气阻稳流-阀切换除氧技术结合气相色谱法快速测定环境空气中的SF_6
|
摘要
建立了气相色谱-微池电子俘获检测器(GC-μECD)快速定量分析SF_6的方法。采用十通阀进样,以相同规格的5?分子筛柱作为分离柱和分析柱,通过气阻稳流、分离柱与分析柱前端压力的匹配解决了色谱分析基线的波动;通过阀切换除氧技术提高了SF_6气相色谱分析速率。结果表明,在优化的试验条件下,单个气体样品的分析时间为1.0 min,SF_6的体积比在1.51×10~(-12)～4.97×10~(-8)L·L~(-1)内与其峰高呈线性关系,检出限(3S/N)为1.30×10~(-12) L·L~(-1),测定下限(10S/N)为4.80×10~(-12)L·L~(-1)。采用所建立的方法连续10次分析环境空气样品,SF_6测定结果的相对标准偏差为0.61%。
A method was established to rapid quantitatively analyze SF_6 by gas chromatography(GC) with micro-cell electron capture detector.A gas sample was inducted to GC by a ten-port valve.Two 5? molecular sieve columns with same specification were used for separating and analyzing respectively.Chromatographic baseline fluctuation was eliminated by stabilizing airstream with air resistance and matching the front air pressure of separating column and analytical column.Gas chromatographic analysis rate of SF_6 was improved by removing oxygen through valve switching.The results showed that,under the optimzed experimental conditions,the analysis time of a single gas sample was 1.0 min,and linear relationship was found between peak height and volume ratio of SF_6 within 1.51×10~(-12)-4.97×10~(-8) L·L~(-1),with detection limit(3 S/N)) of 1.30×10~(-12) L·L~(-1),and the lower limit of determination(10 S/N) of 4.80×10~(-12) L·L~(-1).The enviornmental air samples were analyzed 10 times by the proposed method,and the relative standard deviation of the determination results of SF_6 was 0.61%.
A method was established to rapid quantitatively analyze SF_6 by gas chromatography(GC) with micro-cell electron capture detector.A gas sample was inducted to GC by a ten-port valve.Two 5? molecular sieve columns with same specification were used for separating and analyzing respectively.Chromatographic baseline fluctuation was eliminated by stabilizing airstream with air resistance and matching the front air pressure of separating column and analytical column.Gas chromatographic analysis rate of SF_6 was improved by removing oxygen through valve switching.The results showed that,under the optimzed experimental conditions,the analysis time of a single gas sample was 1.0 min,and linear relationship was found between peak height and volume ratio of SF_6 within 1.51×10~(-12)-4.97×10~(-8) L·L~(-1),with detection limit(3 S/N)) of 1.30×10~(-12) L·L~(-1),and the lower limit of determination(10 S/N) of 4.80×10~(-12) L·L~(-1).The enviornmental air samples were analyzed 10 times by the proposed method,and the relative standard deviation of the determination results of SF_6 was 0.61%.
引文
[1] DIETZ R N,DABBERDT W F.Gaseous-tracer technology and applications:American Meteorological Society short course on instruments and techniques for probing the atmospheric boundary layer:BNL-33585.[Sl..:s.n.],1983.
[2] 张俊刚.大气中SF6的分析方法及其实际应用研究[D].武汉:中国地质大学,2006.
[3] 张永义,闫江雨,卫为强.复杂地形条件下大气扩散六氟化硫示踪试验研究[J].辐射防护通讯,2000,20(3):7-14.
[4] 任克斌.SF6-CF2ClBr双示踪技术在测定复杂采空区漏风中的应用[J].煤矿设计,2001(6):37-38.
[5] 邵辉,代广龙,张国枢,等.SF6-CF2ClBr双元示踪气体检测复杂采空区漏风技术[J].煤炭科学技术,1998,26(4):1-4.
[6] 秦波涛,李增华.利用SF6气体测定矿井漏风技术[J].河北煤炭,2002(1):1-2.
[7] 朱能,田哲,王侃红,等.示踪气体跟踪测量方法在空调通风上的应用[J].技术讲座,1999,29(2):58-62.
