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研究旨在确立无火焰石墨炉AAS法测定钒的最佳条件,用以进行饲料中钒元素的测定。通过优化钒元素在石墨炉中测定条件,利用多种不同的基体改进剂及不同的酸作为酸介质,分别测定其对钒测定结果的影响。最终确立了无火焰石墨炉AAS法测定钒的最佳条件:样品干燥温度70～150、灰化温度800～1 600、原子化温度2 700和净化温度2 800℃,300～500μg/mL氯化镧为基体改进剂,4%的盐酸为酸介质。测定方法线性范围为0～0.25μg/mL,检出极限2.08μg/L,曲线相关系数r=0.996 2,回收率为94.54%～97.42%,相对标准偏差为1.5%～2.1%。该法用于饲料中微量钒的测定结果满意。
The aim of this study is to establish the optimal conditions for the determination of vanadium in the flameless graphite furnace AAS method for the determination of vanadium in feed. By optimizing the conditions for the determination of vanadium in a graphite furnace, the effect of different vanadium precursors and different acids on the determination of vanadium was determined. Finally, the optimal conditions for the determination of vanadium by flameless graphite furnace AAS were established. The sample drying temperature was 70-150 ℃, the ashing temperature was 800-1 600, the atomization temperature was 2 700, the purification temperature was 2 800 ℃, and the concentration was 300-500μg / mL. Lanthanum matrix modifier, 4% hydrochloric acid as the acid medium. The linear range of determination was 0 ~ 0.25μg / mL, the detection limit was 2.08μg / L, the correlation coefficient of the curve was 0.996 2, the recovery was 94.54% ~ 97.42% and the relative standard deviation was 1.5% ~ 2.1%. The method for the determination of trace amounts of vanadium in feed is satisfactory.