ICP-AES测定金属钯中的杂质

建立了电感耦合等离子体发射光谱(ICP-AES)，同时测定金属钯中Ag、Al、As、Au、Bi、Ca、Co、Cr、Cu、Fe、Ir、Mg、Mn、Mo、Ni、Pb、Pt、Rh、Ru、Sb、Si、Sn、Ti、Zn等杂质含量的方法。方法简便、快速、准确。各杂质的测定精密度在0．25％-3．0％之间，检出限在0．020-0．062(μg／g)之间，回收率在85％～100％之间。     

火焰原子吸收光谱法测定铜镍矿浮选产品中铜、镍、镁

研究了用火焰原子吸收光谱法在同一溶液体系中直接快速测定金川铜镍矿浮选产品中铜、镍、镁含量新的新方法。考察了产品中高含量的SiO2对测定镁的干扰情况，并提出了排除这项干扰简便方法，根据各元素的标准溶液系列的测定数据，推算出了铜、镍、镁3元素的线性回归方程及线性相关系数，特征浓度铜为0．40mg.L^-1/1%，镍为0．48mg.L^-1／1％，Mg为0．018mg.L^-1／1％；线性浓度范围铜，镍均为0－10mg.L^-1，镁为0．2－1．2mg.L^-1。相对标准偏差铜为2．5％(n=6)，镍为2．3％（n＝6），镁为2．8％（n=6），加标回收率铜为96．5％－102．5％，镍为98．8％－103．5％，镁为98．2％－102．5％，这种方法操作简便，快速，实用，具有较好的精密度和准确度，实际产品分析结果与外检单位及金川公司测定的结果吻合。     

分子筛和担体中主含量元素和杂质元素的同时测定

本文研究了用微波消化试样，ICP－AES法同时测定分子筛及担体中的主含量元素Si、Al和杂质元素Fe、Na、Ca、Mg的方法。相对标准偏差：Si、Al＜2％，Fe、Na、Ca、Mg≤4％，杂质元素回收率为97％－107％。方法快速，简便、准确，可靠。     

等离子体发射光谱法测定铝合金中的杂质元素

本文利用高频电感耦合等离子体光谱仪直接测定铝合金中的Fe,Zn,Mg,Mn,Ti,Cr和Cu杂质元素。选择了合适的实验条件,采用背景扣除法进行校正。方法简便、快速,可靠,具有良好的精密度和准确度。相对标准偏差为1．7％－6．3％,回收率为94％－105％。     

ICP—AES法测定U3O8标样中Al、Cr、Fe、Mg、P、Pb、Ti、V、W

用7402季铵－Kel-F粉萃取色层使铀和待测杂质元素分离，接着用975型ICP光量计测定U3O8标样中Al、Cr、Fe、Mg、P、Pb、Ti、V、W，回收率为95－110％，相对标准偏差≤5％。     

ICP-OES测定奶花芸豆中的微量元素

采用ICP-OES同时测定奶花芸豆样品中的Al、Ba、Ca、Cu、Fe、Mg、Mn、Mo、Ni、Sr、Zn、K、P 13种微量元素,结果表明,奶花芸豆中富含K、Mg、Ca、P.检测结果精密度与准确度良好,加标回收率在92.0％-106％之间,相对标准偏差均在5％以内.该法能够用于奶花芸豆中微量元素的快速、准确测定.     

ICP-AES测定钾混盐中的钾、钠、钙、镁和硫酸根

用蒸馏水溶解盐湖钾混盐矿,电感耦合等离子体原子发射光谱法同时测定K＋、Na＋、Ca2＋、Mg2＋、SO42-.方法检出限：K＋2.4mg/L Na＋ 4.8mg/L、Ca2＋2.4mg/L、Mg2＋2.4mg/L、SO42-7.2mg/L.方法精密度（RSD,n=10）：K＋ 1.23％、Na＋0.87％、Ca2＋ 3.15％、Mg2＋3.02％、SO42-2.28％.加标回收率：K＋101.8％、Na＋ 103.2％、Ca2＋ 98.20％、Mg2＋ 104.8％、SO42-96.80％.     

