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机构地区:[1]辽宁医学院,辽宁锦州121000
出 处:《冶金分析》2015年第3期46-50,共5页Metallurgical Analysis
基 金:辽宁医学院横向课题(LYHX2013001)
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6h进行灰化,采用四硼酸锂(Li2B4O7)熔融、5%硝酸溶解,以5mL 100mg/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、0.007μg/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。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 oth- er elements in acicular petroleum coke didn't interfere with the determination, and there was no interfer- ence between testing elements. Under optimal conditions, the detection limit of potassium, lead, magnesi- um, 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%.
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