[8] 孙雷.SF6气体泄漏监测系统设计[J].电力信息与通讯技术,2015,13(6):106-109.
[9] 羊衍秋,杨通在,郝樊华,等.SF6示踪检测大型容器的动态泄漏[J].核技术,2010,33(4):312-315.
[10] 田杰,羊衍秋,杨亮,等.SF6示踪气体远程泄漏监测系统设计及性能[J].原子能科学技术,2014,48(9):1686-1692.
[11] 雷言,翟远征,王金生,等.年轻地下水定年研究综述[J].地球与环境,2015,43(2):233-242.
[12] MAISS M,BRENNIKMEIJER C A M.Atmospheric SF6:Trends,sources,and propects[J].Environmental Science &Technology,1998,32(20):3077-3086.
[13] 张伟,孙元平,刘彬,等.SiC材料的NLD快速均匀刻蚀[J].微纳电子技术,2015,52(1):54-58.
[14] NAIDU M S.High voltage engineering.[S.l.]:McGraw Hill Professional Publishing,1995.
[15] 李春瑛,杜秋芳.六氟化硫标准气体GC-ECD分析方法的研究[J].分析与测试,2004,22(2):32-36.
[16] 羊衍秋,何玉晖,田杰,等.阀切换技术在大气样品中六氟化硫快速分析中的应用[J].色谱,2007,25(4):609-610.
[17] 薛华,曾帆,杨立涛,等.六氟化硫(SF6)气体的快速定量分析方法[J].低温与特气,2014,32(5):29-31.
[2] 张俊刚.大气中SF6的分析方法及其实际应用研究[D].武汉:中国地质大学,2006.
[3] 张永义,闫江雨,卫为强.复杂地形条件下大气扩散六氟化硫示踪试验研究[J].辐射防护通讯,2000,20(3):7-14.
[4] 任克斌.SF6-CF2ClBr双示踪技术在测定复杂采空区漏风中的应用[J].煤矿设计,2001(6):37-38.
[5] 邵辉,代广龙,张国枢,等.SF6-CF2ClBr双元示踪气体检测复杂采空区漏风技术[J].煤炭科学技术,1998,26(4):1-4.
[6] 秦波涛,李增华.利用SF6气体测定矿井漏风技术[J].河北煤炭,2002(1):1-2.
[7] 朱能,田哲,王侃红,等.示踪气体跟踪测量方法在空调通风上的应用[J].技术讲座,1999,29(2):58-62.
[8] 孙雷.SF6气体泄漏监测系统设计[J].电力信息与通讯技术,2015,13(6):106-109.
[9] 羊衍秋,杨通在,郝樊华,等.SF6示踪检测大型容器的动态泄漏[J].核技术,2010,33(4):312-315.
[10] 田杰,羊衍秋,杨亮,等.SF6示踪气体远程泄漏监测系统设计及性能[J].原子能科学技术,2014,48(9):1686-1692.
[11] 雷言,翟远征,王金生,等.年轻地下水定年研究综述[J].地球与环境,2015,43(2):233-242.
[12] MAISS M,BRENNIKMEIJER C A M.Atmospheric SF6:Trends,sources,and propects[J].Environmental Science &Technology,1998,32(20):3077-3086.
[13] 张伟,孙元平,刘彬,等.SiC材料的NLD快速均匀刻蚀[J].微纳电子技术,2015,52(1):54-58.
[14] NAIDU M S.High voltage engineering.[S.l.]:McGraw Hill Professional Publishing,1995.
[15] 李春瑛,杜秋芳.六氟化硫标准气体GC-ECD分析方法的研究[J].分析与测试,2004,22(2):32-36.
[16] 羊衍秋,何玉晖,田杰,等.阀切换技术在大气样品中六氟化硫快速分析中的应用[J].色谱,2007,25(4):609-610.
[17] 薛华,曾帆,杨立涛,等.六氟化硫(SF6)气体的快速定量分析方法[J].低温与特气,2014,32(5):29-31.