电感耦合等离子体原子发射光谱法测定微孔碳分子筛及其洗脱液中的金属元素含量  

Determination of metals in microporous carbon molecular sieve and its eluent by inductively coupled plasma atomic emission spectrometry

作　　者：黎国兰[1] 陈民助[2] 李松[1,2] 李桂英[2] 胡常伟[2] 

机构地区：[1]绵阳师范学院化学与化学工程学院,四川绵阳621000 [2]四川大学化学学院绿色化学与技术教育部重点实验室,四川成都610064

出　　处：《冶金分析》2009年第8期29-33,共5页Metallurgical Analysis

基　　金：国家自然科学基金项目(20502017)

摘　　要：通过电感耦合等离子体原子发射光谱法(ICP-AES)与试样不同预处理方法相结合分别测定了微孔碳分子筛(CMS)及其洗脱剂(HCl+HF+H2O2)中的Fe,Al,Na,Zn,Ca,Mg,K,Cu8种元素。考察了样品预处理方法对测定结果的影响。结果表明:采用灰化法处理样品除Zn测定结果偏低外,其它元素的测定结果都较酸洗脱法高;在酸洗脱法中,以HCl+HF+H2O2为洗脱剂较用HCl,HNO3,HCl+HF,HCl+HNO3的洗脱效果好。试验选择用灰化法处理样品以测定微孔碳分子筛总体的金属元素含量;用HCl+HF+H2O2为洗脱剂以测定从微孔碳分子筛中洗脱下来的金属元素含量。用该法测定碳分子筛试样总体和洗脱的Fe,Na,Zn,Ca,Mg,K,Cu,平均加标回收率分别为91%～120%和97%～110%,相对标准偏差分别为0.8%～5.6%和1.5%～4.3%。实验还表明,通过用不同的溶液选择性洗脱表面的金属,并与ICP-AES测定相结合有望成为分析多孔碳材料表面的金属元素分布和形态的一种方法。Inductively coupled plasma atomic emission spectrometry （ICP-AES） assisted with the various pretreatments of sample was employed for the simultaneous determination of Fe, A1, Na, Zn, Ca, Mg, K and Cu in microporous carbon molecular sieve and its eluent（HCl＋HF＋ H2O2 ）. The effect of pretreatment methods on the test results was investigated. The results indicated that the determination results of metal elements by pretreating sample with ashing method were higher than those with acid leaching method,except that the result of Zn was low. Among these solutions, the mixture acid with oxidant, like HCl＋ HF＋ H2O2 was more efficient to dissolve the metals than HCl, HNO3, HCl＋ HF and HCl＋ HNO3, and thus are the most suitable for the leaching of the metals in the carbon materials. The established method was applied to determine the content of Fe,Na,Zn,Ca,Mg,K,Cu in one microporous carbon molecular sieve sample and its eluent. 91.0%--120% and 97%--110% of average recoveries and 0. 8%--5.6% and 1.5 %--4.3 0% of RSDs were obtained, respectively. The experimental results also showed that it should be a feasible method for the analysis of distribution and speciation of metal elements on the surface of porous carbon materials by ICP-AES assisted with selective elution of surface metals with various solutions.

关 键 词：电感耦合等离子体原子发射光谱法 碳分子筛 洗脱液 金属元素 

分 类 号：O657.31[理学—分析化学]