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A simple extraction procedure for determination of total mercury in crude oil

机译：一种用于确定原油中总汞的简单提取程序

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Abstract The determination of mercury in crude oil and petroleum products is particularly difficult due to the volatile nature of both mercury and the matrix, which may lead to significant loss of the analyte. A simple extraction method for total mercury has been developed to determine total mercury in crude oil using cold vapor atomic fluorescence spectrometry. The homogenized crude oil sample was diluted to 5, 10, and 20 % (w/w) in toluene. The diluted crude oil samples were spiked with 10 and 40 ng/kg (w/w). The samples were extracted using an oxidant/acid solution, BrCl/HCl. The mercury was extracted into the aqueous phase; the ionic mercury was then reduced to volatile elemental mercury (Hg~0) by stannous chloride (SnCly_2). The mercury vapor was detected by Merlin cold vapor atomic fluorescence spectrometry at a 253.7-nm wavelength. The average recoveries for mercury in spiked diluted crude oil (10 and 40 μg/kg, w/w) were between 96 and 103 %, respectively, in 5 and 10 % spiked diluted crude oil. Whereas, low recoveries (<50 %) were recorded in 20 % diluted spiked crude oil. The method detection limit was calculated as t_(0.01)(n-1)×SD where t is the student's value for 99 % confidence level and standard deviation estimate with n - 1 degrees of freedom. The method detection limit was found to be 0.38 μg/kg based on 5 g of diluted crude oil sample. The method is sensitive enough to determine low levels of mercury in crude oil.
机译：摘要由于汞和基质的挥发性，因此很难测定原油和石油产品中的汞，这可能导致分析物的大量损失。已经开发出一种简单的总汞提取方法，使用冷蒸气原子荧光光谱法测定原油中的总汞。将均质的原油样品在甲苯中稀释至5、10和20％（w / w）。将稀释的原油样品加标10和40 ng / kg（w / w）。使用氧化剂/酸溶液BrCl / HCl萃取样品。汞被萃取到水相中。然后通过氯化亚锡（SnCly_2）将离子汞还原为挥发性元素汞（Hg〜0）。通过Merlin冷蒸气原子荧光光谱法在253.7nm波长处检测到汞蒸气。加标稀释原油（10和40μg/ kg，w / w）中汞的平均回收率分别为5％和10％加标稀释原油中的96％至103％。而在20％的稀释加标原油中记录到低回收率（<50％）。方法检测极限的计算公式为t_（0.01）（n-1）×SD，其中t是学生对99％置信度的值和n-1个自由度的标准差估计值。发现基于5 g稀释原油样品的方法检测极限为0.38μg/ kg。该方法足够灵敏，可以测定原油中的汞含量低。

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