惰气熔融-红外吸收法测定高纯铜中痕量氧

发布时间：2018-03-04 12:03

本文选题：惰性气体熔融法　切入点：红外吸收法　出处：《冶金分析》2015年05期 　论文类型：期刊论文

【摘要】：为降低氧的空白,在不添加助熔剂的条件下建立了惰性气体熔融-红外吸收法准确测定高纯铜中痕量氧的分析方法。实验表明:称取0.8g左右的样品,在标准石墨坩埚中进行测定,控制吹扫时间为35s,排气时间为25s,排气周期为2次,排气功率为4 500W,分析功率为4 000 W,测得空白标准偏差为0.027μg/g,氧的定量限可降至0.27μg/g。准确称取10~30μg高纯氧化铁于锡囊中,用于仪器的校正,获得校正系数为1.034,解决了没有合适标准物质的难题。采用实验方法对高纯铜实际样品进行测定,测得铜中氧的质量分数为2.43μg/g,相对标准偏差(RSD)不大于7.7%。在测量不确定度评定中考虑了校正样品测量重复性、氧化铁试剂纯度、样品测量重复性和空白等影响因素,计算得到铜中氧质量分数的不确定度为0.33μg/g(k=2)。在高纯铜中加入高纯氧化铁进行加标回收试验,回收率在100%~105%之间。
[Abstract]:In order to reduce the blank of oxygen, a method for the determination of trace oxygen in high purity copper by inert gas melting infrared absorption method was established without adding flux. The control blowing time is 35 s, the exhaust time is 25 s, and the exhaust period is 2 times. The exhaust power is 4 500 W, the analytical power is 4 000 W, the blank standard deviation is 0. 027 渭 g / g, and the quantitative limit of oxygen can be reduced to 0. 27 渭 g / g. The calibration coefficient is 1.034, which solves the problem that there is no suitable standard material. The mass fraction of oxygen in copper is 2.43 渭 g / g, and the relative standard deviation (RSDs) is not greater than 7.7.In the evaluation of uncertainty of measurement, the factors affecting the measurement repeatability of calibration sample, the purity of ferric oxide reagent, the repeatability and blank of sample measurement are taken into account. The uncertainty of oxygen content in copper was calculated to be 0.33 渭 g / g 路kg ~ (-2) 路L ~ (-1). The recovery rate was between 100% and 105% by adding high purity iron oxide to high purity copper.
【作者单位】：北京理工大学化工与环境学院;中国计量科学研究院;
【基金】：科技部支撑计划课题(No.2013BAK12B02) 国家质检总局技改项目(No.2014NIM16)
【分类号】：TG115.3

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