PISI-AFS法测定煤、煤矸石和粉煤灰中微量锗  

Determination of trace germanium in coal,coal gangue and fly ash by peristalsis injection and shielded ignition-atomic fluorescence spectrometry

作　　者：刘飞[1,2] 李增强[1,2] 陈欣娟[1,2] 张跃文 王晓玉 

机构地区：[1]国土资源部煤炭资源勘查与综合利用重点实验室,陕西西安710021 [2]陕西煤田地质化验测试有限公司,陕西西安710054

出　　处：《洁净煤技术》2016年第1期14-19,共6页Clean Coal Technology

基　　金：国土资源部煤炭资源勘查与综合利用重点实验室资助项目(ZP2013-7)

摘　　要：为提高煤、煤矸石和粉煤灰中总锗的测定速度,减少有机萃取剂用量,通过优化仪器工作条件,采用混合酸消解样品、蠕动进样、屏蔽式点火等方法,研究了PISI-AFS法测定煤、煤矸石和粉煤灰中微量锗含量的准确度和精密度。结果表明,该方法检出限为0.0425μg/g,相对标准偏差RSD为1.42%,标准工作曲线的线性范围达到1-400 ng/g,锗的加标回收率为98.92%-103.79%。该法与GB/T 8207—2007中的蒸馏分离-苯芴酮分光光度法的测定值的相对误差小于5%。离子干扰试验中,该法测定值的相对误差未超过±5%,说明PISI-AFS法适用于定量测定煤、煤矸石和粉煤灰中微量锗,准确度和精密度均较高。In order to improve determination speed of total germanium in coal,coal gangue and fly ash,and reduce organic solvent amount,the peristalsis injection and shielded ignition- atomic fluorescence spectrometry（ PISI- AFS） was used to determine the trace germanium content in coal,coal gangue and coal ash. The results showed that the detection limit of the method was 0. 0425 μg / g,the relative standard deviation was 1. 42%（ n = 11）,the linearity range of the standard curve could reach 1 - 400 ng / g,the recovery rate of germanium ranged from 98. 92% to 103. 79%. The relative error was less than 5%,which were between the PISI-AFS and distillation-Phenylfluorone spectrophotometry in GB / T 8207—2007. In the ion interference experiment,the relative error fluctulated in a range of-5% to 5%.

关 键 词：锗 煤矸石 粉煤灰 原子荧光法 

分 类 号：TQ531[化学工程—煤化学工程]