盐酸环丙沙星含量测定方法的研究

本文介绍了盐酸环丙沙星含量测定的离子选择电极法，紫外分光光度法和格兰线性滴定三种不同方法。用于原料药回收率的测定分别为９９．４％，９９．６７％和９９．５％；用于片剂回收率测定分别为９８．８５％，９８．８４％和９８．７３％。结果基本相同，与非水滴定法相比具有测试方便、快速等优点。     

不同季节的虎杖根茎中8种矿质元素的光谱测定

采用空气-乙炔火焰原子吸收法,测定虎杖根茎的K,Ca,Na,Mg,Fe,zn,Mn,Cu等8种矿质元素的含量。对测定条件进行了实验,选择了最佳电离抑制剂和酸性介质。实验以氯化铯为电离抑制剂,盐酸浓度控制在2％以内,用氯化锶消除磷对Ca的干扰,使吸光值稳定,用标准曲线法进行测定,获得了满意效果。该方法简单、快速、准确,加标回收率为90．5％～108．2％,相对偏差为0．3％～0．7％,适合于植物矿质元素的分析。实验结果表明：虎杖根茎中含有丰富的矿质元素,其中以K,Ca元素含量最高。这与虎杖的药用效果相符。同时,每种元素含量随季节变化而变化,与其生长发育密切相关。     

ICP-AES法测定水中微量磷

用ICP－AES法测定水中磷，并确定了最佳测定条件，检出限为0．02μg.mL^-1，回收率为96．5％－102．1％，RSD为1．65％－2．83％。该法准确、快速、简便，应用于水中磷的测定，结果令人满意。     

Acid Interferences in Indirect Determination of Silicon bt Atomic Absorption Spectroscopy (AAS)

Although silicon may be determined directly by AAS using a nitrous oxide - acetylene flame, there have been reported procedures for its indirect determination based on interference with other elements, mostly strontium, magnesium, calcium and barium.     

Optical properties of multilayer materials based on silicon and nanosized magnesium silicide crystallites

We have studied the optical properties of silicon with incorporated nanocrystallites of semiconducting magnesium silicide by optical spectroscopy and Raman spectroscopy. We have calculated the optical functions of samples grown with different numbers of layers of incorporated magnesium silicide nanocrystallites. We have determined the contribution of magnesium silicide to the electronic structure of multilayer samples in the photon energy range 1.5–3.0 eV. We have studied the phonon structure of the grown multilayer samples, based on analysis of two-phonon and three-phonon resonances in silicon and Mg₂Si. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 2, pp. 204–209, March–April, 2006.     

原子发射光谱法直接测定焦炭中的15种微量杂质元素

采用原子发射光谱直接测定了焦炭中Si、Mn、Mg、Pb、Sn、Fe、Ni、Al、Ti、Mo、Ca、V、Cu、Zn、Ag等15种微量杂质元素。方法不需要高温灰化及冗长的样品前处理技术,直接粉末进样分析,操作简便、快速,能够满足焦炭中常规杂质分析的需要。     

Pulsed nanosecond annealing of magnesium-implanted silicon

Single-crystalline silicon is implanted by magnesium ions at room temperature and then subjected to pulsed ion-beam annealing. The surface morphology, crystallinity, and optical properties of the implanted silicon are studied before and after annealing. It is shown that ion implantation makes a near-surface layer of silicon about 0.1 m thick amorphous. Pulsed nanosecond ion-beam annealing results in silicon recrystallization and the formation of crystalline magnesium silicide precipitates. Optimal values of the implantation dose and pulse energy density for the formation of magnesium silicide precipitates in the near-surface layer of silicon are found.     

Phase identification of microfeatures using EPMA methods,especially high-resolution X-ray spectroscopy

Methods of electron-probe microanalysis (EPMA), with some input from scanning and transmission electron microscopy (SEM/TEM), are applied for the identification of micro-scale constituents in a solid matrix. The subject of the study is a magnesium alloy composite, which contains silicon carbide-based fibres made by a liquid metal infiltration process. Backscattered electron imaging of the composite in the SEM showed that during composite manufacture, fibres were chemically attacked by the metal, many of the fibres exhibiting three distinct grey levels, indicative of different reaction zones, and others appearing uniformly black. EPMA measurements showed that each region contained ∼12 wt.% oxygen and that penetration of the fibre by magnesium was accompanied by a reduction in the concentration of silicon and carbon. From studying the position and shape of specific X-ray lines it was shown that magnesium penetration involved a chemical reaction with silicon oxycarbide, established in earlier EPMA studies as one of the fibre constituents. Also, in the outermost region, aluminium in the alloy reacted with free carbon in the fibre to form aluminium carbide and with magnesium to produce a Mg–Al intermetallic. The composition of black fibres was quite different from the grey ones, with negligible silicon and only a small amount of aluminium. Oxygen levels in black fibres were consistent with complete oxidation, indicating these fibres were subjected, locally, to severe oxidising conditions during composite manufacture. In the metal matrix itself, particles of a mixed magnesium/aluminium oxide, silicon carbide and magnesium silicide were observed, the latter two phases forming as silicon and carbon were ejected from fibres.     

