等离子体质谱法测定地质样品中痕量稀土元素的基体效应 …

采用模拟地质样品中稀土元素间天然组成比的基体匹配校正标准溶液进行外标校正,有效地抑制了地质样品分析中的基体效应,以＾１１５Ｉｎ－＾１０３Ｒｈ双内标元素校正,监控和校正分析信号的短期和长期漂移;通过单个稀土元素及钡的氧化物,氢氧化物的测定计算出等效的干扰浓度,进而校正了稀土元素分析中多原子离子干扰。建立了地质样吕吕痕量稀土元素测定中基体效应及多原子离子干扰的校正方法。通过对５个标准参考物质的分析,定     

电感耦合等离子体质谱法(ICP-MS)测定高纯氧化铒中稀土杂质

从同位素的选择、基体效应,内标元素的选择及仪器工作条件等方面对实验参数进行了优化,重点研究了等离子体功率及仪器分辨率的改变对铒基体所形成的氢化物多原子离子干扰的影响。通过提高等离子体功率、改变仪器分辨率及数学方程校正等方法,减少和剔除了ErH对Ho和Tm测定的干扰。实验中选取Cs为内标元素,测定了不同含量的高纯氧化铒样品。分析结果与标准加入法结果进行了比较,之间无显著性差异。     

高纯氧化钇电感耦合等离子体原子发射光谱分析中的校正因子法初步研究

本文提出用校正因子法补偿基体效应对待测元素谱线强度的影响。考察了ICP工作参数对校正因子的影响,在优化的条件下,14个稀土元素的校正因子值为1.10～1.40,其波动系数<7.5％。对高纯氧化钇试样进行了分析,并将所得结果同基体匹配法作了比较,分析误差基本符合痕量分析要求。本法的优点是省去了基体匹配,这对高纯稀土分析有一定参考价值。     

电感耦合等离子体质谱准确测定单斜辉石中稀土元素

采用密闭酸溶ICP-MS研究了单斜辉石中稀土元素准确分析方法.以基体匹配的混合标准溶液为外标校正溶液;利用115In-103Rh双内标校正系统;并通过单个稀土元素及钡的氧化物、氢氧化物的测定,计算出等效干扰浓度进行校正,从而有效地抑制了分析信号的漂移、基体效应及多原子离子干扰.通过对4个标准参考物质的分析,测定结果与推荐值一致.该法应用于4个单斜辉石样品分析,方法检出限为0.7～2.5 ng·L-1,RSD≤10%(n=5).     

电感耦合等离子体质谱法测定高纯铁中21种元素时的基体效应北大核心CSCD

对用电感耦合等离子体质谱法测定纯铁中21种元素(包括Li、Be、B、Al、Ti、Mn、Co、Ni、Cu、Zn等),通过加入高纯铁作为基体,试验考察了不同量的铁基体对上述被测元素的信号强度的影响。结果发现:铁基体质量浓度在40mg·L^(-1)以内时,待测元素的相对信号强度与铁基体浓度保持较好的线性关系;当铁基体质量浓度增大至400mg·L^(-1)时,除了Mn、Co两元素外,铁基体对其他待测元素均产生一定的抑制作用。基于对内标元素的基体效应分析,选择与待测元素有相似基体效应的内标元素,以校正基体效应。     

等离子体质谱法测定地质样品中痕量稀土元素的基体效应及多原子离子干扰的校正研究

采用模拟地质样品中稀土元素间天然组成比的基体匹配校正标准溶液进行外标校正,有效地抑制了地质样品分析中的基体效应;以¹¹⁵In-¹⁰³Rh双内标元素校正,监控和校正分析信号的短期和长期漂移;通过单个稀土元素及钡的氧化物、氢氧化物的测定计算出等效的干扰浓度,进而校正了稀土元素分析中多原子离子干扰.建立了地质样品中痕量稀土元素测定中基体效应及多原子离子干扰的校正方法,通过对5个标准参考物质的分析,定量测定限为0.0090.133μg·g^-1,RSD小于5%.     

