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    混合酸溶解-电感耦合等离子体原子发射光谱法测定土壤中17种元素

    Determination of 17 Elements in Soil by Inductively Coupled Plasma Atomic Emission Spectrometry After Dissolution with Mixed Acid

    • 摘要: 称取0.250 0 g样品置于聚四氟乙烯坩埚中,加几滴水润湿样品,加入1.5 mL硝酸、1.5 mL盐酸、3 mL氢氟酸和1 mL高氯酸,盖上坩埚盖,置于排风橱中,放置过夜。将聚四氟乙烯坩埚放置于控温电热板上,于190~210℃加热,蒸发至白烟冒尽,关闭电源,然后加入5 mL盐酸(1+1)溶液,加入2滴过氧化氢,在电热板上利用余温加热至固体盐类完全溶解,继续加热5~10 min至溶液清亮,冷却后将溶液用水定容至25.0 mL,静置3 h后用电感耦合等离子体原子发射光谱法同时测定样品溶液中硫、铍、铈、钴、铜、锂、锰、镍、钪、镧、钒、锌、镁、钙、钾、钠和铁等17种元素。17种元素的质量浓度在一定范围内与其发射强度呈线性关系,检出限在0.02~50 μg·g-1之间。方法用于土壤国家标准物质中上述17种元素的测定,结果与认定值相符,测定值的相对标准偏差(n=12)小于4.0%。

       

      Abstract: The sample (0.250 0 g) was added into a Teflon crucible, and a few drops of water was added to wet the sample. Then 1.5 mL of nitric acid, 1.5 mL of hydrochloric acid, 3 mL of hydrofluoric acid and 1 mL of perchloric acid were added, and the crucible was covered with a lid and placed in the fume hood overnight. The Teflon crucible was placed on a temperature-controlled electric heating plate, and heated at 190-210 ℃. The solution was evaporated until the white smoke was exhausted, and the power was turned off. 5 mL of hydrochloric acid (1+1) solution and 2 drops of hydrogen peroxide were added. The residual temperature of the hot plate was used to continue to dissolve the solid salt, and the crucible was heated further for 5-10 min until the solution was clear. After cooling, the solution was made up to 25.0 mL with water and let stand still for 3 h. Inductively coupled plasma atomic emission spectrometry was used to simultaneously determine 17 elements, such as sulfur, bismuth, antimony, cobalt, copper, lithium, manganese, nickel, strontium, barium, vanadium, zinc, magnesium, potassium, calcium, sodium and iron in the sample solution. Linear relationships were found between emission intensity and mass concentration of the 17 elements in definite ranges, and the detection limits were in the range of 0.02-50 μg·g-1. The method was applied to the determination of the above 17 elements in the national standard materials of soil, giving the results consistent with the certified values, and the relative standard deviations (n=12) of the measured values less than 4.0%.

       

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