摘要
使用传统的电感耦合等离子体质谱法(ICP-MS)测定磷酸中杂质元素存在严重的多原子离子干扰,本文利用碰撞反应界面技术(CRI)有效地消除或降低了多原子离子干扰。实验表明,直接稀释磷酸样品后,采用89 Y-115In-209 Bi三内标元素可补偿仪器的信号漂移和基体效应;采用无CRI模式可直接测定Mg、Al、Sr、Cd和Pb;采用He作为碰撞反应气可消除V、Cr、Mn、Co、Ni、Cu、Zn和As的质谱干扰,并确定最佳He流量为90mL/min;采用H2作为碰撞反应气可消除Fe和Se的质谱干扰,并确定最佳H2流量为70mL/min。方法检出限为0.5～10ng/g,加标回收率为80%～120%。采用本方法测定工业和食品级磷酸样品,测得结果和其它方法一致,相对标准偏差不大于6.6%(n=6),适用于大批量样品的分析。
There is serious interference from polyatiomic ions in the determination of impurity elements in phosphoric acid by traditional inductively coupled plasma mass spectrometry（ICP-MS）.In this paper,the interference was effectively eliminated or reduced by collision reaction interface technique（CRI）.The experiments indicated that,after the phosphoric acid sample was diluted directly,the instrument signal shift and matrix effect could be compensated with 89Y-115In-209Bi as internal standard elements;Mg,Al,Sr,Cd and Pb could be determined by non CRI mode;the spectral interference of V,Cr,Mn,Co,Ni,Cu,Zn and As could be eliminated with He as reaction gas,and the optimal flow rate of He was optimized as 90 mL/min;the spectral interference of Fe and Se could be eliminated with H2 as reaction gas,and the optimal flow rate of H2 was optimized as 70 mL/min.Detection limits of this method were 0.5-10 ng/g,and the recoveries of standard addition were 80%-120%.The proposed method was applied to determine industrial-level and food-level phosphoric acids samples.The results were consistent with those obtained by other methods,and the relative standard deviations（RSD） were less than 6.6%（n=6）,which could meet the requirement for batch sample analysis.
出处
《冶金分析》
CAS
CSCD
北大核心
2012年第12期15-21,共7页
Metallurgical Analysis
基金
广西自然科学基金项目资助(桂科自0991295)
防城港市科学研究与技术开发计划项目资助(防科20123611)
关键词
磷酸
杂质元素
电感耦合等离子体质谱法
碰撞反应
phosphoric acid
impurity elements
inductively coupled plasma mass spectrometry
collision reaction
作者简介
陈永欣（1981-），男，工程师，研究方向：光谱分析方法开发和应用；E—mail：henyx81@yahoo．com．cn
