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    全自动淋洗样品预处理-气相分子吸收光谱法测定土壤阳离子交换量

    Determination of Cation Exchange Capacity of Soil by Gas Molecular Absorption Spectrometry with Sample Treatment by Automatic Rinsing Device

    • 摘要: 称取经风干并过2 mm筛孔的网筛的土壤样品2.000 g置于反应瓶中,采用全自动淋洗仪,加入1.00 mol·L-1乙酸铵溶液80 mL对土样进行处理。经过前处理,土样中的阳离子全部被NH4+离子所取代。此时,仪器将自动吸入乙醇对土样进行反复淋洗。淋洗结束后,将土样完全转移至蒸馏瓶中进行蒸馏。馏出液接收于预置有20 g·L-1硼酸吸收液20 mL的100 mL比色管中,待管中溶液总体积达到90 mL时,取下比色管,加水定容至100.0 mL。此吸收液中氨氮的含量用气相分子吸收光谱法进行测定。此吸收液最长可放置24 h,在24 h以内测定结果不受放置时间的影响。标准曲线系用氨氮标准溶液(0.10~2.00 mg·L-1范围内)按气相分子吸收光谱法进行测定并制作。土样的阳离子交换量(CEC)系根据所测得的氨氮含量按公式换算求出。按此方法分析了4种土壤标准物质,所测得的CEC值与认定值相符,其测定值的相对标准偏差(n=6)均小于2.0%。

       

      Abstract: 2.000 g of air-dried soil sample having passed through a sieve with 2 mm bore were taken and pre-treated by an automatic rinsing device with 80 mL of 1.00 mol·L-1 ammonium acetate solution, to exchange all the cations in the soil sample by NH4+, after which the soil sample was rinsed repeatedly with ethanol. After rinsing, the soil sample was transferred to a distiller to distill ammonia from the sample, and the distillate was led to a colorimetric tube in which 20 mL of 20 g·L-1 boric acid solution was added as absorbent. When the solution attained to ca. 90 mL during distillation, the colorimetric bute was removed from the distiller, and volume of the solution was made up to 100.0 mL with water. Content of NH4-N in the absorption solution was then determined by gas molecular absorption spectrometry (GMAS). The absorption solution can be kept as long as 24 h before the spectrometric determination. No significant deviation of results of NH4-N was found for determination in this absorption solution with preservation time within 24 h. Standard NH4+-N solution was used for preparation of standard curve (in the linearity range of 0.10 to 2.00 mg·L-1) by the GMAS method. Values of cation exchange capacity (CEC) were calculated by the formula given based on data of NH4+-N found. The proposed method was tested by analyzing 4 CRMs of soil, giving values of CEC in consistency with the certified values. RSDs (n=6) found for these 4 samples were all less than 2.0%.

       

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