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Determination of inorganic nutrients in wheat flour by laser-induced breakdown spectroscopy and energy dispersive X-ray fluorescence spectrometry

机译:激光诱导击穿光谱和能量色散X射线荧光光谱法测定小麦粉中的无机养分

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Laser-induced breakdown spectroscopy (UBS) and energy dispersive X-ray fluorescence spectrometry (EDXRF) were evaluated for the determination of P, K, Ca, Mg, S, Fe, Cu, Mn and Zn in pressed pellets of wheat flours. EDXRF and LIBS calibration models were built with analytes mass fractions determined by inductively coupled plasma optical emission spectrometry after microwave-assisted acid digestion in a set of 25 wheat flour laboratory samples. Test samples consisted of pressed pellets prepared from wheat flour mixed with 30% mm~(-1) cellulose binder. Experiments were carried out with a LIBS setup consisted of a Q-switched Nd:YAG laser and a spectrometer with Echelle optics and ICCD, and a benchtop EDXRF system fitted with a Rh target X-ray tube and a Si(Li) semiconductor detector. The correlation coefficients from the linear calibration models of P, K, Ca, Mg, S, Fe, Mn and Zn determined by LIBS and/or EDXRF varied from 0.9705 for Zn to 0.9990 for Mg by LIBS, and from 0.9306 for S to 0.9974 for K by EDXRF. The coefficients of variation of measurements varied from 1.2 to 20% for LIBS, and from 0.3 to 24% for EDXRF. The predictive capabilities based on RMSEP (root mean square error of prediction) values were appropriate for the determination of P, Ca, Mg, Fe, Mn and Zn by LIBS, and for P, K, S, Ca, Fe, and Zn by EDXRF. In general, results from the analysis of N1ST SRM 1567a Wheat flour by LIBS and EDXRF were in agreement with their certified mass fractions.
机译:评价了激光诱导击穿光谱法(UBS)和能量色散X射线荧光光谱法(EDXRF)以确定压制的小麦粉中P,K,Ca,Mg,S,Fe,Cu,Mn和Zn的含量。用微波辅助酸消解后,在一组25个小麦粉实验室样品中,通过电感耦合等离子体光发射光谱法测定的分析物质量分数建立了EDXRF和LIBS校准模型。测试样品由混合有30%mm〜(-1)纤维素粘合剂的小麦粉制成的压制小丸组成。实验是使用LIBS装置进行的,该装置由Q开关Nd:YAG激光器,带有Echelle光学器件和ICCD的光谱仪以及台式EDXRF系统组成,该系统配有Rh目标X射线管和Si(Li)半导体探测器。通过LIBS和/或EDXRF确定的P,K,Ca,Mg,S,Fe,Mn和Zn线性校准模型的相关系数从Zn的0.9705到LIBS的Mg的0.9990,以及S的0.9306到0.9974的线性对于EDXRF的K。对于LIBS,测量的变化系数从1.2到20%不等,对于EDXRF,测量的变化系数从0.3到24%不等。基于RMSEP(预测的均方根误差)值的预测能力适用于通过LIBS测定P,Ca,Mg,Fe,Mn和Zn,以及用于P,K,S,Ca,Fe和Zn的测定。 EDXRF。通常,LIBS和EDXRF对N1ST SRM 1567a小麦粉的分析结果与它们的认证质量分数一致。

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