分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
9期
1306-1312
,共7页
原子发射光谱%微波诱导等离子体%表面进样%基体辅助%环境分析
原子髮射光譜%微波誘導等離子體%錶麵進樣%基體輔助%環境分析
원자발사광보%미파유도등리자체%표면진양%기체보조%배경분석
Atomic emission spectrometry%Microwave induced plasma%Surface sampling%Matrix assisted%Environmental analysis
采用基体辅助等离子体表面进样原子发射光谱技术对环境样品中的13种金属元素( Ag, Au, Ba, Cd, Cr, Cu, Eu, La, Mn, Ni, Pb, Sr, Y)进行检测。实验采用滤纸作为样品基体,样品直接滴加在滤纸上。将等离子体射流尾焰烧蚀滤纸表面,滤纸受热燃烧并释放出燃烧热,样品在等离子体辐射热和滤纸燃烧热的共同作用下原子化并激发,即可得到样品的特征光谱。液/固态样品均采用表面进样的方式实现样品引入,无需复杂的流动进样系统,并简化了繁琐的样品处理过程。本方法具有分析速度快(≤15 s)、用样量少(微升/微克级)、装置简洁、操作简单等优点,可实现对大量环境样品的现场高通量分析。在实验优化条件下,样品体积为1μL 时,本方法对以上13种元素的检出限为1.0~88 ng/mL,相对标准偏差为2.3%~6.8%(n=10)。该技术成功用于水样、土壤、海底沉积物等环境样品中金属元素的分析,结果均与理论值吻合。
採用基體輔助等離子體錶麵進樣原子髮射光譜技術對環境樣品中的13種金屬元素( Ag, Au, Ba, Cd, Cr, Cu, Eu, La, Mn, Ni, Pb, Sr, Y)進行檢測。實驗採用濾紙作為樣品基體,樣品直接滴加在濾紙上。將等離子體射流尾燄燒蝕濾紙錶麵,濾紙受熱燃燒併釋放齣燃燒熱,樣品在等離子體輻射熱和濾紙燃燒熱的共同作用下原子化併激髮,即可得到樣品的特徵光譜。液/固態樣品均採用錶麵進樣的方式實現樣品引入,無需複雜的流動進樣繫統,併簡化瞭繁瑣的樣品處理過程。本方法具有分析速度快(≤15 s)、用樣量少(微升/微剋級)、裝置簡潔、操作簡單等優點,可實現對大量環境樣品的現場高通量分析。在實驗優化條件下,樣品體積為1μL 時,本方法對以上13種元素的檢齣限為1.0~88 ng/mL,相對標準偏差為2.3%~6.8%(n=10)。該技術成功用于水樣、土壤、海底沉積物等環境樣品中金屬元素的分析,結果均與理論值吻閤。
채용기체보조등리자체표면진양원자발사광보기술대배경양품중적13충금속원소( Ag, Au, Ba, Cd, Cr, Cu, Eu, La, Mn, Ni, Pb, Sr, Y)진행검측。실험채용려지작위양품기체,양품직접적가재려지상。장등리자체사류미염소식려지표면,려지수열연소병석방출연소열,양품재등리자체복사열화려지연소열적공동작용하원자화병격발,즉가득도양품적특정광보。액/고태양품균채용표면진양적방식실현양품인입,무수복잡적류동진양계통,병간화료번쇄적양품처리과정。본방법구유분석속도쾌(≤15 s)、용양량소(미승/미극급)、장치간길、조작간단등우점,가실현대대량배경양품적현장고통량분석。재실험우화조건하,양품체적위1μL 시,본방법대이상13충원소적검출한위1.0~88 ng/mL,상대표준편차위2.3%~6.8%(n=10)。해기술성공용우수양、토양、해저침적물등배경양품중금속원소적분석,결과균여이론치문합。
A novel method for the determination of metallic elements in environmental samples was developed based on the matrix-assisted plasma surface sampling atomic emission spectrometry ( AES system) . A piece of filter paper was used as sample substrate. By direct interaction of the plasma tail plume with the filter paper surface, the filter paper absorbed energy from the plasma source and released combustion heating to the analytes originally present on its surface, thus to promote the atomization and excitation process. Surface sampling was performed in both cases of liquid and solid state analytes. Therefore, no flow injection system was required and sample pretreatment process was simplified. The proposed method provides several advantages, including fast analysis speed ( about 240 samples/h ) , little sample consumption (μL or μg level) , simplicity in instrument design, and also ease of system operation. These advantages made it attractive as a potential miniaturized AES system for in situ and high-throughput elemental analyses. Quantitative analysis of metal ions were achieved in this study for elements Ag, Au, Ba, Cd, Cr, Cu, Eu, La, Mn, Ni, Pb, Sr and Y. Under optimal conditions, the LOD values of the 13 elements ranged from 1. 0 to 88 μg/L. The repeatability, expressed as relative standard deviation ( RSD) from 10 replicates, ranged from 2. 3% to 6. 8%. To validate the proposed method, the system was employed to determine metal elements in standard reference materials of environmental samples. The content of each element was well in agreement with the certified values.