CAJ | 학술논문

建立了离子交换色谱-直接电导检测法分离测定3种同系物季铵盐离子液体阳离子（四甲基铵、四乙基铵和四丙基铵阳离子）的方法。采用磺酸型阳离子交换色谱柱，以乙二胺-柠檬酸-乙腈为淋洗液，考察了淋洗液种类、浓度及色谱柱温度对3种阳离子保留的影响。并根据测定对象不同，调整乙二胺浓度及乙腈含量以改善分离效果。淋洗液中增加乙腈含量，可明显缩短四丙基铵阳离子的保留时间，并改善其色谱峰形。季铵阳离子同系物的保留符合碳数规律。优化的色谱条件为：流速1.0 mL/min，色谱柱温度40℃；以0.02 mmol/L乙二胺-0.12 mmol/L 柠檬酸（ pH 4.0）为淋洗液分离测定四甲基铵；以0.2 mmol/L乙二胺-0.4 mmol/L 柠檬酸-1％乙腈（ pH 4.0）为淋洗液分离测定四乙基铵和四丙基铵。所测阳离子的检出限（ S/N=3）分别为0.015，0.22，1.88 mg/L，相对标准偏差（n=5）均小于2.3％。将方法应用于表面活性剂和实验室合成的离子液体的分析，加标回收率为99％~104％。本方法简单、准确、可靠，具有良好的实用性。
건립료리자교환색보-직접전도검측법분리측정3충동계물계안염리자액체양리자（사갑기안、사을기안화사병기안양리자）적방법。채용광산형양리자교환색보주，이을이알-저몽산-을정위림세액，고찰료림세액충류、농도급색보주온도대3충양리자보류적영향。병근거측정대상불동，조정을이알농도급을정함량이개선분리효과。림세액중증가을정함량，가명현축단사병기안양리자적보류시간，병개선기색보봉형。계안양리자동계물적보류부합탄수규률。우화적색보조건위：류속1.0 mL/min，색보주온도40℃；이0.02 mmol/L을이알-0.12 mmol/L 저몽산（ pH 4.0）위림세액분리측정사갑기안；이0.2 mmol/L을이알-0.4 mmol/L 저몽산-1％을정（ pH 4.0）위림세액분리측정사을기안화사병기안。소측양리자적검출한（ S/N=3）분별위0.015，0.22，1.88 mg/L，상대표준편차（n=5）균소우2.3％。장방법응용우표면활성제화실험실합성적리자액체적분석，가표회수솔위99％~104％。본방법간단、준학、가고，구유량호적실용성。
A method of ion-exchange chromatography with direct conductivity detection to determine three homologous quaternary ammonium cations( tetramethyl-ammonium cation,tetraethyl-ammonium cation and tetrapropyl-ammonium cation ) was developed. Three homologous quaternary ammonium cations were separated on a sulfonic acid base cation-exchange column using ethylenediamine-citric acid-acetonitrile as eluent. Effects of eluent types,eluent concentrations and column temperatures on retention and separation of three cations were discussed. The separations of the cations were im-proved by changing concentration of ethylenediamine and acetonitrile in eluents. With the increase of acetonitrile concentration,the retention time of tetrapropyl-ammonium cation was obviously reduced, and the chromatogrophic peaks of the cations were improved. The retentions of homologous quaternary ammonium cations accord with carbon number rule. The suitable eluents for analysis of tetramethyl-ammonium cation and tetraethyl-ammonium,tetrapropyl-ammonium cations were 0. 02 mmol/L ethyl-enediamine-0. 12 mmol/L citric acid( pH 4. 0 )and 0. 2 mmol/L ethylenediamine-0. 4 mmol/L cit-ric acid-1% acetonitrile(pH 4. 0),respectively. The flow rate and column temperature were 1. 0 mL/min and 40 ℃,respectively. The detection limits(S/N =3)for three cations were 0. 015, 0. 22,1. 88 mg/L,respectively. Relative standard deviations(n=5)for peak areas were less than 2. 3% . The method was successfully applied in the determination of quaternary ammonium ionic liq-uids synthesized in chemical laboratory and surfacetant tetramethyl-ammonium hydroxide,with recov-eries of 99% -104% . The method is simple,accurate,reliable and practical.