Abstract:The conventional sample preparation method by pressed powder pellet is a simple, efficient, and environmentally friendly technique. However, there are some problems when it is used for the preparation of some sediment samples such as rough sample surface and easy peeling of powder. The pressure which was higher than the traditional value was adopted for sample preparation. A method for determination of 28 major and trace components (including sulfur, sodium oxide, magnesium oxide, aluminum oxide, silicon dioxide, phosphorus pentaoxide, potassium oxide, calcium oxide, titanium dioxide, manganese oxide, ferric oxide, cobalt, nickel, copper, zinc, vanadium, chromium, gallium, niobium, zirconium, yttrium, strontium, rubidium, lead, barium, lanthanum, neodymium, and hafnium) in marine sediment samples was established by X-ray fluorescence spectrometry (XRF). The effect of pressure at 300 kN and 1 600 kN on the sample preparation was discussed. The back propagation (BP) neural network model was introduced to correct the matrix effect of major components based on its nonlinear fitting ability. The results showed that when the sample was prepared at pressure of 1 600 kN, the surface was dense and smooth without cracks and powder dropping. Moreover, the sample preparation repeatability and the measurement precision were both significantly improved. The data set of 17 components in 55 certified reference materials was used as training sample to establish the genetic algorithm-BP neural network prediction model for the major and minor components in marine sediment. The actual sample with relatively low components was determined continuously for 12 times according to the experimental method. The detection limit of method was calculated between 0.63 μg/g and 634 μg/g. The results of precision tests indicated that the relative standard deviations (RSD, n=7) were between 0.16% and 25.1%. The proposed method was applied to the analysis of marine sediment actual samples, and the results were consistent with those obtained by the national standard methods, which could meet the requirements of simultaneous and accurate determination of multiple components in marine sediment samples.
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