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反相萃取色谱是将溶剂萃取与层析结合起来的一种有效分离技术,在无机色谱中已广泛应用,但阴离子反相萃取色谱的研究较少。卤素离子反相萃取色谱的研究虽有报导,但系经典方法,峰十分扩张,需时也较长。本文以高分子胺N263-多孔硅胶为固定相,以硝酸钠为流动相,在国产高效离子交换色谱仪上研究了分离测定卤素离子的条件。表明,在选定条件下,7分钟内可定量分离Cl~-和I~-或Br~-和I~-;因用中性盐洗脱体系,高分子胺的流失甚少,能在较长时间内连续使用数百次,柱效仍不下降。方法具有简便、快速、成本低等优点,应用于自来水、土壤和海带中卤素离子的测定,获良好结果。一、仪器与试剂
RP-HPLC is an effective separation technology combining solvent extraction and chromatography. It has been widely used in inorganic chromatography, but there are few studies on reversed-phase anion-exchange chromatography. Halogen ion reversed-phase extraction of chromatographic studies have been reported, but the classic method, the peak is very expanded, take a longer time. In this paper, macromolecule amine N263-porous silica gel as stationary phase, with sodium nitrate as mobile phase, the conditions of separation and determination of halide ions were studied on domestic high performance ion exchange chromatography. It shows that under the selected conditions, Cl ~ - and I ~ - or Br ~ - and I ~ ~ can be quantitatively separated within 7 minutes. Due to the neutral salt elution system, the loss of the polymer amines is very little, Continuous use for hundreds of times over a long period of time, efficiency is still not declining. The method has the advantages of simplicity, rapidness and low cost, and has been applied to the determination of halogen ions in tap water, soil and seaweed with good results. First, equipment and reagents