CAJ | 학술논문

建立了液液萃取-气相色谱/质谱同时测定水中3种典型季胺盐化合物十二烷基三甲基氯化铵(DTAC)、十六烷基三甲基溴化铵(CTAB)、双十二烷基二甲基氯化铵(DDAC)的分析方法。采用电子轰击(EI)-选择离子模式(SIM)进行定性与定量分析,DTAC和CTAB的特征离子为m/z 58,DDAC的特征离子为m/z 212。考察了萃取剂种类、萃取次数、pH值以及盐度对萃取效率的影响。以HCl及30%NaCl溶液调节水样pH值为1.5及盐度为3%,以5 mL三氯甲烷萃取2次,3种目标化合物的线性范围在0.01~2.0 mg/L之间,检出限LOD(S/N=3)为2.5~8.5μg/L。以此方法测定自来水、湖水、河水、选矿废水样品,3种目标化合物的含量在0.06~2.45 mg/L之间,不同加标水平(0.2,0.5和1.0 mg/L)回收率在65%~113%之间,相对标准偏差在3.8%~23.0%之间。
건립료액액췌취-기상색보/질보동시측정수중3충전형계알염화합물십이완기삼갑기록화안(DTAC)、십륙완기삼갑기추화안(CTAB)、쌍십이완기이갑기록화안(DDAC)적분석방법。채용전자굉격(EI)-선택리자모식(SIM)진행정성여정량분석,DTAC화CTAB적특정리자위m/z 58,DDAC적특정리자위m/z 212。고찰료췌취제충류、췌취차수、pH치이급염도대췌취효솔적영향。이HCl급30%NaCl용액조절수양pH치위1.5급염도위3%,이5 mL삼록갑완췌취2차,3충목표화합물적선성범위재0.01~2.0 mg/L지간,검출한LOD(S/N=3)위2.5~8.5μg/L。이차방법측정자래수、호수、하수、선광폐수양품,3충목표화합물적함량재0.06~2.45 mg/L지간,불동가표수평(0.2,0.5화1.0 mg/L)회수솔재65%~113%지간,상대표준편차재3.8%~23.0%지간。
An analytical method was developed for the simultaneous extraction and determination of three quatermary ammonium compouds ( QACs ) in water samples using liquid-liquid extraction and gas chromatography mass spectrometry. The qualitative and quantitative analysis of the three analytes ( dodecyltrimethylammonium chloride ( DTAC) , CTAB and didodecyl-dimethyl-ammonium chloride ( DDAC) was conducted by application of EI Mass spectra and selected ion monioring ( SIM) . Characteristic ion of the first two (DTAC, CTAB) and the latter was m/z 58, and the characteristic ion of DDAC was m/z 212. To achieve optimum extraction efficiency, several impact factors including different types of extractants, extraction times, pH value and salinity in water sample matrixs were investigated. In the optimized extraction conditions, pH and salinity of water sample was adjusted to 1 . 5 and 3% respectively using hydrochloric acid and sodium chloride , then the processed water sample was extracted by chloroform twice with 5 mL every time in a 125 mL separatory funnel. Good linear relationships of all the three analytes were obtained in the range of 0. 01-2. 0 mg/L. The limits of determination ( LOD, S/N=3 ) was 2. 5-8. 5 μg/L. The method was used to analyse real water samples collected from running water, lake water, river water and beneficiation water. Results of determination displayed the concerntrations of the three analytes in real water samples ranged from 0. 06 mg/L to 2. 45 mg/L, and their recoveries ranged from 65% to 113% with relative standard deviations (RSD) 3. 8%-23% in three different spiked concentrations (0. 2, 0. 5 and 1. 0 mg/L).