微柱流动注射在线预浓集与电热原子吸收光谱法的全自动联用

Automatic Hyphenated Technique of Flow Injection On line Preconcentration with Microcolumn Electrothermal AAS

研究了一种流动注射在线预浓集、分离与电热原子吸收光谱全自动联用的最新技术．在最优化条件下，采用９μＬ微柱预浓集，８０μＬ甲醇洗脱剂可将吸附于微柱上的待测物定量洗脱并全部自动导入石墨炉原子化器．富集倍数高达６４．进行了河水和海水标准参考物质中痕量铅的测定，无基体干扰，不必使用基体改进剂，结果满意．检出限４．５ｎｇ／Ｌ，回收率９７～１０４％，相对标准偏差为２．９％．

A new fully automatic hyphenated technique of on line microcolumn preconcentration separation and electrothermal AAS was studied. When a microcolumn with 9 μL of solid sorbent was used, the adsorbed analyte can be eluted quantitatively with only 80μL of methanol eluent and the total eluate volume was transfered into the graphite atomizer. A enrichment factor of 64 and detection limit (3σ) of 4.5ng L -1 can be achieved. Sea water was analyzed, with a recovery of 98.0%. Results obtained for the standard reference materials of SLRS 1 riverine water and CASS 1 sea water agree well with certified values.