电感耦合等离子体质谱法测定硫酸镍中痕量铊

doi:10.19964/j.issn.1006-4990.2022-0681

Abstract

Abstract:

In order to further improve the analytical accuracy of trace thallium in the field of new energy industrial production，this paper established a method to determine the content of thallium in nickel（Ⅱ） sulfate using iCAP RQ type ICP-MS.The interference of mass spectrometer introduced by this method was analyzed，which could be reduced by using interference ion kinetic energy discrimination elimination mode（KED） analysis mode，controlling the total dissolved solids（TDS） and introducing rhodium and rhenium internal standards.The total amount of soluble solids and the dissolution temperature in the pretreatment conditions were determined to be 0.2% and 210 ℃，The method validation results showed that the detection limit of the method was 0.003 6 ng/mL，the RSD of the precision test was 1.3%~2.5%，and the recovery rate was 98.4%~100.8%.In the comparison between laboratories，the RSD was 0~5.7%，and the reproducibility was good.The method was simple，rapid，and highly accurate，and could be widely used in the monitoring of thallium content in the nickel sulfate industry chain.

Key words: nickel sulfate, thallium, inductively coupled plasma mass spectrometry

CLC Number:

TQ133.54

LIAO Shuangshuang, XIE Tangfeng, GONG Qinxue, YUAN Guobin. Determination of trace thallium in nickel sulfate by inductively coupled plasma mass spectrometry[J]. Inorganic Chemicals Industry, 2023, 55(9): 121-125.

Figures/Tables 8

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References 14

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标准曲线对应质量/ 浓度（ng·mL^-1）	质量浓度/ （ng·mL^-1）	强度/ cps	标准工作曲线
0	0.00	86	f（x）=121 586.571x+86.404，R²=0.999 9
2	2.016	245 204
4	3.985	484 608
10	9.997	1 215 587
20	20.017	2 396 884

试样编号	测定值/（μg·g^-1）	平均值/ （μg·g^-1）	RSD/ %
01	0.105、0.107、0.114、0.113、0.109、0.110、 0.113、0.111、0.110、0.108、0.110	0.110	2.1
02	0.490、0.495、0.485、0.500、0.501、0.486、 0.490、0.494、0.488、0.497、0.503	0.494	1.3
03	0.044 3、0.045 8、0.046 2、0.044 6、0.045 7、0.045 6、0.046 1、0.044 7、0.046 5、0.449、0.045 3	0.045 4	1.7
04	0.024 4、0.024 5、0.024 8、0.025 3、0.025 8、 0.026 2、0.025 5、0.024 7、0.024 3、0.025 6、0.025 8	0.025 2	2.5

试样编号	铊含量/ （μg·g^-1）	加标量/ μg	测定量/ μg	回收量/ μg	回收率/ %
05	0.074	0.012 5	0.019 7	0.012 3	98.4
05	0.074	0.025 0	0.032 3	0.024 9	99.6
06	0.100	0.012 5	0.022 6	0.012 6	100.8
06	0.100	0.025 0	0.034 8	0.024 8	99.2

试样编号	内部实验室/ （μg·g^-1）	第三方实验室/ （μg·g^-1）	RSD/ %
07	0.20	0.21	3.4
08	0.33	0.31	4.4
09	0.10	0.10	0.0
10	0.63	0.62	1.1
11	0.12	0.13	5.7
平均值	0.28	0.27	2.9
COV/%	0.79	0.77	3.4
相关系数	1.00
P值（配对T检验）	0.75

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Determination of trace thallium in nickel sulfate by inductively coupled plasma mass spectrometry

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