用质子诱导伽马射线发射、全反射x射线荧光和仪器中子活化分析测定石墨中的杂质

M. Ghosh, T. Chavan, G. Reddy, Remya Devi P.S, S. Kumar, K. K. Swain
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摘要

石墨中杂质的测定对石墨的质量控制非常重要,因为在各种应用中,即使微量杂质的存在也会影响石墨的性能。当量硼含量(EBC)小于5mg kg-1的石墨被认为是核级石墨。具有高中子吸收截面的元素(硼和稀土)对EBC有显著贡献。非破坏性方法是优选的,因为没有样品处理和消解时挥发性元素损失的可能性。质子诱导伽马射线发射(PIGE)和仪器中子活化分析(INAA)用于核级和商业级石墨中杂质的无损测定。石墨中的低Z元素Li、B、F、Na、Al、Si用PIGE法检测,Na、K、Sc、Cr、Mn、Fe、Co、Zn、Rb、Zr、Sb、Cs、La、Ce、Nd、Sm、Eu、Tb、Yb、Hf、Ta、Th用INAA法检测。Ca、Ti、V、Ni、Sr和Pb等元素在两种无损检测方法中均未被检测到。石墨样品经干法灰化消解后,用全反射x射线荧光(TXRF)测定了这些元素。这些技术的组合被用来获得关于石墨中存在的杂质的最大信息。图形抽象
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Determination of Impurities in Graphite Using Proton Induced Gamma Ray Emission, Total Reflection X-ray Fluorescence and Instrumental Neutron Activation Analysis
Abstract Determination of impurities in graphite is very important for its quality control, as their presence even at trace level can affect the performance of graphite in various applications. Graphite with equivalent boron content (EBC) less than 5 mg kg-1 is considered as nuclear grade. Elements with high neutron absorption cross section (boron and rare earths) contribute significantly to EBC. Non-destructive method is preferred as there is no sample processing and probability of loss of volatile elements while digestion. Proton Induced Gamma Ray Emission (PIGE), Instrumental Neutron Activation Analysis (INAA) were utilized for the non-destructive determination of impurities in both nuclear and commercial grade graphite. Low Z elements like Li, B, F, Na, Al and Si were detected in graphite by PIGE whereas Na, K, Sc, Cr, Mn, Fe, Co, Zn, Rb, Zr, Sb, Cs, La, Ce, Nd, Sm, Eu, Tb, Yb, Hf, Ta, Th were determined using INAA. Few elements like Ca, Ti, V, Ni, Sr and Pb remained undetected by both the non-destructive techniques. These elements were determined by Total Reflection X-ray Fluorescence (TXRF) after digestion of the graphite samples by dry ashing. Combinations of these techniques were utilized to get maximum information regarding the impurities present in graphite. GRAPHICAL ABSTRACT
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