有机离子相微萃取/反微萃取预富集:2-烯酰三氟丙酮- GF-AAS法测定环境水中镍

Mitsuhito Kosugi, Kenta Mizuna, Kazuto Sazawa, Takuya Okazaki, H. Kuramitz, S. Taguchi, N. Hata
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引用次数: 4

摘要

应用离子伴随相微萃取/反微萃取系统对环境水样中痕量镍进行富集、分离和检测。乙烯基三氟丙酮(HTTA)不仅作为镍的螯合剂,而且作为萃取相,即IAP的组成部分。用苯酚磺酸盐(PS−)和四甲基氢氧化铵调节40 mL样品溶液中的镍的ph值,并在三氟乙酸乙酯(TTA−)存在下通过螯合反应转化镍。当加入苄基十二烷基二甲基铵离子(C12BzDMA+)时,溶液中形成IAP悬浮液。IAP由TTA−(一种螯合试剂)、PS−(一种pH缓冲液)和C12BzDMA+(有助于提取螯合物)组成。当溶液离心时,IAP从悬浮液中分离,镍- tta螯合物被萃取到离心管的底相中。除去水相后,用100µL含磷酸的2 M硝酸溶液反萃取IAP中的镍。采用石墨炉原子吸收光谱法(GF-AAS)测定酸相。所提出的方法促进了400倍的富集。检出限为0.02µg L−1。该方法可用于河水和海水样品中镍的测定。
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Organic Ion-Associate Phase Microextraction/Back-Microextraction for Preconcentration: Determination of Nickel in Environmental Water Using 2-Thenoyltrifluoroacetone via GF-AAS
An ion-associate phase (IAP) microextraction/ back-microextraction system was applied for the enrichment, separation, and detection of trace amounts of nickel from environmental water samples. Thenoyltrifluoroacetone (HTTA) acted not only as a chelating reagent for nickel, but also as a component of the extraction phase, i.e., IAP. Nickel in a 40 mL sample solution was pH-adjusted with phenolsulfonate (PS−) and tetramethylammonium hydroxide and converted by chelation reaction in the presence of thenoyltrifluoroacetonate (TTA−). When benzyldodecyldimethylammonium ion (C12BzDMA+) was added, a suspension of IAP formed in the solution. The IAP consisted of TTA−, a chelating reagent, the PS−, a component of pH buffer, and C12BzDMA+, which helps extract the chelating complex. When the solution was centrifuged, the IAP separated from the suspension and the nickel-TTA chelate was extracted into the bottom phase of the centrifuge tube. After the aqueous phase was taken away, 100 µL of nitric acid (2 M) solution containing phosphate was used to back-microextract nickel from the IAP. The acid phase was measured via graphite-furnace atomic-absorption spectrometry (GF-AAS). The proposed method facilitated a 400-fold enrichment. The limit of detection was 0.02 µg L−1. The proposed method was applied for the determination of nickel in river water and seawater samples.
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