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Determination of Cd and Cr in tannin samples by high-resolution continuum source graphite furnace atomic absorption spectrometry and direct solid sample sequential analysis (HR-CS SS-GF AAS)

机译:高分辨率连续谱源石墨炉原子吸收光谱法和直接固体样品顺序分析法(HR-CS SS-GF AAS)测定单宁样品中的Cd和Cr

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摘要

A fast and reliable analytical method for the sequential determination of Cd and Cr in tannin samples by high-resolution continuum source graphite furnace atomic absorption spectrometry with direct solid sampling from the same sample aliquot (HR-CS SS-GF AAS) is proposed. A pyrolysis temperature of 400 degrees C and atomisation temperature of 1500 degrees C were used for the determination of Cd; no losses of Cr were observed at these temperatures. After the atomisation of Cd, the wavelength was changed and Cr was atomised at 2500 degrees C. Several studies with different modifiers were performed, but no chemical modifier was needed. Calibration was achieved using aqueous standards. The linearity of the response, performed by evaluating the absorbance value relative to the sample mass, was investigated as well. Relative standard deviation (RSD) values lower than 15% were found, which are acceptable for direct analysis. The parameters of merit were: a characteristic mass of 0.3 pg and 2.2 pg for Cd and Cr, respectively; the limit of detection (LOD) of 0.5 mu g kg(-1) and 17 mu g kg(-1) for Cd and Cr, respectively; the limit of quantification (LOQ) of 2 mu g kg(-1) and 57 mu g kg(-1) for Cd and Cr, respectively. The accuracy was validated by analysing three certified reference materials (tea, pine needles and bush branches). The results were not statistically different from the certified values at a 95% confidence level. Therefore, calibration using aqueous standards is suitable for this application. This method is simple, fast and suitable for routine analysis.
机译:提出了一种快速可靠的分析方法,该方法通过高分辨率连续谱源石墨炉原子吸收光谱法从同一样品等分试样(HR-CS SS-GF AAS)中进行直接固体采样,顺序测定鞣质中的镉和铬。 Cd的测定采用400°C的热解温度和1500°C的雾化温度。在这些温度下没有观察到Cr的损失。 Cd雾化后,改变波长,并在2500摄氏度下雾化Cr。进行了几种使用不同改性剂的研究,但不需要化学改性剂。使用水性标准液进行校准。还研究了通过评估吸光度值相对于样品质量的响应的线性。发现相对标准偏差(RSD)值低于15%,这对于直接分析是可以接受的。优点参数为:Cd和Cr的特征质量分别为0.3 pg和2.2 pg;镉和铬的检出限(LOD)分别为0.5μg kg(-1)和17μgkg(-1); Cd和Cr的定量限(LOQ)分别为2μg kg(-1)和57μgkg(-1)。通过分析三种认证参考材料(茶,松针和灌木树枝)验证了准确性。在95%的置信水平下,结果与认证值在统计学上没有差异。因此,使用水性标准液进行校准适用于此应用。该方法简单,快速,适合常规分析。

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