摘要
目的:探讨有机改进剂对S2O23-、SCN-、C lO-4的保留时间的影响,并建立同时测定水中7种标准阴离子和S2O23-、SCN-、C lO-4的离子色谱分析方法。方法:采用丙酮和乙腈作有机改进剂,采用M etrosep A Supp 5-100阴离子交换柱,以3.2 mmol/L Na2CO3+1.0 mmol/L NaHCO3为淋洗液,比较加入不同浓度有机改进剂后S2O23-、SCN-、C lO-4的保留时间、C lO4-的峰形和柱压,化学抑制电导检测离子色谱法。结果:随着丙酮浓度的增加,C lO4-的保留时间则由36 m in(0%丙酮)缩短为21 m in(25%丙酮),C lO-4峰形有改善,但柱压也明显增加。采用20%乙腈代替丙酮,保留时间只有轻微改变,但柱压和C lO-4峰形有明显的改善。各阴离子的线性好(r>0.9990),相对标准偏差均小于3.7%(n=6),平均加标回收率均在89.4%~105.3%之间,检出限在2.92~32.1μg/L之间。结论:有机改进剂可缩短分离时间、改善峰形。在本文所作的试验中,加入20%乙腈作为有机改进剂所得分离效果最好。
Objective：To study the influence of organic modifiers on the retention time of thiocyanate, thiosulfate and perchlorate and establish a ion -chromatography method to measure seven standard anions together with thiosulfate,thiocyanate and perchlorate in water. Methods： The influence of different eluents on the retention time of thiocyanate, thiosulfate and perchlorate, the symmetry of perchlorate and the column pressure were evaluated on the metrosep supp 5 - 100, using a 3. 2 mmol/L Na2 CO3/1.0 mmol/L NaHCO3 eluent, chemical suppression and conductivity detection. Acetone, acetonitrile were added to the eluent. Results：A greater proportion of acetone in the eluent had shorter retention time for perchlorate as consequence. The analysis time decreased from 36 rain （0% acetone） to 21 rain （25% acetone）. The symmetry of perchlorate was improved with more acetone in the eluent, but the back pressure of the column increased. Using 20% of acetonitrile instead of acetone resulted in slightly increased retention time. But the symmetry for perchlotate improved and the pressure decreased. In this method, there was good relativity （ r 〉 0. 9990）, the RSD% of ten anions was 〈 3.7 % （ n = 6 ）, and the recovery rate was 89. 4% - 105. 3 %. The method detection limit was 2.92 - 32. 1 μg/L Conclusion：The analysis time can be achieved with organic modifiers in the eluent. To become a nicer peak shape and a better and smaller retention of perchlotate, organic modifiers is added to the eluent. Within the tested eluent compositions,the best results axe obtained with 20% of acetonitrile in the standard eluent.
出处
《中国卫生检验杂志》
CAS
2006年第4期413-415,共3页
Chinese Journal of Health Laboratory Technology
