气相色谱法测定煤层瓦斯中低浓度氢气和氦气
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摘要
利用HP 5890气相色谱仪热导检测器小热导池高灵敏度及大进样量的特点,建立了煤层中低浓度He、H2的气相色谱测定方法,并可同时测定常量CH4。对气相色谱工作条件进行了优化,确定的最佳工作条件是:13X分子筛填充柱,热导检测器(TCD),载气流速为35~42mL/m in,色谱柱温度50℃,汽化室温度50℃,检测室温度100℃,3 mL定量环。He、H2的线性工作范围分别为0.95~19μL/L和2.4~48μL/L,RSD(n=8)分别为1.60%和4.54%,方法的检出限为0.5μL/L。实验了铝箔气袋、橡胶气球和盐水瓶不同包装的样品进样方式及测定情况,结果表明铝箔气袋是最佳选择,盐水瓶次之,橡胶气球对气体有一定的吸附作用。
This paper describes a method for determination of the H_2 and He at low concentration from coal mining underground by gas chromatography.The method is also available for the determination of CH_4 from coal.The working conditions of gas chromatography were optimized.A 13X molecule sieve packed column and thermal conductivity detector(TCD) were used with optimized working conditions of carrier gas flow rate at 35~42 mL/min,column temperature at 50 ℃,injector temperature at 50 ℃ and detector temperature at 100 ℃.The linear ranges for He and H_2 are 0.95~19 μL/L and 2.4~48 μL/L with precision of 1.60% RSD and 4.54% RSD(n=8),respectively.The detection limits for He and H_2 are 0.5 μL/L.Three kinds of packing materials including Al-foil bags,rubber balls and salt water-filling glass bottles were tested.The results show that Al-foil bag is the best one,the salt water-filling glass bottle is next and the rubber ball is not sultable for sampling due to its gas-adsorption property especially for the gases of He and H_2.
This paper describes a method for determination of the H_2 and He at low concentration from coal mining underground by gas chromatography.The method is also available for the determination of CH_4 from coal.The working conditions of gas chromatography were optimized.A 13X molecule sieve packed column and thermal conductivity detector(TCD) were used with optimized working conditions of carrier gas flow rate at 35~42 mL/min,column temperature at 50 ℃,injector temperature at 50 ℃ and detector temperature at 100 ℃.The linear ranges for He and H_2 are 0.95~19 μL/L and 2.4~48 μL/L with precision of 1.60% RSD and 4.54% RSD(n=8),respectively.The detection limits for He and H_2 are 0.5 μL/L.Three kinds of packing materials including Al-foil bags,rubber balls and salt water-filling glass bottles were tested.The results show that Al-foil bag is the best one,the salt water-filling glass bottle is next and the rubber ball is not sultable for sampling due to its gas-adsorption property especially for the gases of He and H_2.
引文
[1]L iang H D.A Probe of the M echan ism of the Outburstof Coal and Gas on Hydrogen Geochem istry[A].Pro-ceed ings 14thAnnual International P ittsburgh Coal Con-ference and W orkshop[C].1997,Session P1,6:5.
[2]梁汉东.井下煤岩钻屑释放氢气与瓦斯突出关系初探[J].煤炭学报,2001,26(6):637—642.
[3]梁汉东.山西5起小煤矿瓦斯爆炸与青海8.1级地震有关吗?[J].科学技术与工程,2003,3(2):197—200.
[4]梁汉东,杜乐天.煤层瓦斯来源系统观[J].中国地球物理年刊,2005,待刊.
[5]梁汉东.影响煤炭安全性的新因素———分子氢自原煤中发射的现象[J].矿业安全与环保,2001,28(2):1—3.
[6]G rossm an S L,David S,Cohen H.Exp losion R isk dur-ing the Confined Storage of B itum inous Coal[J].Fuel,1995,74:1772—1775.
[7]梁汉东.煤与瓦斯突出的化学本质:从原理和证据到现场预报途径[A].见:彭苏萍,程桦.煤矿安全高效开采地质保障体系[M].北京:煤炭工业出版社,2001.147—157.
[8]梁汉东.井下煤岩钻削气体中分子氢的发现与意义[J].中国学术期刊文摘(科技快报),2000,6(10):1293—1295.
[9]梁汉东.突出煤与未突出煤自然状态下分子氢释放的差异[J].中国学术期刊文摘(科技快报),2000,6(10):1295—1297.
[10]徐胜平,江洪清,梁汉东.煤岩中氢气氦气甲烷释放规律的研究[J].矿业安全与环保,2003,30(6):4—6.
[11]朱铭,周瑞光,尹代勋,等.煤层应力变化与He,Ar发射关系[J].中国科学(D),2002,32(6):479—490.
[12]杜乐天.地球排气作用的重要意义及研究进展[J].地质论评,2005,51(2):174—180.
[13]车用太,鱼金子,张培仁,等.H2与He的映震灵敏性及其干扰初析[J].地震,2002,22(2):94—103.
[14]MT/T 77—94,煤层气测定方法[S].
[2]梁汉东.井下煤岩钻屑释放氢气与瓦斯突出关系初探[J].煤炭学报,2001,26(6):637—642.
[3]梁汉东.山西5起小煤矿瓦斯爆炸与青海8.1级地震有关吗?[J].科学技术与工程,2003,3(2):197—200.
[4]梁汉东,杜乐天.煤层瓦斯来源系统观[J].中国地球物理年刊,2005,待刊.
[5]梁汉东.影响煤炭安全性的新因素———分子氢自原煤中发射的现象[J].矿业安全与环保,2001,28(2):1—3.
[6]G rossm an S L,David S,Cohen H.Exp losion R isk dur-ing the Confined Storage of B itum inous Coal[J].Fuel,1995,74:1772—1775.
[7]梁汉东.煤与瓦斯突出的化学本质:从原理和证据到现场预报途径[A].见:彭苏萍,程桦.煤矿安全高效开采地质保障体系[M].北京:煤炭工业出版社,2001.147—157.
[8]梁汉东.井下煤岩钻削气体中分子氢的发现与意义[J].中国学术期刊文摘(科技快报),2000,6(10):1293—1295.
[9]梁汉东.突出煤与未突出煤自然状态下分子氢释放的差异[J].中国学术期刊文摘(科技快报),2000,6(10):1295—1297.
[10]徐胜平,江洪清,梁汉东.煤岩中氢气氦气甲烷释放规律的研究[J].矿业安全与环保,2003,30(6):4—6.
[11]朱铭,周瑞光,尹代勋,等.煤层应力变化与He,Ar发射关系[J].中国科学(D),2002,32(6):479—490.
[12]杜乐天.地球排气作用的重要意义及研究进展[J].地质论评,2005,51(2):174—180.
[13]车用太,鱼金子,张培仁,等.H2与He的映震灵敏性及其干扰初析[J].地震,2002,22(2):94—103.
[14]MT/T 77—94,煤层气测定方法[S].
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