火焰原子吸收光谱法测定针状石油焦中钾铅镁锌铜锰

doi:10.13228/j.boyuan.issn1000-7571.009448

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摘要在电炉上将样品碳化至无烟后将铂坩埚置于高温炉内于750 ℃下灼烧约6 h进行灰化,采用四硼酸锂(Li₂B₄O₇)熔融、5%硝酸溶解,以5 mL 100 mg/mL镧溶液为释放剂,建立了火焰原子吸收光谱法(FAAS)测定针状石油焦样品中钾、铅、镁、锌、铜、锰的方法。实验表明,针状石油焦样品中其他元素不干扰待测元素的测定,待测元素间无相互干扰。在选定的最佳仪器条件下,钾、铅、镁、锌、铜、锰的检出限分别为0.008、0.030、0.001、0.005、0.008、0.007 μg/mL。采用实验方法对2批针状石油焦样品进行测定,结果与电感耦合等离子体发射光谱法(ICP-AES)基本一致,相对标准偏差(n=10)为0.63%~3.4%,加标回收率在98%~104%之间。

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关键词 ：火焰原子吸收光谱法(FAAS), 针状石油焦, 钾, 铅, 镁, 锌, 铜, 锰

Abstract：The sample in platinum crucible was firstly carbonized on electric stove till no smoke appeared and then burned in a high temperature furnace at 750 ℃ for about 6 h for ashing. With lithium tetraborate (Li₂B₄O₇) for fusion, 5% HNO₃ for dissolution and 5 mL of 100 mg/mL lanthanum solution as release agent, a flame absorption atomic emission spectrometry (FAAS) was established for determination of potassium, lead, magnesium, zinc, copper and manganese in acicular petroleum coke. It was found that other elements in acicular petroleum coke didn't interfere with the determination, and there was no interference between testing elements. Under optimal conditions, the detection limit of potassium, lead, magnesium, zinc, copper, manganese was 0.008, 0.030, 0.001, 0.005, 0.008, 0.007 μg/mL, respectively. Two batches of acicular petroleum coke samples were determined by this proposed method, whose results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES). The relative standard deviation (n=10) was 0.63%-3.4%, and the standard addition recovery was 98%-104%.

Key words： flame atomic absorption spectrometry(FAAS) acicular petroleum coke potassium lead magnesium zinc copper manganese

收稿日期: 2014-07-20

基金资助:辽宁医学院横向课题(LYHX2013001)

通讯作者: 卢静华,女,副教授,硕士生导师;E-mail:jinghual888@163.com

作者简介: 文婧(1990-),女,硕士,从事药物分析学研究;E-mail:wenjing549@163.com

引用本文:

文婧,孙洪章,卢静华. 火焰原子吸收光谱法测定针状石油焦中钾铅镁锌铜锰[J]. 冶金分析, 2015, 35(3): 46-50. WEN Jing,SUN Hong-zhang,LU Jing-hua. Determination of potassium,lead,magnesium,zinc,copper and manganese in acicular petroleum coke by flame atomic absorption spectrometry. , 2015, 35(3): 46-50.

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http://yjfx.chinamet.cn/CN/10.13228/j.boyuan.issn1000-7571.009448 或 http://yjfx.chinamet.cn/CN/Y2015/V35/I3/46

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