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Determination of trace elements in B5-diesel oil by HR-CS ET AAS using a simple dilute-and-shoot approach

机译:HR-CS ET AAS使用简单的稀释即取方法测定B5柴油中的微量元素

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This work describes a simple, fast and sensitive procedure for the determination of Al, Cd, Cu, Fe, Pb and Mn in commercial B5-diesel oil samples using high-resolution continuum source electrothermal atomic absorption spectrometry (HR-CS ET AAS). The procedure consists on simple dilution of the samples using n-propanol, with further acidification with HNO3. Calibration against aqueous standards could be employed for the determination of Cu, Fe, Pb and Mn, whereas calibration solutions prepared in n-propanol were required for the determination of Al and Cd. The pyrolysis and atomization curves were investigated for the analytes prepared in aqueous solutions and for the B5-diesel oil samples. A study involving the use of modifiers was carried out. 480 μg of Zr for Al, Mn and Pb determination and 500 μg of Ir for Cd determination were employed as permanent chemical modifiers. Pyrolysis temperatures of 700 °C for Cd, 800 °C for Pb and 1000 °C for the other elements were adopted. The atomization temperatures were optimized as 1500 °C for Cd, 1900 °C for Pb, 2300 °C for Cu, Fe and Mn and 2500 °C for Al. The limits of quantification were determined as 0.001 μg g-1 for Cd and Mn, 0.002 μg g-1 for Pb, 0.006 μg g-1 for Fe and 0.01 μg g-1 for Al and Cu. Recovery tests resulted in recovery values between 89 and 120% for diesel oil samples. The method has proved to be fast, precise and accurate.
机译:这项工作描述了一种简单,快速和灵敏的程序,使用高分辨率连续谱源电热原子吸收光谱法(HR-CS ET AAS)测定商业B5柴油样品中的Al,Cd,Cu,Fe,Pb和Mn。该程序包括使用正丙醇对样品进行简单稀释,然后用HNO3进一步酸化。可以使用相对于水标准品的校准方法来确定Cu,Fe,Pb和Mn,而使用正丙醇制备的校准溶液则需要用于测定Al和Cd。研究了水溶液中制备的分析物和B5柴油样品的热解和雾化曲线。进行了涉及使用改性剂的研究。 480μg的Zr用于Al,Mn和Pb的测定,500μg的Ir用于Cd的测定,作为永久性化学改性剂。 Cd的热解温度为700°C,Pb的热解温度为800°C,其他元素的热解温度为1000°C。雾化温度最优化为Cd 1500°C,Pb 1900°C,Cu,Fe和Mn 2300°C和Al 2500°C。定量限确定为Cd和Mn为0.001μgg-1,Pb为0.002μgg-1,Fe为0.006μgg-1,Al和Cu为0.01μgg-1。回收率测试得出的柴油样品的回收率介于89%至120%之间。该方法已被证明是快速,准确和准确的。

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