氧瓶燃烧-离子色谱法测定香烟中硫含量
IC Determination of Sulfur in Tobacco with Sample Treatment by Oxygen Bomb Combustion
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摘要: 采用氧瓶燃烧法对香烟样品进行燃烧,然后用含有过氧化氢的水溶液吸收释放出来的二氧化硫,并将其转化成为SO42-,过量的过氧化氢通过加热煮沸10 min去除。据此提出了用离子色谱法测定香烟中硫含量的方法。用IonPac AS14离子交换柱,以1.8 mmol·L-1碳酸钠-1.7 mmol·L-1碳酸氢钠溶液为淋洗液等度洗脱。硫的质量浓度在0.02~60 mg·L-1之间与峰面积呈线性关系,方法的检出限(3s)为3.24 μg·L-1。方法用于茶叶(GSB-7)标准样品分析,测定值与认定值相一致。硫的相对标准偏差(n=6)小于1%,回收率在99.2%~99.7%之间。Abstract: The sample of tobacco was combusted in oxygen bomb, and the SO2 evolved were absorbed and transformed to SO42- in 20 mL aqueous solution containing 0.25 mL of 30% hydrogen peroxide, and the excess hydrogen peroxide was removed by heating to boil for 10 min. The content of sulfur (as SO42-) in the absorption solution was determined by IC. Ionpac AS14 column was used as ion exchange column, and a mixture of 1.8 mmol·L-1Na2CO3 and 1.7 mmol·L-1 NaHCO3 was used as eluent. Linear relationship between values of peak area and mass concentration of sulfur was obtained in the range of 0.02-60 mg·L-1, with detection limit (3s) of the method of 3.24 μg·L-1. The proposed method was used in the analysis of standard sample of tea (GSB-7), the results obtained were in conformity with its certified values. Values of recovery found were in the range of 99.2%-99.7% with RSD′s (n=6) less tnan 1%.