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首页> 外文期刊>Spectrochimica Acta, Part B. Atomic Spectroscopy >Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry
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Direct determination of trace elements in boron nitride powders by slurry sampling total reflection X-ray fluorescence spectrometry

机译:浆料采样全反射X射线荧光光谱法直接测定氮化硼粉末中的痕量元素

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摘要

The use of slurry sampling total reflection X-ray fluorescence spectrometry (S1S-TXRF) for the direct determination of Ca, Cr, Cu, Fe, Mn and Ti in four boron nitride powders has been described. Measurements of the zeta potential showed that slurries with good stabilities can be obtained by the addition of polyethylenimine (PEI) at a concentration of 0.1 wt.% and by adjusting the pH at 4. For the optimization of the concentration of boron nitride in the slurries the net line intensities and the signal to background ratios were determined for the trace elements Ca and Ti as well as for the internal standard element Ga in the case of concentrations of boron nitride ranging from 1 to 30 mg mL~(-1). As a compromise with respect to high net line intensities and high signal to background ratios, concentrations of 5 mg mL~(-1) of boron nitride were found suitable and were used for all further measurements. The limits of detection of S1S-TXRF for the boron nitride powders were found to range from 0.062 to 1.6 μg g~(-1) for Cu and Ca, respectively. Herewith, they are higher than those obtained in solid sampling and slurry sampling graphite furnace atomic absorption spectrometry (SoS-GFAAS, S1S-GFAAS) as well as those of solid sampling electrothermal evaporation inductively coupled plasma optical emission spectrometry (SoS-ETV-ICP-OES). For Ca and Fe as well as for Cu and Fe, however, they were found to be lower than for GFAAS and for ICP-OES subsequent to wet chemical digestion, respectively. The universal applicability of S1S-TXRF to the analysis of samples with a wide variety of matrices could be demonstrated by the analysis of certified reference materials such as SiC, Al2O3, powdered bovine liver and borate ore with a single calibration. The correlation coefficients of the plots for the values found for Ca, Fe and Ti by S1S-TXRF in the boron nitride powders as well as in the before mentioned samples versus the reference values for the respective samples over a concentration range from 2.5 to 1470 μg g~(-1) were found to be 0.995, 0.991 and 0.997, respectively.
机译:已描述了使用浆料采样全反射X射线荧光光谱法(S1S-TXRF)直接测定四种氮化硼粉末中的Ca,Cr,Cu,Fe,Mn和Ti。 ζ电势的测量表明,可以通过添加浓度为0.1 wt。%的聚乙烯亚胺(PEI)并将pH值调整为4来获得具有良好稳定性的浆液。为了优化浆液中氮化硼的浓度在氮化硼浓度为1至30 mg mL〜(-1)的情况下,测定了痕量元素Ca和Ti以及内标元素Ga的净线强度和信噪比。作为对高净线强度和高信噪比的折衷,发现浓度为5 mg mL〜(-1)的氮化硼适用于所有进一步的测量。发现氮化硼粉末的S1S-TXRF的检出限分别为Cu和Ca在0.062至1.6μgg〜(-1)之间。因此,它们比固体采样和泥浆采样石墨炉原子吸收光谱法(SoS-GFAAS,S1S-GFAAS)以及固体采样电热蒸发电感耦合等离子体发射光谱法(SoS-ETV-ICP- OES)。但是,对于钙和铁以及铜和铁,发现它们分别低于湿化学消化后的GFAAS和ICP-OES。通过对SiC,Al2O3,牛肝粉和硼酸盐矿石等经过认证的参考材料进行单次校准分析,可以证明S1S-TXRF在各种基质样品分析中的普遍适用性。在2.5到1470μg的浓度范围内,氮化硼粉末以及上述样品中S1S-TXRF测得的Ca,Fe和Ti值的图的相关系数与各个样品的参考值的相关系数g〜(-1)分别为0.995、0.991和0.997。

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