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本文以熔融制样技术和数学校正分析方法的X射线荧光光谱实验手段,对长江口水域3个站位的10个常量元素进行定量分析。这10个常量元素分别是钠、镁、铝、硅、磷、钾、钙、钛、锰和铁,获得较好结果。分析的检出限达到10~(-5)左右;精密度用变差系数K表示,K<0.03826,因此具有较高精密度。最大分析相对误差是0.27%。此外本文还应用无标分析法的X射线衍射实验手段对同样3个站位样品进行形态物相定量分析。分析结果表明,长江口3个站位中沉积物主要成分是α-石英,其次是钠长石、高岭土、绿泥石、伊利石、方解石和蒙脱石等。分析结果与X射线荧光光谱元素定量分析结果基本一致,绝大部分物相定量分析误差小于15%。本文对于了解长江口存在的离子交换、吸附、解吸和絮凝等化学作用过程,均具有重要参考价值。FL指流气正比计数器。*PHA指脉冲高度分析器。1.2X射线荧光光谱法制样方法将试样研磨均匀后,在105℃条件下,烘干2h,准确称取1.000g试样;另外加入Li2B4O72.400g、LiBO24.400g和NH4NO31.0g;将上述混合物放置在5%Au-95%Pt坩埚内均匀混合,随后在850℃条件下预氧化10min,再在1200℃
In this paper, 10 constant elements of three stations in the Yangtze River Estuary were quantitatively analyzed by means of X-ray fluorescence spectrometry with melting sample preparation and mathematical correction analysis. The 10 constant elements are sodium, magnesium, aluminum, silicon, phosphorus, potassium, calcium, titanium, manganese and iron, respectively, with good results. The detection limit of the analysis reached about 10 ~ (-5); the precision was expressed by the coefficient of variation K, K <0.03826, so it had higher precision. The maximum relative error of analysis is 0.27%. In addition, the paper also uses the X-ray diffraction experiment method without standard analysis method to perform the phase quantitative analysis of the same three station samples. The results show that the main sediments in the three stations of the Yangtze River Estuary are α-quartz, followed by albite, kaolin, chlorite, illite, calcite and montmorillonite. The results of the analysis are basically the same as those of the X-ray fluorescence spectrometry. The error of quantitative analysis of most of the phases is less than 15%. This article has important reference value for understanding the chemical process of ion exchange, adsorption, desorption and flocculation in the Yangtze Estuary. FL refers to the gas proportional counter. * PHA refers to the pulse height analyzer. 1.2X-ray fluorescence spectrometry sample preparation After grinding the sample evenly, at 105 ℃ conditions, drying 2h, accurately weighed 1.000g sample; addition of Li2B4O72.400g, LiBO24.400g and NH4NO31.0g; The above mixture was uniformly mixed in a 5% Au-95% Pt crucible, followed by pre-oxidation at 850 ° C for 10 minutes and then at 1200 ° C