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Determination of Trace Elements in High Purity Tungsten by Solid-Phase Extraction/ICP-MS

机译:固相萃取/ ICP-MS测定高纯钨中的痕量元素

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To establish a rapid trace-quantification scheme for elements contained in highly purified tungsten, we studied the most suitable conditions for separating the elements using solid-phase-extraction as a pretreatment for inductively coupled plasma-mass spectrometry (ICP-MS). We used chemically bonded silica gels belonging to the functional group of benzylsulfonic acid as extracting agent. Tungsten was anionized by adding hydrogen peroxide solution to a sample that had been decomposed with acid. We separated the cation trace impurities that were present in the chemically bonded silica gel of the ion-exchange type. The target elements retained in the chemicals were then eluted using 10 cm~3 of 2 kmol/m~3 nitric acid. Quantities of the obtained target elements were determined using ICP-MS. Highly sensitive quantification was established for 15 trace elements in highly purified tungsten, and for Be, Al, Mg, Mn, Fe, Co, Ni, Cu, Zn, Ga, Cd, In, Tl, Pb, and Bi with the following detection limits [3 sigma; ng/g (ppb)]: Be 0.11, Al 0.14, Mg 0.12, Mn 0.15, Fe 1.81, Co 0.086, Ni 0.082, Cu 0.092, Zn 0.12, Ga 0.074, Cd 0.012, In 0.069, Tl: 0.082, Pb 0.071. and Bi 0.036.
机译:为了建立高纯钨中所含元素的快速痕量量化方案,我们研究了使用固相萃取作为电感耦合等离子体质谱法(ICP-MS)的预处理来分离元素的最合适条件。我们使用属于苄磺酸官能团的化学键合硅胶作为萃取剂。通过将过氧化氢溶液添加到已被酸分解的样品中,使钨阴离子化。我们分离了离子交换型化学键合硅胶中存在的阳离子痕量杂质。然后使用10 cm〜3的2 kmol / m〜3硝酸洗脱保留在化学品中的目标元素。使用ICP-MS确定获得的目标元素的数量。建立了高纯度钨中15种痕量元素以及铍,铝,镁,锰,铁,钴,镍,铜,锌,镓,镉,铟,锡,铅和铋的高灵敏度定量分析方法,并进行了以下检测极限[3 sigma; ng / g(ppb)]:Be 0.11,Al 0.14,Mg 0.12,Mn 0.15,Fe 1.81,Co 0.086,Ni 0.082,Cu 0.092,Zn 0.12,Ga 0.074,Cd 0.012,In 0.069,Tl:0.082,Pb 0.071 。和Bi 0.036。

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