4-甲基-2-戊酮萃取分離-電感耦合等離子體質(zhì)譜法測定高純硒中17種雜質(zhì)元素
發(fā)布時間：2018-08-30 09:05
【摘要】：利用電感耦合等離子體質(zhì)譜法(ICP-MS)測定5N~6N(純度為99.999%~99.999 9%)高純硒中痕量雜質(zhì)元素時,硒的基體效應(yīng)明顯,影響結(jié)果的準確性。采用硝酸溶解高純硒,經(jīng)4-甲基-2-戊酮選擇性萃取硒后,對水相進行測定,建立了電感耦合等離子體質(zhì)譜法測定高純硒中的Li、Be、B、Sc、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、As、Sr、Cd、Ba、Pb共17種痕量雜質(zhì)元素的方法。實驗表明,萃取時當鹽酸濃度為7mol/L、MIBK體積為20mL和萃取時間為2min時,水相中硒的質(zhì)量濃度低于5mg/L,此時硒基體對測定的影響可忽略。方法中各元素校準曲線的線性關(guān)系均大于0.999 5,各待測元素的方法檢出限為0.2~7.0ng/g。按照實驗方法對高純硒樣品中這17種雜質(zhì)元素進行測定,測定結(jié)果的相對標準偏差(RSD,n=6)在5.0%~11.2%之間,加標回收率在91%~103%之間。
[Abstract]:In the determination of trace impurities in high purity selenium by inductively coupled plasma-mass spectrometry (ICP-MS), the matrix effect of selenium is obvious and the accuracy of the results is affected. A method for the determination of Li,Be,B,Sc,Ti,V,Cr,Mn,Co,Ni,Cu,Zn,As,Sr,Cd,Ba,Pb in high purity selenium by inductively coupled plasma mass spectrometry (ICP-MS) after selective extraction of selenium by 4-methyl-2-pentanone was developed. The results show that when the concentration of hydrochloric acid is 7 mol / L ~ (MIBK) and the extraction time is 2min, the mass concentration of selenium in aqueous phase is less than 5 mg / L, and the effect of selenium matrix on the determination is negligible. The calibration curve of each element is linear more than 0.999, and the detection limit of each element is 0.2ng / g. The relative standard deviation (RSD,n=6) of the 17 impurity elements in high purity selenium samples was between 5.0% and 11.2%, and the recovery rate was between 91% and 103%.
【作者單位】： 成都理工大學(xué);
【分類號】：O657.63;TQ125.2
本文編號：2212619
[Abstract]:In the determination of trace impurities in high purity selenium by inductively coupled plasma-mass spectrometry (ICP-MS), the matrix effect of selenium is obvious and the accuracy of the results is affected. A method for the determination of Li,Be,B,Sc,Ti,V,Cr,Mn,Co,Ni,Cu,Zn,As,Sr,Cd,Ba,Pb in high purity selenium by inductively coupled plasma mass spectrometry (ICP-MS) after selective extraction of selenium by 4-methyl-2-pentanone was developed. The results show that when the concentration of hydrochloric acid is 7 mol / L ~ (MIBK) and the extraction time is 2min, the mass concentration of selenium in aqueous phase is less than 5 mg / L, and the effect of selenium matrix on the determination is negligible. The calibration curve of each element is linear more than 0.999, and the detection limit of each element is 0.2ng / g. The relative standard deviation (RSD,n=6) of the 17 impurity elements in high purity selenium samples was between 5.0% and 11.2%, and the recovery rate was between 91% and 103%.
【作者單位】： 成都理工大學(xué);
【分類號】：O657.63;TQ125.2
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