微波等离子体炬原子发射光谱法测定原油中钙

发布时间：2018-03-12 07:10

本文选题：微波等离子体炬原子发射光谱法(MPT-AES)　切入点：原油　出处：《冶金分析》2017年01期 　论文类型：期刊论文

【摘要】：微波等离子体炬原子发射光谱法(MPT-AES)是利用微波源提供能量,其与电感耦合等离子体原子发射光谱法(ICP-AES)特点类似,具有原子化效率高、分析速度快和操作简单等优点,但是目前对该技术的应用研究仅限于仪器工作条件的优化,对某些共存元素的干扰缺乏有效的解决措施。实验以氩气为载气和工作气,详细考察了MPT-AES测定原油中钙的工作条件和共存元素对钙测定的影响。结果表明,选择Ca 393.366nm为分析谱线,微波功率为85 W,载气流量为1 350 mL/min,工作气流量为650 mL/min,钙质量浓度在0.010~6.00μg/mL范围内与其对应的发射强度呈线性,线性相关系数r=0.999 8;方法中钙的检出限为5.6×10-3μg/mL。干扰试验结果表明,7倍于钙质量浓度的钠,3倍于钙质量浓度的铁、钴,1倍于钙质量浓度的镁、铜、铝不影响钙的测定;1倍于钙质量浓度的钒、镍干扰钙的测定。在0.5mL 5g/L EDTA和0.5mL 10g/L邻菲罗啉溶液的联合作用下,可使铝、钴、镍、镁、铁、铜、钒的允许量至少提高到5倍。将实验方法应用于原油中钙的测定,测定结果与火焰原子吸收光谱法(FAAS)基本一致,相对标准偏差(RSD,n=6)为1.6%~2.2%。
[Abstract]:Microwave plasma torch atomic emission spectrometry (MPT-AESs) provides energy by microwave source, which is similar to inductively coupled plasma atomic emission spectrometry (ICP-AESS). It has the advantages of high atomization efficiency, fast analysis speed and simple operation. However, at present, the research on the application of this technology is limited to the optimization of the working conditions of the instrument, and the interference of some coexisting elements is not solved effectively. In the experiment, argon is used as carrier gas and working gas. The working conditions of determination of calcium in crude oil by MPT-AES and the influence of coexisting elements on the determination of calcium were investigated in detail. The results showed that Ca 393.366nm was selected as the analytical line. The microwave power is 85 W, the carrier gas flow rate is 1 350 mL / min, the working gas flow rate is 650 mL / min, and the mass concentration of calcium is linear in the range of 0.010 渭 g / mL to 6.00 渭 g / mL. The detection limit of calcium in the method is 5.6 脳 10 ~ (-3) 渭 g 路mL ~ (-1). The results of interference test show that the concentration of Ca ~ (2 +) is 3 times that of Na ~ (2 +) and Fe of Ca ~ (2 +), and that of Co ~ (2 +) is 1 times that of mg and Cu (Ca ~ (2 +)). Aluminum does not affect the determination of calcium by twice the mass concentration of calcium. Nickel interferes with the determination of calcium. Under the combined action of 0.5 mL 5g / L EDTA and 0.5mL 10g / L phenanthroline solution, aluminum, cobalt, nickel, magnesium, iron, copper, The allowable amount of vanadium is at least 5 times higher. The results obtained by using the experimental method for the determination of calcium in crude oil are in good agreement with the flame atomic absorption spectrometry (Faas), and the relative standard deviation (RSDN) is 1.6% and 2.2%.
【作者单位】：辽宁石油化工大学化学化工与环境学部;
【分类号】：TE622;O657.31

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