样品粒径、制样方法对波长色散X射线荧光光谱法测定土壤样品中19种元素的影响  

Effects of sample particle size and preparation on the determination of 19 elements in soil samples by wavelength dispersive X-ray fluorescence spectrometry

作　　者：耿梅梅[1] 张丽萍[1] 王久荣[1] 李春勇[1] GENG Mei-mei;ZHANG Li-ping;WANG Jiu-rong;LI Chun-yong(Institute of Subtropical Agriculture,Chinese Academy of Sciences,Changsha Hunan 410125)

机构地区：[1]中国科学院亚热带农业生态研究所,湖南长沙410125

出　　处：《中国土壤与肥料》2023年第6期239-250,共12页Soil and Fertilizer Sciences in China

基　　金：国家自然科学基金区域联合重点项目(U20A2011)。

摘　　要：利用波长色散X射线荧光光谱仪建立了压片、熔融土壤样品中As、Co、Cr、Cu、Mn、Ni、P、Pb、S、Ti、V、Zn、Al_(2)O_(3)、CaO、Fe_(2)O_(3)、K_(2)O、MgO、Na_(2)O、SiO_(2)19种元素的分析方法。探讨了样品粒径、制样方法对19种元素检测的影响。方法精密度结果表明,样品中As、Co元素含量在10 mg/kg以上时,0.149 mm(100目)样品压片、0.075 mm(200目)样品压片及样品熔融制样的19种元素的相对标准偏差(RSD)值均小于10%,As、Co含量在10 mg/kg以下时,200目压片制样的19种元素RSD值小于10%。准确度结果表明,压片制样的标准物质含量在5 mg/kg以上的As、Co、Cu及其他16种元素准确度符合要求;熔融制样的标准物质中高含量的As、Co、Cu、Pb元素及其他15种元素准确度符合要求。不同粒径实验结果显示,元素含量在10 mg/kg以上时,100目、200目压片制样19种元素的RSD值小于10%。不同制样方法的实验结果表明,熔融制样不适用于低含量的As、Co、Cu、Pb元素分析,Cr、P、S、Mn、Ni、V、Zn、Ti、Al_(2)O_(3)、CaO、Fe_(2)O_(3)、K_(2)O、MgO、Na_(2)O、SiO_(2)熔融制样与压片制样RSD值小于10%。压片制样方法操作更简单,成本更低,更适用于大批量土壤样品中As、Co、Cr、Cu、Pb、P、S、Mn、Ni、V、Zn、Ti、Al_(2)O_(3)、CaO、Fe_(2)O_(3)、K_(2)O、MgO、Na_(2)O、SiO_(2)19种元素的分析;对于As、Co元素含量在10 mg/kg以上的样品,利用100目、200目样品压片制样均可获得准确、可靠的结果,对于As、Co含量在10 mg/kg以下的样品,建议使用200目样品压片制样。Methods for analysis of 19 elements in pressed and fusion soil samples,including As,Co,Cr,Cu,Mn,Ni,P,Pb,S,Ti,V,Zn,Al_(2)O_(3),Cao,Fe_(2)O_(3),K_(2)O,MgO,Na_(2)O and SiO_(2),were established by using wavelength dispersive X-ray fluorescence spectrometer.The effects of sample size and sample preparation method on the determination of 19 elements were discussed.The results of method precision showed that when the contents of As and Co in the samples were more than 10 mg/kg,the RSD values of 19 elements in 0.149 mm(100 mesh)pressed,0.075 mm(200 mesh)pressed and fusion samples were less than 10%.When the contents of As and Co were less than 10 mg/kg,the relative standard deviation(RSD)values of 19 elements of 200 mesh pressed were less than 10%.The accuracy results showed that the accuracy of pressed reference material with more than 5 mg/kg As,Co,Cu and all contents of other 16 elements met the requirements;the accuracy of fusion reference materials with high contents of As,Co,Cu,Pb and other 15 elements met the requirements.The experimental results of different particle sizes showed that when the elements contents were more than 10 mg/kg,the RSD values of 19 elements in 100 mesh and 200 mesh pressed results were less than 10%.The experimental results of different sample preparation methods showed that,fusion preparation was not applicable to analysis As,Co,Cu and Pb elements with low content,the RSD values of Cr,P,S,Mn,Ni,V,Zn,Ti,Al_(2)O_(3),CaO,Fe_(2)O_(3),K_(2)O,MgO,Na_(2)O and SiO_(2)with fusion and pressed preparation were less than 10%.The pressed preparation method has simpler operation and lower cost,it is more suitable for the analysis of 19 elements such as As,Co,Cr,Cu,Pb,P,S,Mn,Ni,V,Zn,Ti,Al_(2)O_(3),CaO,Fe_(2)O_(3),K_(2)O,MgO,Na_(2)O and SiO_(2)in a large number of soil samples.For samples with As and Co above 10 mg/kg,accurate and reliable results can be obtained by using 100 mesh and 200 mesh pressed samples.For samples with As and Co below 10 mg/kg,it is recommended to use 200 mesh sample pressed prepa

关 键 词：波长色散X射线荧光光谱 粉末压片 熔融制样 土壤 粒径 

分 类 号：S151.95[农业科学—土壤学] O657.34[农业科学—农业基础科学]