样品经硝酸和氢氟酸分解后,以高纯钴为基体配制校准系列溶液,在电感耦合等离子体原子发射光谱仪上测定了样品溶液中磷含量.通过试验确定了酸度、样品提升量、雾化气流速、功率、观测高度、分析谱线等分析条件.铌和锆的干扰试验结果表明,样品中的铌和锆不影响磷含量的测定.考察了快速自动谱线拟合技术(FACT),结果表明,使用该技术能够消除Co 178.205 nm谱线对P 178.222 nm的干扰.在用P 178.222 nm和P 213.618 nm作分析线测定磷时,方法的检出限分别为0.000 6％和0.000 5％(相对于0.2 g样品,定容至50mL),加标回收率在93％～112％之间,相对标准偏差小于10％(n=7).本方法测定样品中磷含量的结果同光度法测定结果相符.%The samples were decomposed by nitric acid and hydrofluoric acid. The calibration series solution was prepared using high-purity cobalt as matrix. Then, the content of phosphorus in sample solution was determined by inductively coupled plasma atomic emission spectrometry. The analytical conditions were obtained, including acidity, sample uptake, atomization gas flow rate, power, observation height and analytical lines. The interference test of niobium and zirconium was conducted. The results showed that the niobium and zirconium in sample did not interfere with the determination of phosphorus content. The fast automated curve-fitting technique (FACT) was investigated. The results showed that, the interference of Co 178. 205 nm with P 178. 222 nm could be eliminated by this technique. The content of phosphorus was determined under optimal conditions. The detection limits of this method was 0. 000 6% of P 178. 222 nm and 0. 000 5% of P 213. 618 nm (for 0. 2 g of sample in 50 mL). The recoveries of standard addition were 93%-112%. The relative standard deviation (RSD) was smaller than 10% (n=7). The determination results of phosphorus content in sample were consistent with those obtained by photometry.
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