微波消解-原子吸收分光光度法联合测定茶园土壤中铜、铬的优化研究  

The optimization study on determination of copper and chromium in the tea soil using microwave digestion technique combining atomic absorption spectrometry

作　　者：卞彩霞 李娜[1] 赵悦竹 曹海生[1] 谷勋刚[1] BIAN Caixia;LI Na;ZHAO Yuezhu;CAO Haisheng;GU Xungang(School of Resource and Environment,Anhui Agricultural University,Hefei 230036)

机构地区：[1]安徽农业大学资源与环境学院,合肥230036

出　　处：《安徽农业大学学报》2021年第3期429-436,共8页Journal of Anhui Agricultural University

基　　金：国家自然科学基金(31470688);安徽省科技重大专项(17030701049)共同资助。

摘　　要：为了调查皖东南地区红壤中铜、铬元素,检测茶园土壤施用畜禽粪便有机肥是否受到污染,建立了微波消解联合原子吸收分光光度的方法,用于准确、快速测定茶园土壤中铜、铬的含量。在微波消解过程中,采用硝酸、盐酸、氢氟酸和高氯酸为氧化剂,应用正交法优化其用量,优化结果为硝酸4 mL、盐酸3 mL、氢氟酸2 mL、高氯酸0.5 mL。火焰及石墨炉原子吸收法分别以铜、铬标准溶液为对象,优化仪器测定主要参数,火焰法优化结果为:测定波长324.75 nm,狭缝宽度0.7 mm、空气-乙炔比为7.5∶2.5、灯电流6 mA、观测高度0 mm。石墨炉法的结果为:灰化温度为1200℃,维持时间为20 s;原子化温度为2250℃,维持时间为4 s。以优化的方法测定质控样品,并进行加标回收验证,确定该方法测定红壤中铜、铬的稳定性好,准确度高。将建立的方法应用到郎溪县茶园土壤中铜、铬调查时,能准确表征其含量水平。In order to investigate the content of copper and chromium in red soil of southeast Anhui,and verify whether the tea soil was contaminated by application of livestock manure organic fertilizer,the microwave digestion technique combining atomic absorption method was constructed for accurate and rapid determination of copper and chromium in the soil.During microwave digestion process,nitric acid,hydrochloric acid,hydrofluoric acid,and per-chloric acid were used as oxidizing agent for microwave digesting of the soils.The optimized results were obtained by orthogonal experiments,which were 4,3,2,and 0.5 mL for nitric,hydrochloric,hydrofluoric,and per-chloric acid,respectively.The standard solutions of copper and chromium were used as research object to optimize major parameters of the apparatus,which were determined by flame and graphite furnace atomic absorption respectively.The major parameters for flame atomic absorption,such as determining wavelength,slit width,ratio of air and acetylene gas,lamp current,and observed altitude,were 324.75 nm,0.7 mm,7.5 to 2.5,6 mA,and 0 mm,respectively.And those for graphite furnace atomic absorption,such as ash temperature and hold time were 1200℃ and 20 s,respectively.And atomization temperature and hold time were 2250℃ and 4 s,respectively.The certified sample and the spiked red soils were analyzed by the optimized method,the result confirmed it is great stable and high accurate for determination of copper and chromium.Application of the method to the investigation of copper and chromium in tea soil in Langxi County,it is found the content level of copper and chromium was accurately characterized.

关 键 词：原子吸收分光光度仪 微波消解 铜 铬 茶园土壤 

分 类 号：S153.61[农业科学—土壤学] S571.106.1[农业科学—农业基础科学]