岩矿测试
巖礦測試
암광측시
ROCK AND MINERAL ANALYSIS
2015年
4期
480-486
,共7页
高松%邓银舟%李玉芹%刘园园%张兰英%刘娜%庞英明
高鬆%鄧銀舟%李玉芹%劉園園%張蘭英%劉娜%龐英明
고송%산은주%리옥근%류완완%장란영%류나%방영명
地下水%有机磷农药%针捕集%吹扫提取%气相色谱法
地下水%有機燐農藥%針捕集%吹掃提取%氣相色譜法
지하수%유궤린농약%침포집%취소제취%기상색보법
groundwater%organophosphorus pesticides%needle trap%extraction by purge%Gas Chromatography
基于针捕集适于免溶剂提取气态介质样品的特点,通过蠕动泵将针捕集与水样组成闭合循环吹扫系统,提高目标物的水样/顶空亨利系数,建立了针捕集闭合循环提取耦合气相色谱快速分析地下水中4种半挥发性有机磷农药(敌敌畏、甲拌磷、甲基对硫磷、马拉硫磷)的方法,该方法集采样、提取、净化、浓缩、色谱进样于一体。确定了针捕集提取水样最佳条件为:采样流速11.11 mL/min,水样提取温度40℃,在此条件下获得浓度均为1 mg/L的4种有机磷农药的针捕集吸附穿透体积,其中甲基对硫磷最大为600 mL。以5μg/L、50μg/L和200μg/L三个浓度水平的加标平均回收率为62.3%~103.0%,除敌敌畏低浓度水平的RSD为26.1%外,其余组分的RSD﹤7.7%;方法检出限为0.016~0.157μg/L,接近或优于现行国标及相关研究结果。
基于針捕集適于免溶劑提取氣態介質樣品的特點,通過蠕動泵將針捕集與水樣組成閉閤循環吹掃繫統,提高目標物的水樣/頂空亨利繫數,建立瞭針捕集閉閤循環提取耦閤氣相色譜快速分析地下水中4種半揮髮性有機燐農藥(敵敵畏、甲拌燐、甲基對硫燐、馬拉硫燐)的方法,該方法集採樣、提取、淨化、濃縮、色譜進樣于一體。確定瞭針捕集提取水樣最佳條件為:採樣流速11.11 mL/min,水樣提取溫度40℃,在此條件下穫得濃度均為1 mg/L的4種有機燐農藥的針捕集吸附穿透體積,其中甲基對硫燐最大為600 mL。以5μg/L、50μg/L和200μg/L三箇濃度水平的加標平均迴收率為62.3%~103.0%,除敵敵畏低濃度水平的RSD為26.1%外,其餘組分的RSD﹤7.7%;方法檢齣限為0.016~0.157μg/L,接近或優于現行國標及相關研究結果。
기우침포집괄우면용제제취기태개질양품적특점,통과연동빙장침포집여수양조성폐합순배취소계통,제고목표물적수양/정공형리계수,건립료침포집폐합순배제취우합기상색보쾌속분석지하수중4충반휘발성유궤린농약(활활외、갑반린、갑기대류린、마랍류린)적방법,해방법집채양、제취、정화、농축、색보진양우일체。학정료침포집제취수양최가조건위:채양류속11.11 mL/min,수양제취온도40℃,재차조건하획득농도균위1 mg/L적4충유궤린농약적침포집흡부천투체적,기중갑기대류린최대위600 mL。이5μg/L、50μg/L화200μg/L삼개농도수평적가표평균회수솔위62.3%~103.0%,제활활외저농도수평적RSD위26.1%외,기여조분적RSD﹤7.7%;방법검출한위0.016~0.157μg/L,접근혹우우현행국표급상관연구결과。
Based on the merits of solvent-free extraction of gaseous samples by needle trap,closed circulating purge system consisting of needle trap and water sample by peristaltic pump is established to enhance the Henry ’s law constant of analytes in the gas/liquid phase. In this study,the method for determination of dichlorvos,phorate, methyl parathion and malathion in groundwater by circulating extraction with needle trap coupled with Gas Chromatography was established. This method integrated sampling,extraction,purification,concentration,and chromatography. The optimum conditions for the extraction by needle trap include sampling flow rate of 11. 11 mL/min and extraction temperature of 40℃. Under these conditions,the maximum breakthrough volume of 1 mg/L methyl parathion is 600 mL. The recoveries range from 62. 3% to 103. 0% for 5 μg/L,50 μg/L and 200 μg/L analytes. Low level dichlorvos has a relative standard deviation of 26. 1%,and other components are lower than 7. 7%. The detection limits of the proposed method range from 0. 016 to 0. 157 μg/L,close to,or better than the results of current standard method and related study.