分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
5期
729-734
,共6页
赵红帅%刘保献%常淼%沈秀娥%王小菊%徐稣士%赵起越
趙紅帥%劉保獻%常淼%瀋秀娥%王小菊%徐穌士%趙起越
조홍수%류보헌%상묘%침수아%왕소국%서소사%조기월
细颗粒物%PM2. 5%多环芳烃%气相色谱-三重四级杆质谱%控温超声
細顆粒物%PM2. 5%多環芳烴%氣相色譜-三重四級桿質譜%控溫超聲
세과립물%PM2. 5%다배방경%기상색보-삼중사급간질보%공온초성
Fine particulate matter%Polycyclic aromatic hydrocarbons%Gas chromatography tandem mass spectrometry%Temperature controlled ultrasonic extraction
建立了控温超声提取-气相色谱三重四级杆质谱测定大气细颗粒物( PM2.5)中多环芳烃( Polycyclic aromatic hydrocarbon,PAHs)的分析方法。 PM2.5中的PAHs用二氯甲烷-正己烷(2:1, V/V)控温超声提取3次,每次提取20 min,气相色谱-串联质谱分析,得到16种PAHs和6种替代物的标准曲线线性关系良好,相关系数均大于0.99,16种PAHs的检出限范围为0.013~0.12μg/L。实验中还观察到PAHs在空白滤膜中有微量存在,回收率实验中得到6种替代物的回收率在58.7%~108.2%之间,16种PAHs的空白滤膜加标的平均回收率在88.3%~104.0%之间,相对标准偏差均低于9.0%,实际滤膜加标的平均回收率在77.3%~98.7%之间,相对标准偏差均低于6.0%,本方法能够满足实际大气样品的测定。
建立瞭控溫超聲提取-氣相色譜三重四級桿質譜測定大氣細顆粒物( PM2.5)中多環芳烴( Polycyclic aromatic hydrocarbon,PAHs)的分析方法。 PM2.5中的PAHs用二氯甲烷-正己烷(2:1, V/V)控溫超聲提取3次,每次提取20 min,氣相色譜-串聯質譜分析,得到16種PAHs和6種替代物的標準麯線線性關繫良好,相關繫數均大于0.99,16種PAHs的檢齣限範圍為0.013~0.12μg/L。實驗中還觀察到PAHs在空白濾膜中有微量存在,迴收率實驗中得到6種替代物的迴收率在58.7%~108.2%之間,16種PAHs的空白濾膜加標的平均迴收率在88.3%~104.0%之間,相對標準偏差均低于9.0%,實際濾膜加標的平均迴收率在77.3%~98.7%之間,相對標準偏差均低于6.0%,本方法能夠滿足實際大氣樣品的測定。
건립료공온초성제취-기상색보삼중사급간질보측정대기세과립물( PM2.5)중다배방경( Polycyclic aromatic hydrocarbon,PAHs)적분석방법。 PM2.5중적PAHs용이록갑완-정기완(2:1, V/V)공온초성제취3차,매차제취20 min,기상색보-천련질보분석,득도16충PAHs화6충체대물적표준곡선선성관계량호,상관계수균대우0.99,16충PAHs적검출한범위위0.013~0.12μg/L。실험중환관찰도PAHs재공백려막중유미량존재,회수솔실험중득도6충체대물적회수솔재58.7%~108.2%지간,16충PAHs적공백려막가표적평균회수솔재88.3%~104.0%지간,상대표준편차균저우9.0%,실제려막가표적평균회수솔재77.3%~98.7%지간,상대표준편차균저우6.0%,본방법능구만족실제대기양품적측정。
An analytical method was described for the determination of polycyclic aromatic hydrocarbons ( PAHs) in atmospheric fine particulate matter ( PM2. 5 ) by gas chromatography-triple quadrupole mass spectrometry with controlled temperature ultrasonic extraction. The PAHs in PM2. 5 were extracted 3 times and each was 20 min with a mixed solution of dichloromethane and n-hexane ( 2: 1 , V/V ) by controlling temperature, and analyzed by gas chromatography-triple quadrupole mass spectrometry. The results showed that 16 PAHs and 6 substitutes had good liner relationship, and the correlation coefficients were above 0. 99, the lowest detection limits for 16 PAHs were between 0. 013-0. 12 μg/L. PAHs were also detected in blank membrane, and the precision test shows that 6 substitutes recoveries range from 58. 7% to 108. 2%, the average recoveries in blank membrane of 16 PAHs were between 88 . 3%-104 . 0%, the relative standard deviationa of all PAHs are below 9 . 0% but actual membrane average recoveries are between 77 . 3%-98 . 7%, and the relative standard deviationa of all PAHs were below 6 . 0%. This method can meet the detection requirements for atmospheric samples.