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    石墨加热-冷凝回流消煮-电感耦合等离子体原子发射光谱法快速测定土壤中缓效钾的含量

    Rapid Determination of Slow-Release Potassium in Soil by Inductively Coupled Plasma Atomic Emission Spectrometry with Graphite Heating and Condensation Reflux Digestion

    • 摘要: 为解决行业标准NY/T 889—2004测定土壤中缓效钾时油浴加热操作困难、硝酸易溅射、火焰光度计灵敏度低等问题,用石墨加热替代油浴加热,用自制冷凝回流消化管替代NY/T 889—2004中的消化管和漏斗,提出了题示研究。取过16目(1 mm)筛的风干土壤样品2.50 g置于自制冷凝回流消化管中,加入1 mol·L−1硝酸溶液25.0 mL,摇匀,置于石墨消解仪中,于135 ℃煮沸12 min(从沸腾开始计时),趁热倒入漏斗中,滤液置于100 mL容量瓶中,用0.1 mol·L−1硝酸溶液15 mL冲洗消化管,再倒入漏斗,共重复4次,合并所有滤液,最后用水定容。在射频功率1 150 W,辅助气流量0.6 L·min−1,分析谱线766.491 nm的条件下采用电感耦合等离子体原子发射光谱法测定缓效钾的含量。结果表明,钾元素的质量浓度在0.10~30.00 mg·L−1内与对应的响应强度呈线性关系,检出限(3.143s)为1 mg·kg−1。按照标准加入法进行回收试验,回收率为88.0%~97.5%。方法用于15种标准物质分析,测定值均在认定值的不确定度范围内,且测定值的相对标准偏差(n=7)均不大于7.0%。

       

      Abstract: In order to solve the problems of the industry standard NY/T 889—2004 for determination of slow-release potassium in soil, including difficult oil-bath heating operation,easy sputtering of nitric acid, and low sensitivity of flame photometer. The oil-bath heating was replaced with the graphite heating,and the digestion tube and funnel in NY/T 889—2004 were replaced with a self-made condensation reflux digestion tube, the study mentioned by title was proposed. 2.50 g of air dried soil sample that passed through a 16 mesh (1 mm) sieve was taken and placed in a self-made condensation reflux digestion tube. 25.0 mL of 1 mol·L−1 nitric acid solution was added and shaken well. The mixture was placed in a graphite digestion apparatus, boiled at 135 ℃ for 12 min (counting from boiling) and poured into a funnel. The filtrate was taken and placed in a 100 mL-volumetric flask. 15 mL of 0.1 mol·L−1 nitric acid solution was used to rinse the digestion tube and the solution was poured into the funnel . This process was repeated 4 times, all filtrates were combined, and the mixture was made its volume with water. The content of slow-release potassium was determinde by inductively coupled plasma atomic emission spectrometry under the conditions of radio-frequency power of 1 150 W, auxiliary gas flow rate of 0.6 L·min−1, and analysis spectral line of 766.491 nm. As shown by the results, linear relationship between the corresponding the response intensities and mass concentrations of slow-release potassium was kept in the range of 0.10-30.00 mg·L−1, with detection limit (3.143s) of 1 mg·kg−1. Test for recovery was made according to the standard addition method, giving results in the range of 88.0%-97.5%. This method was used for the analysis of 15 standard substances, and the determined values were found within the uncertainty range of the certified values, and RSDs (n=7) of the determined values were not more than 7.0%.

       

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