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回复【Alfan】:重油样品测定的前处理

原子吸收光谱(AAS)

  • 引用:
    杨老师,首先向您问好,我99年在您那实习,学到不少东西,非常感谢!
    我有个用户想测原油中的重金属,请问是否可以用原子吸收?如果能,请问样品如何处理?在哪能了解到相关方法介绍?
    **********************
    我查了一下文献,分析样品为重油的不多。以下是查到的简单与处理方法。所涉及的元素已经包括一些重金属
    石墨炉和氢化法测重油中的 As, Cd, Co, Cr, Cu, Hg, Mn, Ni, Pb and V determined using GFAAS or CVAA Safter
    digesting sample with HNO3-H2SO4. Good recoveries for all elementsexcept Hg (70%). (Detection limits 0.004-0.046 mg kg-1)

    重油中测铅火焰法 Ash at 550 .degree.C for 2 h and dissolved in HClO4. FI sample introduction 重油中测钒石墨炉法 Oil sample (10-30 g) ashed at 550 .degree.C then dissolved in 1+1 HCl(50 ml).
    V determined in 20 .mu.l portion at 318.4 nm using Ar ascarrier gas. LOD was 6.9 ng g(-1)
    我看错了,你要的是原油分析,原油的预处理如下:
    Various samples of petroleum and by-products analysed for Cu, Fe, Ni,Pb, and U. Method validated by the analysis of SRMs
    As ,Pb ETA Convert to water soluble iodide by reaction with a solution of iodine(5% m/V) in toluene and extract into dilute HNO3; add 1% m/V Ni(NO3)2solution to droplet in atomiser as matrxmodify
    As ,Pb ETA Pipette 20 ml into a 250-ml separating funnel, add 5 ml 5% iodine intoluene, shake and leave for 60 s; add 10 ml 1% HNO3 and extract for 60s; repeat two separate extractions,
    Flame Method proposed for coulometric preparation of reference solutions ofCo, Cu, Ni, V and Zn in acetone-ethanol-xylene mixtures by anodicdissolution of the corresponding metal at specified current.
    Comparison of sample treatment procedures for determination of Fe incomplex organic mixtures using FAAS and ETAAS. Use of ETAAS after dilution in IBMK is recommended approach

    Fe,ETA Samples diluted with xylene and analysed using ETAAS. (Concentrationrange 0.00018-0.0023% m/m)
    另外,威尔茨的“原子吸收光谱法”中有一些评述。孙汉文的书中也可能有。抱歉!
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  • 第1楼2005/03/23

    谢谢杨老师!
    通常我们在处理原油时,是先用二甲苯、甲醛和混合酒精等进行一系列的溶解处理,然后过滤杂质。如果我们在进行这样的处理后,再进行分析的后续处理,这样会不会有影响分析效果?

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