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Spectrophotometric determination of uranium with arsenazo-III in perchloric acid

机译:高砷酸中砷偶氮Ⅲ分光光度法测定铀。

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A short, sensitive and reliable spectrophotometric method, which has advantages over all known "wet chemistry" methods for uranium determination with regard to tolerance to common interferences, has been developed for the determination of uranium. Selectivity, molar absorptivity and the determination range of uranium have been enhanced by using 0.07% arsenazo-III as a chromogenic reagent. The use of 3 mol dm(-3) perchloric acid as a medium of determination was found to be excellent in terms of good solvent compatibility on dilution, destruction of organic contamination and simplicity of operation. The uranium-arsenazo-III complex formed instantly, and was found to be stable for more than 3 weeks with constant absorbance. Beer's law was obeyed up to a uranium concentration of 16 mu g g(-1), with a molar absorptivity at 651 nm of 1.45 x 10(5) mol(-1) dm(3) cm(-1) at 24 +/- 2 degrees C. Only phosphate and citrate at 70-fold excess over uranium interfere seriously, whereas other anions studied could be tolerated up to a 70-fold excess over uranium. Of the cations studied, only Mn(II), Co(II), Ni(II), Cu(II) and Cr(III) decreased the normal absorbance of the complex. Iron(III), Ce(III) and Y(III) enhanced the absorbance. Other cations studied did not affect the absorbance up to a 50-fold excess. The accuracy was checked by determining uranium from standard solutions in the range 10-50 mu g g(-1). It was found to be accurate with a 96.0-99.6.% recovery rate. The method has been successfully applied to standard reference materials and ore samples at mu g g(-1) levels. (c) 2005 Elsevier Ltd. All rights reserved.
机译:已经开发了一种短,灵敏且可靠的分光光度法,该方法在确定铀方面具有优于所有已知的“湿化学”方法确定铀的常见干扰能力。通过使用0.07%的砷偶氮-III作为显色剂,可以提高铀的选择性,摩尔吸收率和测定范围。发现使用3 mol dm(-3)高氯酸作为测定介质在稀释时具有良好的溶剂相容性,破坏有机污染物和操作简单方面非常出色。铀-砷偶氮-III络合物立即形成,并在稳定的吸光度下稳定超过3周。遵循比尔定律直到铀浓度为16μgg(-1),在651 nm处的摩尔吸收率为1.45 x 10(5)mol(-1)dm(3)cm(-1)在24 + / -2摄氏度。仅磷酸根和柠檬酸根比铀高出70倍,而其他阴离子却可以耐受铀比70倍高。在所研究的阳离子中,只有Mn(II),Co(II),Ni(II),Cu(II)和Cr(III)会降低络合物的正常吸收率。铁(III),铈(III)和钇(III)提高了吸光度。研究的其他阳离子最多不会吸收50倍以上的吸光度。通过确定标准溶液中10-50μgg(-1)范围内的铀来检查准确性。发现它是准确的,回收率为96.0-99.6。%。该方法已成功应用于μg g(-1)水平的标准参考物质和矿石样品。 (c)2005 Elsevier Ltd.保留所有权利。

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