On-line electrolytic dissolution for lead determination in high-purity copper by isotope dilution inductively coupled plasma mass spectrometry

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• 作者：Packer ; Ana Paula ; Gervasio ; Ana Paula G. ; Miranda ; Carlos E.S. ; Reis ; Boaventura F. ; Meneg&aacute ; rio ; Amauri A. ; et. al.
• 关键词：Copper alloys ; Flow injection ; Electrolytic dissolution ; Isotope dilution ; ICP-MS
• 刊名：Analytica Chimica Acta
• 出版年：2003
• 出版时间：June 6, 2003
• 年：2003
• 卷：485
• 期：2
• 页码：145-153
• 全文大小：246 K

文摘

A flow injection system combining electrolytic dissolution (ED) and programmable isotope dilution (ID) for determination of lead in high-purity copper by inductively coupled plasma mass spectrometry (ED-ID-ICP-MS) is proposed. ED was performed employing a Teflon chamber in where a gold cathode was placed. Best electrolytic conditions were achieved by using an 1.5molL⁻¹ nitric acid as electrolytic solution and applying 2.5A (dc) current during 4s. Lead was determined in the electrolytic dissolved sample, which has undergone on-line isotope dilution exploiting binary sampling approach. Isotope dilution was carried out measuring the isotope ratio ²⁰⁶Pb/²⁰⁸Pb before and after on-line addition of the ²⁰⁸Pb-enriched solution. Precision of isotope ratio measurements for a sample containing 7–70μgPbg⁻¹ was characterized by relative standard deviation (R.S.D.) of 0.5 % (n=3) and the proposed methodology presented an R.S.D. lower than 4 % (n=9). Accuracy was assessed comparing obtained results with those obtained by conventional dissolution and no significant difference at 95 % confidence level was observed.