环境土壤标准物质的研究与制备

Study and Preparation of Environmental Soils Standard Reference Materials

用高铝陶瓷球磨机加工在１２０℃下烘干３０ｈ的风砂土、黑土和暗棕壤土壤样品。用Ｘ－射线荧光光谱法等分析样品中Ｃｕ、Ｆｅ、Ｔｉ等元素，做均匀度检验，结果表明样品均匀。定值分析采用ＮＡ、ＩＣＰ－ＭＳ等１８种不同原理的分析技术。在１年多时间里，用Ｘ－射线荧光光谱法做稳定性实验，表明样品稳定。在ＩＢＭ计算机上处理获取的全部数据．用Ｇｒｕｂｂｓ、多重比较Ｓ法等剔除离群值，求出最佳估计值。以最佳估计值按定值原则确定标准值。

he samples of sandy soil, dark soil and dark brownpodzolitic soil were collected, dried at 120℃ for 30hours, and then ground in a high-aluming ceramicball mill. X-ray fluorecence spectrometry was usedto test the homogeneity of Cu ,Zn, Fe, Mn, Ti, Sr, V,Zr,etc. A two- level nested variance analysis andcoparison, F-test and t-test were carried out. TheresultS showed that the samples were homogeneous.Eighteen different techniques were used forcertification, including plasma spectrometry, atomicabsorption spectrometry, plasma mass spectrometry,X-ray fluorescence, neutron activation, etc. Foreach of moot elements, two or more different,reliable analytic methods were adopted. A computerwas used to process the data obtained by statisticalmethod. Any group- outliers were rejected byusingGrubbs, T, Dixon, Multi-level comparative Smethod, average geometric variation- Grubbs test.The best estimated values were obtained by takingthe averages of preferred averages of all the data andanalytic data as the four central values. The bestestimated values thus calculated and complied withthe certified values rule are taken as standardvalues. An evaluation of stability of the sampleswas made by X- ray fluorescence spectrometryduring one year period. The results indicated thatthe storage stability of this standard referencematerial was satisfactory.