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通过两步接枝法制备了一种季铵型离子交换纤维PP-g-DMAEMA-Br,将其用作纤维管内固相微萃取方法中的吸附剂,并结合紫外-可见分光光度法富集检测水溶液中痕量的Cr(Ⅵ),开发了一套预富集检测水中痕量Cr(Ⅵ)的新工艺。研究了样品流速,p H值对纤维微柱吸附水中痕量Cr(Ⅵ)的影响,以及洗脱剂类型、浓度、体积、洗脱剂流速对Cr(Ⅵ)洗脱回收率的影响。在最佳条件下,该方法对于Cr(Ⅵ)最低检测限为0.2μg/L,富集因子为100,富集效率为98.06~101.26%,时间为15min左右。该方法简单快速,灵敏度高,重复性好,可以和便携式仪器连用,适用于在线检测、尤其是偏远地区的实际样品测定。
A quaternary ammonium ion-exchange fiber PP-g-DMAEMA-Br was prepared by two-step grafting method, which was used as adsorbent in solid-phase microextraction of fiber tube and was enriched by UV-visible spectrophotometry A trace of Cr (Ⅵ) in aqueous solution was detected and a new preconcentration process for the determination of trace Cr (Ⅵ) in water was developed. The effects of sample flow rate and p H value on the trace Cr (Ⅵ) adsorption on the fiber column and the influence of the type, concentration, volume and eluent flow rate of the sample on the elution recovery of Cr (Ⅵ) were studied. Under the optimum conditions, the detection limit of Cr (Ⅵ) was 0.2 μg / L for Cr (Ⅵ), the enrichment factor was 100, the enrichment efficiency was 98.06 ~ 101.26% and the time was about 15 min. The method is simple, fast, sensitive and reproducible. It can be used with portable instruments and is suitable for on-line testing, especially in remote areas.