微波消解-ICP-AES法测定菜油中P、S

Determination of phosphorous and sulfur in rapeseed oil by microwave digestion and ICP-AES

采用微波加热,在高温高压下酸消解样品,运用电感耦合等离子体原子发射光谱法(ICP-AES)同时测定菜油中P、S。本法选用紫外区谱线P178.221nm、S180.669nm,避免了基体中存在的Fe、Zn、Al、Cu、Mn、Ca等元素的光谱干扰。实验通过用纯氮吹扫光谱仪光路的方法消减空气中氧对紫外线的吸收,获得了足够的灵敏度。该方法简便、快速,稳定可靠,P、S检出限分别为0.067、0.078μg/ml,RSD为1.35%～5.05%,回收率为89.0%～100.9%。

Rapeseed oil samples were dig ested by acid in a microwave system under hig h temperature and hig h pressure,and then ICP-AES was applied to the determination of phosphorous and sulfur in the samples.In this method,ultraviolet line P178.221nm and S180.669nm were measured,which avoids serious spectrum interferences of Fe,Zn,Al,Cu,Mn,Ca etc in matrix.By purg ing lig ht route of spectrog raph with N 2 ,it eliminated oxyg en's absorption to ultraviolet lig ht and g ained g ood sensitivities.The proposed method is simple and rapid with g reat reliability.The detection limits of phosphorous and sulfur were0.067and0.078mg/ml,respectively.The RSD is in the rang e of 1.35%～5.05%,and the recovery is in the rang e of 89.0%～100.9%.