摘要
建立了样品经盐酸、氢氟酸、硝酸、高氯酸分解后直接用火焰原子吸收(FAAS)或电感耦合等离子体发射光谱(ICP-OES)来测定锌冶炼石膏渣中Zn、Mg、K、Na的两种分析方法,用这两种方法测定国家标准样品,测定结果与标准值相符。对锌冶炼石膏渣样品进行多组平行实验和加标回收实验,两种方法测定Zn、Mg、K、Na的相对标准偏差均小于5%,加标回收率均在95%~105%,两种方法均有较好的精密度和准确度。FAAS测定Zn、Mg、K、Na的检出限分别为(0.031、0.022、0.019、0.015)μg/mL,测定下限分别为(0.10、0.074、0.063、0.052)μg/mL,样品测定范围分别为0.01%~0.40%、0.007 4%~0.40%、0.006 3%~0.40%、0.005 3%~0.40%;ICP-OES测定Zn、Mg、K、Na的检出限分别为(0.005 3、0.005 1、0.023、0.01 7)μg/mL,测定下限分别为(0.018、0.018、0.077、0.057)μg/mL,样品测定范围分别为0.001 8%~1.00%、0.001 8%~1.00%、0.007 7%~0.20%、0.005 7%~0.20%。
Two kinds of analysis methods were established, which samples were decomposed by hydrochloric acid, hydrofluoric acid, nitric acid, perchloric acid, then Zn, Mg, K, Na in zinc smelting by-product gypsum residues were analyzed directly by flame atomic absorption and inductively coupled plasma emission spectrometry, the national standard samples were tested by these two kinds of methods, the testing results were in conformity with the standard values. Multiple group parallel experiments and standard addition test of zinc smelting gypsum residues were carried out, by using these two kinds of methods, the relative standard deviation for determination of Zn, Mg, K, Na all less than 5%, the adding standard recovery rate all in between 95% ~105%, two kinds of methods all have good precision degree and accuracy degree. The detection limit measured by FAAS of Zn, Mg, K, Na separately is( 0.031、 0.022、 0.019、0.015) μg/mL,, the lower limit of measurement separately is( 0.10、 0.074、 0.063、 0.052) μg/mL, the measuring range of sample separately is 0.01%~0.40%, 0.0074%~0.40%, 0.0063%~0.40%, 0.0053%~0.40%;the detection limit measured by ICP-OES of Zn, Mg,K, Na separately is( 0.0053、 0.0051、 0.023、 0.017) μg/mL, the lower limit of measurement separately is( 0.018、 0.018、 0.077、0.057) μg/mL, the measuring range of sample separately is 0.0018%~1.00%, 0.0018%~1.00%, 0.0077%~0.20%, 0.0057%~0.20%.
作者
龙兴杰
罗开良
LONG Xing-jie;LUO Kai-liang(Yun-Tin Wenshan Zinc and Indium Smelting Co.,Ltd.,Wenshan,Yunnan 663700,China)
出处
《云南冶金》
2022年第6期122-127,共6页
Yunnan Metallurgy
关键词
锌冶炼
石膏渣
电感耦合等离子体发射光谱
火原子吸收
zinc smelting
gypsum residues
inductively coupled plasma emission spectroscopy
flame atomic absorption
