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无氧铜中氧的含量通常控制在几个ppm,这给分析工作者带来了某些困难。不少作者已对无氧铜和高纯铜中微量氧的测定进行了研究。本文着重探讨脉冲色谱法测定无氧铜中微量氧时样品表面处理、空白值及测定条件。 一、试剂、仪器及其工作条件 四氯化碳(99.5%);磷酸(d1.75),硝酸(d1.42;1+1),盐酸(1+1),乙二醇,过氧化氢(30%),锡粒(99.9%),均为分析纯级;冰醋酸(d1.05),优级纯;镍丝(真空熔炼);工业纯氩(99.99%)。 SQM—1型脉冲色谱仪,由自动恒温循环冷却装置为脉冲炉提供40°±1℃的冷却水。采用M22T14Ⅰ型光谱纯石墨坩埚。
Oxygen levels in oxygen-free copper are typically controlled to a few ppm, giving analysts some difficulty. Many authors have studied the determination of trace oxygen in oxygen-free copper and high purity copper. This article focuses on the determination of trace oxygen in oxygen-free copper by pulse chromatography sample surface treatment, the blank value and the determination of conditions. I. Reagents, Equipment and Working Conditions Carbon tetrachloride (99.5%); phosphoric acid (d1.75), nitric acid (d1.42; 1 + 1), hydrochloric acid (1 + 1), ethylene glycol, hydrogen peroxide (30%), tin particles (99.9%), all analytical grade; glacial acetic acid (d1.05), excellent pure; nickel wire (vacuum melting); SQM-1 pulse chromatograph, the automatic constant temperature circulating cooling device for the pulse furnace to provide 40 ° ± 1 ℃ cooling water. Using M22T14 Ⅰ pure graphite crucible spectrum.