氧弹燃烧灰化分光光度法测定有机物中的硅

采用氧弹燃烧灰化进行样品预处理 ,亚铁还原硅钼蓝分光光度法测定有机物中微量硅。通过试样分析和回收率实验 ,结果表明 ,方法的回收率为 95 %— 10 2 % ,可用于有机样品中硅的定量测定。     

Effects of magnesium film thickness and annealing temperature on formation of Mg2Si films on silicon (1 1 1) substrate deposited by magnetron sputtering

Magnesium films of various thicknesses were first deposited on silicon (1 1 1) substrates by magnetron sputtering method and then annealed in annealing furnace filled with argon gas. The effects of the magnesium film thickness and the annealing temperature on the formation of Mg₂Si films were investigated by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The Mg₂Si thin films thus obtained were found to be polycrystalline and the Mg₂Si (2 2 0) orientation is preferred regardless of the magnesium film thickness and annealing temperature. XRD results indicate that high quality magnesium silicide films are produced if the magnesium/silicon samples are annealed at 400 °C for 5 h. Otherwise, the synthesized films annealed at annealing temperatures lower than 350 °C or higher than 450 °C contain magnesium crystallites or magnesium oxide. SEM images have revealed that microstructure grains in the polycrystalline films are about 1-5 μm in dimensions, and the texture of the Mg₂Si films becomes denser and more homogeneous as the thickness of the magnesium film increases.     

Laser-induced implantation and diffusion of magnesium into silicon

Laser-induced diffusion (“implantation”) of magnesium atoms into silicon was studied experimentally. Neodymium-glass laser irradiation (λ=1.06 μm, τ ∼ 0.4 ms) was found to increase the diffusion coefficient and solubility of magnesium in silicon. Current-voltage and capacity-voltage characteristics, as well as thermostimulated current spectra of 〈Si + Mg〉 crystals, were obtained.     

胶磷矿中杂质赋存形式及酸解过程变化

我国中低品位胶磷矿量大、分布广,磷矿中杂质种类及含量对于磷石膏结晶及磷酸品质均有较大影响。以湖北某地区的典型低品位胶磷矿为原料,采用X射线光电子能谱仪、扫描电镜、能谱等方法,分析了磷矿及反应后磷石膏中的主要杂质种类及含量变化,并以此推测湿法磷酸过程中杂质的主要变化。结果表明磷矿中的主要成分是氟磷灰石和石英,杂质组分占比最高的分别是硅、铝、氟、镁,其中硅主要以石英和硅酸钙存在,氟主要存在于氟磷酸钙中,铝是以不同形式的铝硅酸盐存在的,而镁则是以MgF₂和部分硅酸盐存在。通过酸解反应,钙与硫酸根生成磷石膏,硅元素主要存在于固相石膏中,而铝、氟、镁则大部分进入到液相磷酸中,其中存在于固相中的硅则基本以石英形式存在,硅酸钙溶解于酸液中,铝主要以铝硅磷的化合物存在,氟则以氟硅化物形式存在,大部分的MgF₂溶解进入液相,磷石膏中镁主要以镁硅酸盐形式存在。通过磷矿中杂质存在形式及反应过程的变化研究,可以更好的明晰酸解过程中的体系变化,从而为磷石膏结晶过程的考察和控制提供理论基础。     

P掺杂单壁硅纳米管Mg原子吸附性能的第一性原理研究

采用密度泛函理论的广义梯度近似和平面波赝势方法,研究P掺杂单壁硅纳米管对Mg原子的吸附性能.计算本征、掺杂P、施加形变作用（压缩和拉伸）的（6,6）硅纳米管外壁对Mg原子的吸附能,分析掺杂P前后的成键情况及电荷布局数.结果表明,掺杂P使体系形成Mg-P和Si-P间的离子性键,增强了Si-Si间的离子性键,P掺杂硅纳米管超晶格中离子键与共价键共存;掺杂P后显著提高了硅纳米管外壁对Mg原子的吸附能力;硅纳米管外壁对Mg原子的吸附能在0.25%,0.50%,1.00%,1.25%的压缩量和1.00%,1.25%的拉伸量时增大,可显著增强硅纳米管材料作为增强相时与基体界面间结合的粘附性.