Determination of Nb and Re in High Purity Tungsten by Precipitation Separation-Inductively Coupled Plasma Mass Spectrometry

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Fig. 1. The interference on Nb and Re of W standard solution with different concentrations

Fig. 2. The influence of the amount of precipitant on the residual amount of tungsten

Fig. 3. The effect of the amount of buffer solution on the residual amount of tungsten

Fig. 4. The effect of aging time on the residual amount of tungsten

ICP-MS工作仪器参数	数值	ICP-OES工作仪器参数	数值
RF功率/W	1 550	RF功率/W	1 200
采样深度/mm	8.0	等离子体气流量/(L·min^-1)	15.0
载气流量/(L·min^-1)	0.90	辅助气流量/(L·min^-1)	1.00
稀释气流量/(L·min^-1)	0.35	雾化气流量/(L·min^-1)	0.70
泵速/(r·s^-1)	0.20	泵速/(r·min^-1)	12
测量方式	跳峰	观测高度/mm	8
扫描次数	3	积分时间/s	5
积分时间/s	0.1	-	-

Table 1. Operation parameters of ICP-MS and ICP-OES

Table 2. The mass spectrum interference of the determination of Nb and Re in high-purity tungsten by ICP-MS

Table 3. The selection of internal standard elements

Table 4. The limits of detection and quantitation(μg·g^-1)

待测元素	测定值/ (μg·g^-1)	RSD/ %	加标量/ (μg·g^-1)	回收值/ (μg·g^-1)	回收率/%
Nb	0.024	12	0.050	0.078	108
Re	0.21	4.8	0.20	0.42	105

Table 5. Precision and recovery of the method

待测元素	测定值/ (μg·g^-1)	RSD/%	加标量/ (μg·g^-1)	加标回收率/%
Nb	0.021	8.8	0.050	109
Re	9.42	1.0	10.00	100

Table 6. The analytical results of sample

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