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采用微波灰化-电感耦合等离子体-发射光谱法测定石油沥青中的钙、铁、钠、镍和钒元素。石油沥青样品通过硫酸酸解处理,解决了样品无法低温灰化的问题,并对微波灰化温度、硫酸用量、升温程序及样品称样量进行了详细研究,结合差示扫描量热法确立了石油沥青微波灰化前处理的最佳条件。钙、铁、钠、镍和钒元素方法检出限分别为0.04、0.10、0.64、0.28、0.22mg·kg-1。加标回收率在79.7%—97.8%之间,相对标准偏差为3.4%—8.3%,重复性和回收率实验结果表明该方法能满足石油沥青中元素分析的要求。
Determination of Calcium, Iron, Sodium, Nickel and Vanadium in Petroleum Asphalt by Microwave Ashing - Inductively Coupled Plasma - Atomic Emission Spectrometry. The petroleum asphalt sample is treated by sulfuric acid to solve the problem that the sample can not be ashed at low temperature, and the microwave ashing temperature, the amount of sulfuric acid, the temperature rising program and the sample weighing amount are studied in detail, and the differential scanning calorimetry Optimum conditions for pretreatment of petroleum asphalt with microwave ashing. The detection limits of calcium, iron, sodium, nickel and vanadium were 0.04, 0.10, 0.64, 0.28 and 0.22 mg · kg-1, respectively. The spiked recoveries ranged from 79.7% to 97.8%, and the relative standard deviations (RSDs) ranged from 3.4% to 8.3%. The repeatability and recovery experiments showed that the proposed method could meet the requirements of elemental analysis in petroleum bitumen.