CN1094163A - 脉石中的重烃的鉴定方法及其装置 - Google Patents
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Abstract
本发明提供分离和分析含有沉积岩中的重烃的
方法,它包括:
A)将沉积岩样品和一种或多种惰性溶剂置于一
样品管中;
B)预热该样品管;
C)移去溶剂及原先含于岩石中的烃;
D)冷凝蒸汽并将其加入分离、分析装置中。
本发明还提供实施上述方法的装置。
Description
本发明涉及含于脉石中的重烃的鉴定方法。本发明还涉及用于上述方法的装置。
“重烃”意指含有15个或更多个碳原子的烃。
在有机地球化学中,对沉积岩或化石中存在的生物指示层的分析非常重要。分析上述岩石的常用方法是首先用适宜溶剂提取岩石,然后用GC-FID或GC-MS分析提取物。但是该方法花费大,这是由于脉石的提取需要很长时间,同时有时提取物不能直接用于气相色谱分析、需要进行进一步的制备色谱分离。另一方法基于加热脱吸(TD),它首先使含于岩石中的化合物汽化(通过加热至约320℃),然后直接用GC分析。该方法按下列方式操作:
将粉料状沉积岩样品置于一样品管中,样品管一端用惰性材料、优先玻璃棉封上,并将此样品管置于惰性气体物流通过的装置中;
以适当程序将该样品管升温至希望值,通常为约320℃;
该气体物流将从岩石中脱吸的烃输送至一冷阱中,使所述烃冷凝;
终止向样品管中输入气体并将含有冷凝物的冷阱加热;同时通过温度梯度作气相色谱分析;不通过样品管的该惰性气体物流现在通过加热的阱,将该烃转移至色谱柱中,色谱柱配有分流器,能使需要的气体量加入柱中。
该方法的缺点是在脉石中通常仍残留有重烃,使分析结果错误,该结果主要是为了确定脉石中的重烃的种类及含量。
本发明提供一种克服了上述缺点的分析含于沉积岩中的烃的方法,它是对加热脱吸分析方法的改进。
因而,本发明提供含于沉积岩中的烃、特别是重烃的分离和分析方法,其特征在于包括下列步骤:
A)将沉积岩样品和一种或多种惰性溶剂置于一样品管中;
B)在惰性气体中,将此样品管预热至在60-150℃的某-温度,并在此温度下保持一定时间;
C)在一惰性气体物流中,将样品管加热至-温度,以移去溶剂和原先含于岩石中的烃;
D)在一冷却容器中,使惰性气体输送的蒸汽冷凝;
E)加热该容器,并用所述惰性输送气体将容器中的物质加入到分离和分析装置中。
参照附图,下面进一步说明本发明。
图1是用二氯甲烷处理岩石样品30秒(色谱a)、2分钟(色谱b)和3分钟(色谱c)所得的色谱图。横轴为时间(分钟),纵轴为峰强度。色谱图还给出一些峰代表的碳原子数。
图2是用本发明方法处理三种不同的脉石(样品A、B和C)得到的色谱图。
图3是用常用加热脱吸方法处理图2中的样品得到的色谱图。
图4是用于实施本发明方法的装置的示意图。
为了不干扰随后的气相色谱分析,该惰性溶剂优选选自常压下沸点低于约100℃的烃或氯代烃,也可使用这些溶剂的混合物。例如,正戊烷、正己烷、庚烷或二氯甲烷。优选的溶剂用量根据各种指数、特别是待分析的脉石的量而定。一般情况下,1-10mg的脉石优选使用5-50微升溶剂。
样品管由热稳定材料制成,优选无机惰性材料如玻璃或石英。
为使溶剂与脉石接触紧密,脉石优选为粉料,并且在含有惰气的介质中,优选在玻璃棉中。
另外,优选样品放于样品管的一端,样品管的另一端为空的。
在步骤(B)中,为了从岩石中提取所有的烃,温度升至60℃-150℃、优选80℃-110℃。在此步骤中,优选予热只加热样品管放有样品的那一端,这可使释放出来的烃沿整个管重新冷凝。
在上述温度下脉石料与溶剂的接触时间至关重要。其接触时间应足以使含于该脉石样品中几乎所有的烃被提取出来。图1是在约95℃下、用二氯甲烷处理相同的脉石样品30秒、2分钟和3分钟所得的色谱图。处理时间超过3分钟的色谱图基本相同。因此,在上述条件下,溶剂与岩石的接触时间必须至少为3分钟。
根据本发明方法操作的优点从图2与图3可明显看出。图2是根据本发明方法处理三种不同脉石所得的色谱图,图3是根据通常加热脱吸方法处理上述三种样品所得的色谱图。马上可以看出,某些烃只有用本发明方法才能鉴定出,而用通常加热脱吸方法无法鉴定。
步骤(B)完成后,在惰性气体物流中加热样品管至-温度使提取出的烃完全移去(步骤C)。在优选的气体流速20-60毫升/分时,样品管应加热至220-340℃、优选240-320℃、更优选至约300℃。
然后,在一装置中、优选在一阱中,使烃蒸汽冷凝(步骤D),冷却以保证烃蒸汽完全冷凝。在本发明一优选实施方案中,将阱冷却至-100℃至-20℃、优选至约-30℃。这样,先前含于脉石中的所有重烃都被冷凝。如果也要分析较轻的烃,可冷却至-150℃。在此温度下,所有的轻质烃也被冷凝,但是它们的分析-对可得到的信息不太重要-被步骤(A)中所用的溶剂干扰。
该肼必须由耐热惰性材料制成,使其不会释放出可污染待分析组分的物质。
烃在肼中冷凝后,通过将先前冷却的肼加热至220-340℃、且优选至约300℃(步骤E),将烃在惰性气体物流中加到气相色谱柱中。
烃的分离和分析是常用的气相色谱,可与质谱联用。
