditions, flake graphite is more suitable for the synthesis of SiC powder than activated carbon because of its relatively smaller particle size and flake shape, which make the conversion more complete. The major phase composition of the full conversion products is β-SiC, with traces of α-SiC. Glow discharge mass spectroscopy measurements indicated that SiC powder synthesized with this chemical reaction method can meet the purity demand for the growth of high-resistivity SiC single crystals.

Modification Behavior of Trace Rare Earth on Impurity Phases in Commercial Purity Aluminum

Modifying effect and mechanism of trace rare earth on Fe(Si) rich impurity phases in commercial purity aluminum were studied with the aids of SEM, EDAX, TEM, etc. It is found that Ce rich mixed rare earth (RE) is an effective modifying agent, which makes the coarse Fe rich impurity phases transform into complex compounds of tiny, sphere/short stick form, thus improving mechanical properties of this material; its modifying mechanism is in that RE gathering in front of solid/liquid interface enters into the impurity phases, forming complex (AlFeSiRE) compounds; or is adsorbed in the impurity phases surface, impeding the growth of impurity phases; however, excessive RE will result in the increasing of RE compounds (secondary phases), and plasticity reduction of this material. Therefore, its addition amount should be less than 0 07% (mass fraction).