用电感耦合等离子体质谱法测定高纯稀土中稀土杂质时的基体影响

考察了基体对待测稀土杂质元素信号的影响，研究了内标对基体效应的补偿作用。对于不同的基体元素最佳的内标元素是不一致的，Ｇａ、Ｉｎ、Ｉ、Ｃｓ和Ｔｌ是稀土纯度分析中合适的内标元素。内标法简便易行，效果好，其测定方法的精度和回收率令人满意。     

流动注射-电感耦合等离子体发射光谱联用技术研究——Ⅳ.痕量钪的快速测定

本文提出了用流动注射-电感耦合等离子体发射光谱(FIA-ICP-AES)测定工艺流程Sc试液中痕量钪的新方法。考察了基体Fe和Ti的光谱干扰;对常规进样和FIA进样中的基体效应进行了比较。当采用0.5ml体积进样,以Sc 363.075nm为分析线,Sc的检出限为8.4ng/ml,R.S.D.为2.5％。此法可以直接用于基体浓度在Fe≤30mg/ml和Ti≤10mg/ml范围内痕量钪的测定,而无需分离基体或在标样和试样之间进行基体浓度匹配。本法分析速度快(90个样/小时)、操作简便和精密度好,可以作为工艺流程中测定痕量Sc的快速的分析方法。     

ICP-AES内标法测定分子筛的组成

首次通过ICP-AES仪研究了分子筛化学组成全分析的方法，采用HNO3-HF混合酸密闭溶样，用H3BO3配合F^-，分别采用内标法和基体消除法消除基体效应．将研究结果与经典方法比较表明：采用本文研究的分析方法，结果准确可靠，符合分析要求，尤其对杂原子分子筛以及金属氧化物修饰的分子筛的组成分析具有应用价值．     

电感耦合等离子体发射光谱法测定锌铝镁合金中铝、镁含量

采用基体匹配法绘制校准曲线和镧元素作内标校正来消除基体效应和仪器漂移的影响,建立了电感耦合等离子体发射光谱仪测定锌铝镁合金中铝、镁元素的分析方法.将方法应用于锌铝镁合金试样的测定,结果的相对标准偏差(RSD)在0.86％～2.13％之间,加标回收率为96.4％～99.6％.并与化学分析方法进行了比对,两种方法测定值吻合...     

一种用于电热蒸发-原子光谱的微型化固相萃取技术

与传统的液 液萃取相比 ,固 液萃取技术具有省时、溶剂用量少、不易乳化和高富集因子等优点[1],它可与各种检测方法联用[2 ],已在痕量无机物或有机物的分离富集与测定中广泛应用 .但是常规的固相萃取中的洗脱过程存在洗脱体积大 ,时间长及要求二次处理等缺点 ,这与电热蒸发 (ＥＴＶ)进样 /电感耦合等离子体原子发射光谱 /质谱 (ＩＣＰ ＡＥＳ/ＭＳ)和电热原子吸收光谱 (ＥＴＡＡＳ)很不匹配 .基于此 ,本文设计了一种填充有Ｐ5 0 7萃淋树脂 ( 1 40目 )的超微柱 ( 0 6μｍ(ｉ.ｄ .)× 1 0ｍｍ) .它既可用作分离富集柱 ,又可作为ＥＴＶ ＩＣＰ…     

高纯氧化钬的电感耦合等离子体原子发射光谱分析及光谱干扰的校正

本文提出了以PGS-2型平面光栅摄谱仪与Plasma Therm ICP-5000D射频发生器联用,乙醇溶液预去溶进样方法,直接同时测定高纯氧化钬中5个稀土杂质元素的方法,并讨论了基体浓度对分析方法检出限的影响和光谱干扰及其校正。当样品溶液中稀土总浓度为5mg/ml时,测定下限分别为铽0.003％,镝、铒和铥0.002％,钇0.0003％。其相对标准偏差为2.8％～7.4％。     