本发明还提供了用于分析含于脉石中的烃、特别是重烃的装置,它包括-可同时使用-可移动的加热器-惰性材料的样品管,用配有压力调节器和指示计及电磁阀输送的惰性气体通过该样品管,样品管的出口与多向阀连通,多向阀经-界面与肼连通,该肼可冷凝源于待分析样品和所用溶剂的蒸汽,并且(如需要)通过在惰性气体物流中加热又可将它们释放出去;该肼与分离与分析系统连接,该装置的特征在于在所述电磁阀与所述样品管之间装有气体的单向控制单元和加热单元。
在优选实施方案中,所述单向控制单元由单向阀或毛细管限制系统组成,加热单元由电阻单元组成。
非限定性地,所述装置可配有用于清洗管道中积聚的烃杂质的系统,该系统由装有选自用于提取中的溶剂的小容器组成,灯芯浸在该溶剂中。
图4示出了本发明的设备的优选实施方案,对本发明作非限制说明。
在图4中,1表示两个交替操作的电磁开关阀;2是压力调节器;3是示压计;4是非限定性的管道清洗装置;5是旁路管道;6是一电磁阀;7是用作单向控制单元的毛细管,它也可以是一单向阀;8是用电阻单元加热至约150℃的管道段,但是,加热系统也可由耐热浆膏(Paste)组成,其中装有控温的电阻和/或热电隅;9是样品管;10是可移动加热器,由稳定在操作温度的适宜形状的铝块组成;11是多向阀;12是三向阀;13是可在-150至340℃操作的肼;14是气相色谱加热器;15是分流器阀;16是通用的电导型或火陷离子化型气相色谱检测计;17是分流阀;18是气相色谱柱;19是可调节排气阀。
参照图4,本发明装置按下列方式操作。
输送气体或是氢气或是氦气,由气相色谱检测计确定。用氢气时,其进口压力约为0.5kg/Cm2,氦气时,压力为0.7-0.8Kg/Cm2。使气体通过开关1,然后用调节器调整压力至希望值,压力值由示压计3读出。非限定性地,该气体可通过含有溶剂的装置4(该溶剂通常是用于从脉石中提取烃的溶剂),使气体夹带部分溶剂,以清除先前分析时残留在管道中的痕量烃。经过4以后,输送气体分成两支。
借助于多向阀和管道5可将提取出的和加热脱吸的烃从肼13中转移至气相色谱柱中。另一支包括替换样品管时关闭的电磁阀6、限制单元7、控温管道8、样品管9和加热器10。
岩石样品适当研磨,并与几微升溶剂一起放于样品管中。在烃转移过程中,多向阀11用控温金属块10恒温至约300℃,以防止烃的再冷凝。阀11关闭通向样品管9的通路,将样品管装有待分析样品和所用溶剂的那一端加热至约95℃,至少保持3分钟。在此步骤中,从岩石中提取出来的烃在样品管9另一较冷的端冷凝,并且样品管中气体用阀11堵住,因而可使管道5中的输送气体向下游流动。
溶剂与待鉴定脉石的热接触完成以后,已恒温于约300℃的加热器10移至样品管,同时切换阀11。因而切断管道5中的气体输送,使加热脱吸的提取物从样品管转移至肼13中。在此步骤中,三向阀12与关闭的电磁阀17连通。几微升溶剂产生的蒸汽不能立即转移至冷却的阱中,它会向进料管道反向扩散。毛细管限制单元7和加热管线段8防止这种反向扩散和冷凝现象,因而使蒸汽按要求流出。
在阱中冷凝蒸汽的时间通常需要约15分钟。
阱冷却至约-30℃时,由于二氯甲烷溶剂极易挥发,该溶剂和轻烃不会全部保持在阱中,而重烃可以。
用惰性气体将没有保持在阱中的所有物质转移至气相色谱加热器14中,在此进入与可调节分流器15连接的支管,在此步骤中,该支管打开使轻烃排到外面,并且气相色谱柱18与检测计16连接。
根据色谱柱与分流器之间的压降比,输送气体还部分进入气相色谱柱18中。由于色谱柱加热器在约50℃,迫使输送气体中的二氯甲烷排出色谱柱,在此检测计可检测它的存在,在整个步骤之后用一电位计与检测计连接,所显示的巨大溶剂峰即时消失。
提取和脱吸步骤之后,将阱迅速升温至约300℃,关闭分流器,迫使释放出来的烃只能进入色谱柱18中,该色谱柱按一定程序降温(例如2分钟升至50℃、再过2分钟升至100℃,40分钟后升温至300℃,在300℃保持20分钟并在10分钟内恢复至50℃),进行气相色谱分析,可与质谱联用。
程序升温以后,分流器15重新打开恢复至起始状态。
在气相色谱分析过程中,不改变阀11的状态,可放入只装有玻璃棉的新样品管9。通过操作三向阀12,该样品管可与阀19连通。由于可手工移动加热器10,可将其移至样品管,惰性气体物流可通过阀19除去含于玻璃棉中的污染物。该去污染操作使分析更准确且不用中断任何操作步骤即可进行。
操作完以后,操作若将阀12设置在起始状态,使该系统准备进行新的分析。
Claims (15)
1、一种分离和分析含于沉积岩中的烃、特别是重烃的方法,其特征为包括下列步骤:
A)将沉积岩样品和可提取含于岩石中的烃的一种或多种溶剂置于一样品管中;
B)将该样品管在惰性气体中预热至60-150℃并在此温度下保持一定时间;
C)在惰性气体物流中加热该样品管,使溶剂和原先含于岩石中的烃完全移去;
D)在一冷却容器中冷凝由惰性气体输送的蒸汽;
E)加热该容器并用所述惰性输送气体将容器中的物质加到分离和分析装置中。
2、权利要求1的方法,其特征为,该惰性溶剂选自常压下沸点低于约100℃的烃或氯代烃。
3、权利要求2的方法,其特征为,该惰性溶剂为二氯甲烷。
4、权利要求1的方法,其特征为,溶剂与脉石的接触时间(步骤B)至少为3分钟。
