摘要
针对国家标准测定煤中锗存在的缺点,研究了流动注射-离子交换分离-二溴邻硝基苯基荧光酮光度法测定煤中锗含量的分析方法.该法采用流动注射技术进行痕量锗的离子交换分离与富集,在0.40 mol/L的HCl介质中,Ge4+与Cl-形成络阴离子,被阴离子交换树脂交换富集,用0.60 mol/L的HNO3-1.5%柠檬酸溶液洗脱,用二溴邻硝基苯基荧光酮(DBoN-PFO)光度法测定锗,大量共存离子不干扰锗的测定.测定样品的相对标准偏差为2.67%～5.02%(n=8),加标回收率为96.39%～103.63%,方法的检出限为0.18μg/L,其准确度和精密度均满足国家标准的要求.
Aimed at solving the problem that determination of germanium in standard of China has shortcoming, a analytical method for the determination of trace germanium in coal by flow injection-ion exchange separation-4, 5- dibromo-2-nitro-phenylfluorone spectrophotometry was studied. Trace germanium was separated and preconcentrat- ed after ion exchange by flow injection in the method. In the medium of 0. 40 mol/L hydrochloric acid, Ge^4＋ re acts with Cl^- to form a anion complex which is then adsorbed on the column of alkali anion exchange resin. The anion complex is desorbed from the column with solution of 0. 60 mol/L nitric acid-1.5% citric acid and it reacts with 4, 5-dibromo-2-nitro-phenylfluorone （DBoN-PFO） to form a color complex for spectrophotometric determination of germanium, a lot of co-ions don＇t disturb the determination of germanium after separation and preconcentration. The detection limit of the method is 0. 18μg/L and the recovery of the method is founded to be 96. 39%-103.63% while the relative standard deviation （RSD） is 2. 67% -5.02% （n =8）. The precision and veracity of the method fit to restrict of GB.
出处
《煤炭学报》
EI
CAS
CSCD
北大核心
2005年第4期511-515,共5页
Journal of China Coal Society
关键词
流动注射
离子交换分离
分光光度法
煤
锗
flow injection
ion exchange separation
spectrophotometry
coal
germanium