溶胶-凝胶法制备的Y_2O_3薄膜的光波导性质研究

用醋酸钇溶解于甲氧基乙醇的溶胶 凝胶法制备了Y2 O3光波导薄膜。通过二乙烯三胺的络合作用 ,获得了均匀和稳定的前驱液 ,并用浸渍提拉法得到了薄膜。差热分析、红外吸收光谱被用来表征Y2 O3凝胶和粉末。用XRD、扫描电子显微镜、m线法和波导荧光光谱法研究了Y2 O3光波导薄膜的结构和光波导性质。结果表明 ,Y2 O3薄膜对于光活性掺杂是一种很好的基质材料 ,预示Y2 O3薄膜在光电子方面具有巨大的应用前景。     

Determination of yttrium, scandium and other rare earth elements in uranium-rich geological materials by ICP-AES

A rapid method is described for the determination of yttrium, scandium, and other rare earth elements (REEs) in uranium-rich geological samples (containing more than 0.1% U) and in pitch blende type of samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) after separation of uranium by selective precipitation of the analytes as hydroxides using H(2)O(2)/NaOH in the presence of iron as carrier. Uranium goes into solution as soluble peruranate complex. The precipitated rare earth hydroxides (including Y and Sc) are filtered and dissolved in hydrochloric acid prior to their aspiration into plasma for their individual estimation after selecting interference free REE emission lines. The method has also been applied to some international reference standards like SY-2 and SY-3 (by doping a known amount of uranium) along with one in-house pitch blende sample and the REE values were found to be in agreement with the most usable values, offering an R.S.D. of 1-8.8% for all the REEs', Y and Sc. The method compared well, with the well- established cation exchange separation procedure.     

Synthesis and structure of tridentate bis(phosphinic amide)-phosphine oxide complexes of yttrium nitrate. Applications of 31P,89Y NMR methods in structural elucidation in solution

The synthesis and characterisation of a tridentate ligand containing two diphenylphosphinic amide side-arms connected through the ortho position to a phenylphosphine oxide moiety and the 1:1 and 2:1 complexes formed with yttrium nitrate are reported for the first time. The free ligand (R(P1)*,S(P3)*)-11 is obtained diastereoselectively by reaction of ortho-lithiated N,N-diisopropyl-P,P-diphenylphosphinic amide with phenylphosphonic dichloride. Complexes [Y((R(P1)*,S(P3)*)-11)(NO(3))(3)] and [Y((R(P1)*,S(P3)*)-11)(2)(NO(3))](NO(3))(2) were isolated by mixing ligand 11 with Y(NO(3))(3)·6H(2)O in acetonitrile at room temperature in a ligand to metal molar ratio of 1:1 and 2:1, respectively. The 1:1 derivative is the product of thermodynamic control when a molar ratio of ligand to yttrium salt of 1:1 is used. The new compounds have been characterised both as the solid (X-ray diffraction) and in solution (multinuclear magnetic resonance). In both yttrium complexes the ligand acts as a tridentate chelate. The arrangement of the two ligands in the 2:1 complex affords a pseudo-meso structure. Tridentate chelation of yttrium(III) in both complexes is retained in solution as evidenced by (89)Y NMR data obtained via(31)P,(89)Y-HMQC, and (89)Y,(31)P-DEPT experiments. The investigation of the solution behaviour of the Y(III) complexes through PGSE NMR diffusion measurements showed that average structures in agreement with the 1:1 and 1:2 stoichiometries are retained in acetonitrile.     

