高级检索

    超声交换-抽滤淋洗-全自动凯氏定氮法测定土壤中阳离子交换量

    Determination of Cation Exchange Capacity in Soil by Automatic Kjeldahl Nitrogen Method after Ultrasonic Exchange and Suction Filtration Leaching

    • 摘要: 当土壤样品pH≤7.5时,取2.00 g样品,用1 mol·L-1乙酸铵溶液冲洗至土壤无结块,并定容至50 mL,超声交换6 min。当土壤样品pH>7.5时,取2.00 g样品,加入1 mol·L-1氯化铵溶液50 mL,在电炉上煮沸,直至表面皿上蒸出的水的酸度达到pH 7(依此判断氨已煮尽),再加入1 mol·L-1乙酸铵溶液,超声交换6 min。启动抽滤模式,将超声好的样品倒在布氏漏斗上,用40 mL乙醇洗涤沉淀,重复洗涤4次,直至无NH4+洗出(用纳氏试剂检测)。将沉淀、滤纸和约1 g预先高温灼烧好的固体氧化镁试剂置于全自动凯氏定氮仪上,设置盐酸溶液浓度为0.05 mol·L-1、20 g·L-1硼酸吸收液(内含甲基红-溴甲酚绿指示剂)用量为20 mL,蒸馏时间为5.0 min,自动完成消化、蒸馏和滴定操作,仪器输出结果即为测定值。结果表明:方法检出限(3.143s)为0.083 cmol·L-1;按照试验方法分析土壤有效态成分分析标准物质,测定值的相对标准偏差(RSD,n=5)均小于5.0%,且测定值均在认定值的不确定度范围内;方法用于分析不同来源地不同类型的样品,所得测定值的RSD (n=5)小于标准(LY/T 1243-1999)方法的,相对误差为-1.5%~6.6%,t检验结果(0.041 9)小于临界值(t10,0.95=2.228),两种方法无显著性差异。

       

      Abstract: When the pH of soil sample was not more than 7.5, 2.00 g of the sample was taken and washed with 1 mol·L-1 ammonium acetate solution until there was no caking, and the mixture obtained was diluted to 50 mL and exchanged with ultrasound for 6 min. When the pH of soil sample was more than 7.5, 2.00 g of the sample was taken and mixed with 50 mL of 1 mol·L-1 ammonium chloride solution. The mixture obtained was boiled on electric furnace until the acidity of the water evaporated on the watch glass reached to pH 7 (judging that the ammonia had been boiled out), and 1 mol·L-1 ammonium acetate solution was added into the above mixture and exchanged with ultrasound for 6 min. After turning on suction filtration, the sample obtained by ultrasound was poured onto the Brinell funnel, the precipitation was washed with 40 mL ethanol, and the washing process was repeated 4 times until no NH4+ was washed out (detected with Nessler reagent). The precipitation, filter paper together with about 1 g of solid magnesium oxide reagent burned at high temperature in advance were placed on the Automatic Kjeldahl nitrogen analyzer with the concentration of hydrochloric acid solution of 0.05 mol·L-1, the amount of 20 g·L-1 boric acid absorption solution containing methyl red-bromocresol green indicator of 20 mL and the distillation time of 5.0 min, to automatically complete the digestion, distillation and titration operations. The output result of the instrument was the determined value. As found by results, the detection limit (3.143s) was 0.083 cmol·L-1. The proposed method was applied to the analysis for the soil active composition analysis reference materials, and RSDs (n=5) of the determined values were less than 5.0%, and the determined values were within the uncertainty ranges of the certified values. Different types of samples from different regions were analyzed, and RSDs (n=5) of the determined values were less than those given by standard method of LY/T 1243-1999, with the relative errors of the determined values in the range of -1.5%-6.6%. The result (0.041 9) of t-test was less than the critical value (t10,0.95=2.228), and it turned out that no significant difference exited between the two methods.

       

    /

    返回文章
    返回