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Simultaneous determination of Cr, Fe, Ni and V in crude oil by emulsion sampling graphite furnace atomic absorption spectrometry

机译:乳浊液进样石墨炉原子吸收光谱法同时测定原油中铬,铁,镍,钒

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In this work a simple and reliable method for the simultaneous determination of Cr, Fe, Ni and V in crude oil, using emulsion sampling graphite furnace atomic absorption spectrometry is proposed. Under the best conditions, sample masses around 50 mg were weighed in polypropylene tubes and emulsified in a mixture of 0.5% (v v~(-1)) hexane + 6% (m v~(-1)) Triton X-100?. Considering the compromised conditions, the pyrolysis an atomization temperatures for the simultaneous determination of Cr, Fe, Ni and V were 1400 ℃ and 2500 ℃, respectively. Aliquots of 20 μL of reference solution and sample emulsion were co-injected into the graphite tube with 10 μL of 1.0 g L~(-1) Mg(NO3)2 as chemical modifier. The detection limits (" = 10, 3σ) and characteristic masses were, respectively: 0.07 μg g~(-1) and 19 pg for Cr; 2.15 μg g~(-1) and 31 pg for Fe; 1.25 μg g~(-1) and 44 pg for Ni; and 1.15 ng g~(-1) and 149 pg for V. The reliability of the proposed method was checked by fuel oil Standard Reference Material (SRMTriton X-100? 1634c - NIST) analysis. The concentrations found presented no statistical differences compared to the certified values at 95% confidence level.
机译:在这项工作中,提出了一种简单而可靠的方法,该方法使用乳化液采样石墨炉原子吸收光谱法同时测定原油中的Cr,Fe,Ni和V。在最佳条件下,在聚丙烯试管中称量约50 mg的样品质量,并在0.5%(v v〜(-1))己烷+ 6%(m v〜(-1))Triton X-100?的混合物中乳化。考虑到折衷条件,同时测定Cr,Fe,Ni和V的热解原子化温度分别为1400℃和2500℃。将20μL参考溶液和样品乳液的等分试样与10μL1.0 g L〜(-1)Mg(NO3)2作为化学改性剂共注入到石墨管中。检出限(“ = 10,3σ)和特征质量分别为:Cr为0.07μgg〜(-1)和19 pg; Fe为2.15μgg〜(-1)和31 pg; 1.25μgg〜(镍的比重为-1)和44 pg;钒的比重为1.15 ng g〜(-1)和149 pg。通过燃油标准参考材料(SRMTriton X-100?1634c-NIST)分析检查了该方法的可靠性。发现的浓度与95%置信水平下的标准值相比无统计学差异。

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