Use of a single calibration graph for the determination of major elements in geological materials by laser ablation inductively coupled plasma atomic emission spectrometry with added internal standards

The possibility of internal standardisation in laser ablation inductively coupled plasma atomic emission spectrometry (LA-ICP-AES) of geological materials by added Sc₂O₃ and Y₂O₃ has been examined to cover the wide range of concentrations of major and minor constituents both in silicate rocks and limestones. A Nd?:?YAG laser (355 nm, 10 Hz, 10 mJ per shot) was used for the ablation of discs obtained by fusion of the mixture of samples and oxides of Sc and Y with lithium tetraborate. The flux/sample ratio was in the range from 6 to 10. The contents of analytes were within the concentration range from hundredths to tens of percentage. The trace elements copper and nickel were studied, too. An ICP emission spectrometer OPTIMA 3000 DV was used for the measurement of Si, Al, Ca, Mg, Sr, Ba, Fe, Ti, Mn, Ni, Cu, Na and K analyte lines and Y and Sc reference lines in the axial observation mode. The long-term and the short-term repeatability of measurement were improved by employing scandium or yttrium internal references lines for the above analytes from 6% to 1.5% of RSD and from 2.4% to 1.0% of RSD, respectively. The correlation of signals with concentrations was improved in terms of the correlation coefficient r from 0.90–0.97 to 0.98–0.998 and the relative uncertainity on the centroid of concentrations was improved 2–3 times. A single calibration graph covering the concentration range both in silicates and carbonates is possible for each of elements, as the matrix effects are compensated for by internal standards and the excess of Li₂B₄O₇.     

Determination of impurity elements in high-purity solid precursors based on tantalum pentoxide by inductively coupled plasma mass spectrometry

Conditions for the inductively coupled plasma mass-spectrometric (ICP MS) analysis of high-purity tantalum pentoxide and tantalum pentoxide doped with rare-earth elements without the separation of a sample matrix from analytes (Mg, Al, Si, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zr, Nb, Mo, Sn, W, Gd, Dy, Er, and Pb) were determined. The metrological parameters of ICP MS analysis (accuracy, precision, and detection limits) were calculated. It was established that, in the analysis of test sample solutions with tantalum concentrations higher than 30 mg/L, a matrix effect appeared: the intensity of the measured ion current of analytes decreased against the background of a high concentration of sample matrix (tantalum) ions. This caused a proportional underestimation of the results of analysis. It was shown that it is reasonable to plot calibration functions against the background of a solution containing no more than 30 mg/L of tantalum ions. The results of the ICP MS analysis were compared with X-ray fluorescence (XRF) and optical emission spectrometry (OES) analysis data and calculation data on the amounts of admixtures introduced into tantalum pentoxide at the stage of the extraction preparation of a precursor.     

Using of Fractional Separation for the Analysis of MoO<Subscript>3</Subscript> by Atomic Emission Spectrometry with Inductively Coupled Plasma and Electrothermal Vaporization

The introduction of various forms of molybdenum into an inductively coupled plasma was studied in the vaporization of solutions from a graphite tube. A temperature program is selected that enables the separated vaporization of analytes and molybdenum (matrix) for atomic emission spectrometry with inductively coupled plasma and electrothermal vapoization (ETV–ICP–AES) analysis. The limits of detection for analytes in the ETV–ICP–AES analysis of molybdenum trioxide are evaluated using the fractional separation of analytes and the matrix.     

Nanocrystalline and mesostructured Y2(O3) as supports for gold catalysts

The structure of yttrium oxide influences the CO oxidation activity of Au/Y2(O3) catalysts; nanocrystalline Y2(O3) stabilizes more active species of gold and increases the activity of the gold catalyst in comparison with mesostructured and precipitated Y2(O3).     

Controllable synthesis of Y2O3 microstructures for application in cataluminescence gas sensing

Y(2)O(3) dumbbells, microspheres, and nanosheets were synthesized by a facile hydrothermal procedure followed by calcination. Electron microscopy, X-ray diffraction, and N(2) adsorption measurements were used to characterize the yttrium oxide microstructures. On the basis of a time-dependent study of nanostructure evolution and the effect of other processing parameters, a kinetic "homogeneous nucleation-self assembly-anisotropic growth" mechanism is proposed to explain the growth of these microstructures under hydrothermal conditions. The sensitivity of as-prepared Y(2)O(3) structures to a series of gaseous chemicals was examined by using a homemade cataluminescence sensing system. The designed cataluminescence sensor based on the yttrium oxide dumbbells shows good sensing performance for 16 common volatile organic compounds.