高压密闭消解处理草酸-草酸铵浸提剂方法的改进  

Improvement on the treatment of oxalic acid-ammonium oxalate extractant by high pressure closed digestion

作　　者：任冬 刘彤彤 刘安安 钱银娣 REN Dong;LIU Tong-tong;LIU An-an;QIAN Yin-di(Zhangye Geo-mine Survey Instisute of Non-ferrous MetalGeological Exploration Bureau ,Gansu Zhangye 734000)

机构地区：[1]甘肃省有色金属地质勘查局张掖矿产勘查院

出　　处：《中国土壤与肥料》2019年第3期198-201,共4页Soil and Fertilizer Sciences in China

摘　　要：采用高压密闭消解处理草酸-草酸铵浸提剂后,能充分破坏草酸盐及有机质,用酸量小,样品空白值低,安全可靠,能有效防止样品污染,挥发损失。土壤样品经草酸-草酸铵浸提后,吸取上清液于高压密闭消解罐中,经电热板上处理,再加入2mL浓硝酸,于180℃烘箱中保温至少3h,开盖,定容,采用ICP-MS测定有效钼。方法检出限(3s)为0.014μg/g,相对标准偏差(n=12)为4.4%~7.6%。经国家一级标准物质验证,以及利用本法与NY/T1121方法比对,两者之间数据相吻合。本方法可行性强,适合批量样品分析。Oxalate and organic matter can be fully destroyed by high-pressure sealed digestion of oxalic acid-ammonium oxalate leaching agent.The method is safe and reliable,the amount of acid used is little,and the blank value of the sample is low,and it can effectively prevent sample pollution and the volatilization loss.Soil samples were leached by oxalic acidammonium oxalate,the supernatant was absorbed in a high-pressure sealed digestion tank,treated by electric heating plate, and then added 2 mL concentrated nitric acid.The soil samples were kept in an oven at 180℃ for at least 3 hours,then the concentration of effective molybdenum was determined by ICP-MS.The detection limit(3 s)was 0.014μg/g and RSD(n=12) was 4.4%~7.6%.The method has been verified by the national first-class reference material and compared with the NY / T1121 method.The data are in good agreement.The method is feasible and suitable for batch sample analysis.

关 键 词：土壤 高压密闭消解 草酸-草酸铵 有效钼 

分 类 号：S151.9[农业科学—土壤学]