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研究了微波消解-氢化物发生-原子荧光光谱法联合测定脱盐乳清粉中砷和汞,建立了脱盐乳清粉用微波消解的最佳分析条件,此方法灵敏度高,准确度好。在最佳条件下,以50g/L硫脲+50g/L抗坏血酸为预还原剂,荧光强度与砷浓度在0.0362ng·mL-1～100ng·mL-1范围内呈线性关系,检出限达0.0362 ng·mL-1,荧光强度与汞浓度在0.0282ng·mL-1～50ng·mL-1范围内呈线性关系,检出限达0.0282 ng·mL-1;测定8个脱盐乳清粉样品中砷汞,相对标准偏差:砷为1.59以下,汞为1.53以下;回收率:砷为90.8%～115.0%,汞为92.2%～110.5%。
The microwave digestion - hydride generation - atomic fluorescence spectrometry was combined with the determination of arsenic and mercury in demineralized whey powder. The optimum analytical conditions for the demineralization of desalted whey powder were established. The method has high sensitivity and good accuracy. Under the optimal conditions, the fluorescence intensity was linear with the concentration of arsenic in the range of 0.0362 ng · mL -1 -100 ng · mL -1 with 50 g / L thiourea + 50 g / L ascorbic acid as the prereducing reducing agent. The detection limit 0.0362 ng · mL-1. The fluorescence intensity was linear with the concentration of mercury in the range of 0.0282 ng · mL-1 to 50 ng · mL-1 with the detection limit of 0.0282 ng · mL-1. Eight demineralized whey powder samples In arsenic and mercury, the relative standard deviations were as follows: arsenic was below 1.59 and mercury was below 1.53. The recoveries were 90.8% ~ 115.0% for arsenic and 92.2% ~ 110.5% for mercury.