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    硒粉催化-连续流动分析法测定烟叶中总氮的含量

    Determination of Total Nitrogen in Tobacco by Selenium Powder Catalysis-Continuous Flow Analysis

    • 摘要: 取约0.2 g烟末样品置于消化管中,加入3 mL物质的量比为0.25%的硒/硫酸混合消化储备溶液,混匀,加入3.0 mL的30%(质量分数)过氧化氢溶液,升温至330 ℃保持1.0 h,冷却后用蒸馏水定容至75 mL,在连续流动分析仪上于660 nm处比色测定总氮含量。结果表明,总氮的质量浓度在0.020 5~0.205 0 g·L-1内与其对应的吸光度呈线性关系,检出限(3s)为2.364 mg·L-1。方法用于分析实验室控制样品,测定值与标称值一致。日内平行测定实验室控制样品6次,日间平行测定5次,测定值的相对标准偏差均小于3.0%。按照标准加入法进行回收试验,回收率为95.1%~102%。

       

      Abstract: About 0.2 g of the tobacco powder sample was taken into digestive tube, then 3 mL of mixed digestion reserve solution of selenium powder and sulfuric acid at mole ratio of 0.25% was added. After blending, 3.0 mL of 30%(mass fraction) hydrogen peroxide was added. The mixture was heated to 330 ℃, keeping for 1.0 h. After cooling, the obtained solution was made its volume up to 75 mL by distilled water. Total nitrogen was determined by continuous flow analyzer at 600 nm. As shown by the results, linear relationship between the corresponding absorbance and mass concentration of total nitrogen was found in the range of 0.020 5-0.205 0 g·L-1, with detection limit (3s) of 2.364 mg·L-1. This method was applied for determination of laboratory control samples, and the determined values were consistent with the nominal values. Laboratory control sample was determined 6 times in parallel for intraday and 5 timies for interday by this method, with RSDs of the determined values less than 3.0%. Test for recovery was made by standard addition method, giving results in the range of 95.1%-102%.

       

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