环境监控与预警
環境鑑控與預警
배경감공여예경
Environmental Monitoring and Forewarning
2015年
5期
20-24
,共5页
许家慧%普学伟%施艳峰%觉玉峰
許傢慧%普學偉%施豔峰%覺玉峰
허가혜%보학위%시염봉%각옥봉
吹扫捕集%气相色谱/质谱法%乙醛%丙烯醛%丙烯腈%吡啶
吹掃捕集%氣相色譜/質譜法%乙醛%丙烯醛%丙烯腈%吡啶
취소포집%기상색보/질보법%을철%병희철%병희정%필정
Purge-and-trap%Gas chromatography-mass spectrometry%Acetaldehyde%Acrolein%Acrylonitrile%Pyridine
水中的乙醛、丙烯醛、丙烯腈和吡啶经吹扫捕集、解吸后，用HP－VOC毛细管色谱柱进行GC分离，用GC－MS法选择离子模式（ SIM）下进行检测，外标法定量。结果表明，选择取样量25 mL，吹扫流量为40 mL／min，吹扫温度为40℃，吹扫时间为15 min，解吸时间为2 min，解吸温度为200℃，烘焙时间20 min，乙醛和吡啶质量浓度在0．025～0．60 mg／L之间，丙烯醛和丙烯腈质量浓度在0．0025～0．10 mg／L之间时，校准曲线呈线性关系，相关系数r＞0．995，乙醛、丙烯醛、丙烯腈和吡啶的方法检出限分别为0．0016，0．0013，0．0005和0．0021 mg／L。对3个不同浓度样品进行空白加标实验，测量的回收率为87．8％～114．3％，相对标准偏差（n＝6）为2．51％～10．4％。对3批实际水样进行分析，其中一个废水水样加标回收率为79．2％～103．8％，相对标准偏差（n＝6）为3．04％～6．39％。
水中的乙醛、丙烯醛、丙烯腈和吡啶經吹掃捕集、解吸後，用HP－VOC毛細管色譜柱進行GC分離，用GC－MS法選擇離子模式（ SIM）下進行檢測，外標法定量。結果錶明，選擇取樣量25 mL，吹掃流量為40 mL／min，吹掃溫度為40℃，吹掃時間為15 min，解吸時間為2 min，解吸溫度為200℃，烘焙時間20 min，乙醛和吡啶質量濃度在0．025～0．60 mg／L之間，丙烯醛和丙烯腈質量濃度在0．0025～0．10 mg／L之間時，校準麯線呈線性關繫，相關繫數r＞0．995，乙醛、丙烯醛、丙烯腈和吡啶的方法檢齣限分彆為0．0016，0．0013，0．0005和0．0021 mg／L。對3箇不同濃度樣品進行空白加標實驗，測量的迴收率為87．8％～114．3％，相對標準偏差（n＝6）為2．51％～10．4％。對3批實際水樣進行分析，其中一箇廢水水樣加標迴收率為79．2％～103．8％，相對標準偏差（n＝6）為3．04％～6．39％。
수중적을철、병희철、병희정화필정경취소포집、해흡후，용HP－VOC모세관색보주진행GC분리，용GC－MS법선택리자모식（ SIM）하진행검측，외표법정량。결과표명，선택취양량25 mL，취소류량위40 mL／min，취소온도위40℃，취소시간위15 min，해흡시간위2 min，해흡온도위200℃，홍배시간20 min，을철화필정질량농도재0．025～0．60 mg／L지간，병희철화병희정질량농도재0．0025～0．10 mg／L지간시，교준곡선정선성관계，상관계수r＞0．995，을철、병희철、병희정화필정적방법검출한분별위0．0016，0．0013，0．0005화0．0021 mg／L。대3개불동농도양품진행공백가표실험，측량적회수솔위87．8％～114．3％，상대표준편차（n＝6）위2．51％～10．4％。대3비실제수양진행분석，기중일개폐수수양가표회수솔위79．2％～103．8％，상대표준편차（n＝6）위3．04％～6．39％。
A method for simultaneous determination of acetaldehyde,acrolein,acrylonitrile and pyridine in water by purge-and-trap-gas chromatography-mass spectrometry ( GC-MS) was reported.These compounds were concentrated by purging and trapping fol-lowed by desorption before GC-MS measurement using the HP-VOC capillary column for separation and selective ion mode ( SIM) for MS detection.External calibration was used for quantification.The following experimental conditions were used:the sampling vol-ume was 25 mL,purging gas flow was 40 mL/min,purging temperature was 40 ℃,purging time was 15 min,desorption time was 2 min,desorption temperature was 200℃,and baking time was 20 min.Under this condition,it was determined that the concentrations of acetaldehyde and pyridine were between 0.025 and 0.60 mg/L,and acrolein and acrylonitrile were between 0.002 5 and 0.10 mg/L.The calibration curve showed good linearity with the correlation coefficient r>0.995.The method detection limits of acetalde-hyde,acrolein,acrylonitrile and pyridine were 0.001 6,0.001 3,0.000 5 and 0.002 1 mg/L,respectively.The recovery rates ranged between 87.8%and 114.3%in three different spiked levels.The relative standard deviation (n=6) was from 2.51%to 10.4%. Three batches of water samples were analyzed.The recovery rates ranged between 79.2%and 103.8%for the waste water,and rela-tive standard deviation (n=6) was from 3.04%to 6.39%.
