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Simultaneous determination of Mo and Ni in wine and soil amendments by HR-CS GF AAS

机译:HR-CS GF AAS同时测定葡萄酒和土壤改良剂中的钼和镍

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The use of high-resolution continuum-source graphite furnace atomic absorption spectrometry (HR-CS GF AAS), equipped with a linear charge-coupled device (CCD) array detector, makes simultaneous determination of more than one element possible. In this work, HR-CS GF AAS was used for the simultaneous determination of Mo (313.259 nm) and Ni (313.410 nm), for which two analytical methods were developed: direct solid sample analysis for soil amendments and direct sample injection for wine samples. For both these methods, a pyrolysis temperature of 1200 ?°C and an atomization temperature of 2650 ?°C were used. Aqueous standard solutions were used for calibration. The linear correlation coefficient was higher than 0.997 for the two analytes. Detection limits of 0.05 and 0.8 ??g La?’1 for wine samples and 0.04 and 0.60 mg kga?’1 for soil amendments were found for Mo and Ni, respectively. To investigate the accuracy of the developed method, digested and undigested wine samples were evaluated with spike recovery values between 94% and 106%. For solid samples, three CRM were evaluated, and the values found for Mo were not significantly different from the certified ones; however, those for Ni were always too high. It was found that this was due to a direct line overlap of the Ni line with the Fe line. This effect was overcome by determining Fe using the unresolved analytical line doublet at 312.565/312.568 nm and subtracting this value from the total concentration (Ni + Fe) determined at 313.410 nm. Note that this interference was not observed in wine samples because of their low Fe concentration.
机译:高分辨率线性连续源石墨炉原子吸收光谱法(HR-CS GF AAS)配备了线性电荷耦合器件(CCD)阵列检测器,可以同时测定多种元素。在这项工作中,HR-CS GF AAS用于同时测定Mo(313.259 nm)和Ni(313.410 nm),为此开发了两种分析方法:用于土壤改良剂的直接固体样品分析和用于葡萄酒样品的直接样品注射。对于这两种方法,均使用了1200°C的热解温度和2650°C的雾化温度。使用水性标准溶液进行校准。两种分析物的线性相关系数均高于0.997。对于葡萄酒样品,Mo和Ni的检出限分别为0.05和0.8?g La?1,对土壤改良剂的检出限为0.04和0.60 mg kga?'1。为了研究开发方法的准确性,评估了消化和未消化的葡萄酒样品的峰值回收率在94%至106%之间。对于固体样品,评估了三种CRM,其Mo值与认证值无显着差异。但是,镍的含量总是很高。发现这是由于Ni线与Fe线的直线重叠。通过使用在312.565 / 312.568 nm处未解析的分析谱线对确定Fe,并从在313.410 nm处确定的总浓度(Ni + Fe)中减去该值,可以克服这种影响。请注意,由于葡萄酒样品中的铁含量较低,因此未观察到这种干扰。

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