5、权利要求1的方法,其特征为,步骤B在80-110℃下进行。
6、权利要求1的方法,其特征为,在步骤C中,样品管加热至220-340℃的温度。
7、权利要求6的方法,其特征为,该温度为240-320℃。
8、权利要求7的方法,其特征为,该温度为约300℃。
9、权利要求1的方法,其特征为,在步骤D中,蒸汽被冷却至-100至-30℃而被冷凝。
10、权利要求1的方法,其特征为,在步骤E中,将先前冷却的容器加热至220-340℃。
11、用于分析含于脉石中的烃、特别是重烃的装置,它包括-可同时使用-可移动的加热器-惰性材料的样品管,使用配有压力调节器和指示计及电磁阀的管道输送的惰性气体通过该样品管,样品管的出口与多向阀连通,多向阀经一界面与肼连通,该肼可冷凝源于待分析样品和所用溶剂的蒸汽,并且(如需要)通过在惰性气体物流中加热又可将它们释放出去;该肼与分离与分析系统连接,该装置的特征在于在所述电磁阀与所述样品管之间装有气体的单向控制单元和加热单元。
12、权利要求11的装置,其特征在于,该单向控制单元为单向阀;
13、权利要求11的装置,其特征在于,该单向控制单元为毛细管限制单元。
14、权利要求11的装置,其特征在于,该加热单元是-电阻单元。
15、权利要求11的装置,其特征在于,在压力调节器和指示计与多向阀之间配有装有溶剂的容器,灯芯浸在该溶剂中。
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ITMI930519A IT1272110B (it) | 1993-03-19 | 1993-03-19 | Procedimento per la determinazione di idrocarburi pesanti in matrici rocciose ed apparecchiatura utile allo scopo |
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US5719323A (en) * | 1996-04-12 | 1998-02-17 | The United States Of America As Represented By The Secretary Of The Army | Method of measuring the decomposition of a gaseous material under controlled temperature and time conditions |
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-
1993
- 1993-03-19 IT ITMI930519A patent/IT1272110B/it active IP Right Grant
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1994
- 1994-03-15 EP EP94200658A patent/EP0616214A1/en not_active Withdrawn
- 1994-03-16 US US08/213,707 patent/US5390529A/en not_active Expired - Fee Related
- 1994-03-17 NO NO940971A patent/NO940971L/no unknown
- 1994-03-18 CN CN94102931.XA patent/CN1094163A/zh active Pending
- 1994-03-18 CA CA002119415A patent/CA2119415A1/en not_active Abandoned
- 1994-03-18 BR BR9401210A patent/BR9401210A/pt not_active Application Discontinuation
- 1994-03-18 JP JP6074044A patent/JPH06324024A/ja not_active Withdrawn
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ITMI930519A1 (it) | 1994-09-19 |
US5390529A (en) | 1995-02-21 |
CA2119415A1 (en) | 1994-09-20 |
IT1272110B (it) | 1997-06-11 |
BR9401210A (pt) | 1994-12-27 |
EP0616214A1 (en) | 1994-09-21 |
NO940971L (no) | 1994-09-20 |
ITMI930519A0 (it) | 1993-03-19 |
NO940971D0 (no) | 1994-03-17 |
JPH06324024A (ja) | 1994-11-25 |
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