Rapid on-line preconcentration and suppressed micro-bore ion chromatography of part per trillion levels of perchlorate in rainwater samples
Rapid on-line preconcentration and suppressed micro-bore ion chromatography of part per trillion levels of perchlorate in rainwater samples
复制标题
DOI：
10.1016/j.aca.2006.01.038
复制
发表时间：
2006-05-10
影响因子：
6.2
通讯作者：
Paull, Brett
中科院分区：
文献类型：
--
作者：
Barron, Leon;Nesterenko, Pavel N.;Paull, Brett
建立了一种快速测定雨水和饮用沃茨中高氯酸盐的方法。在优化的方法中，采用在线预浓缩技术，使用10 mm x 4.6 mm Phenomenex Onyx单片保护柱，（N-十二烷基-N，N-二甲基铵基）十一烷酸酯用于选择性预浓缩，随后洗脱到固定体积的进样环中（浓缩柱的“中心切割"），并使用IonPac AS 16（250 mm x 2 mm）阴离子交换柱和氢氧化钾浓度梯度进行分离。离线优化研究表明，涂层整料显示近定量回收高达50 μ g/L高氯酸盐水平从试剂水中制备的标准。在线预浓缩高氯酸盐得到的检测限下降到56纳克/升试剂水，70和80纳克/升之间的雨水样品和2.5微克/升，在未经预处理的饮用水。经过额外的样品硫酸盐/碳酸盐去除步骤后，在饮用水中也可以观察到低ng/L的高氯酸盐浓度。完整的在线方法显示了n = 10次重复运行R.S.D.的重现性。
The development of a rapid method for the determination of perchlorate in rain and drinking waters is presented. In the optimised method, an on-line preconcentration technique was employed utilising a 10 mm x 4.6 mm Phenomenex Onyx monolithic guard cartridge coated with (N-dodecyl-N,N-dimethylammonio)undecanoate for selective preconcentration, with subsequent elution into a fixed volume injection loop ('heart-cut' of the concentrator column eluate) and separation using an IonPac AS 16 (250 mm x 2 mm) anion exchange column and a potassium hydroxide concentration gradient. Off-line optimisation studies showed that the coated monolith displayed near quantitative recovery up to 50 mu g/L perchlorate level from standards prepared in reagent water. On-line preconcentration of perchlorate obtained detection limits down to 56 ng/L in reagent water, between 70 and 80 ng/L in rainwater samples and 2.5 mu g/L in non-pretreated drinking water. After an additional sample sulphate/carbonate removal step, low ng/L perchlorate concentrations could also be observed in drinking water. The complete on-line method exhibited reproducibility for n = 10 replicate runs of R.S.D.