CN112666108B - Method for detecting mixed gas after pyrolysis of environment-friendly gas by infrared spectrum - Google Patents
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- 238000000197 pyrolysis Methods 0.000 title claims abstract description 25
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 17
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- 238000001514 detection method Methods 0.000 claims abstract description 58
- 239000001307 helium Substances 0.000 claims abstract description 35
- 229910052734 helium Inorganic materials 0.000 claims abstract description 35
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000012159 carrier gas Substances 0.000 claims abstract description 21
- 239000012535 impurity Substances 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000004458 analytical method Methods 0.000 claims abstract description 9
- 238000004566 IR spectroscopy Methods 0.000 claims description 14
- 230000007613 environmental effect Effects 0.000 claims description 12
- 239000002808 molecular sieve Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims 1
- 238000004451 qualitative analysis Methods 0.000 abstract description 8
- 238000011160 research Methods 0.000 abstract description 4
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- 238000010586 diagram Methods 0.000 description 5
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 1
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- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及环保气体及其混合气体热解后的检测分析领域，尤其涉及一种涉及红外光谱对环保气体热解后混合气体检测方法。The invention relates to the detection and analysis field of environmental protection gas and its mixed gas after pyrolysis, in particular to a method for detecting the mixed gas after pyrolysis of environmental protection gas by infrared spectroscopy.
背景技术Background technique
环保绝缘气体C4F7N、C5F10O、C6F12O在电气设备中作为绝缘介质使用时需要与一些缓冲气体CO2、N2等混合，而检测这些混合气体在高温下的分解产物是环保型绝缘气体替代SF6作为绝缘介质研究的重要环节。而目前的实验过程中存在掺杂其他气体的问题，掺杂其他气体后的混合气体对红外光谱图定性分析产生了干扰，严重影响了实验结果的准确性。Environmentally friendly insulating gases C 4 F 7 N, C 5 F 10 O, and C 6 F 12 O need to be mixed with some buffer gases such as CO 2 and N 2 when they are used as insulating media in electrical equipment. The detection of the decomposition products of these mixed gases at high temperatures is an important link in the research of environmentally friendly insulating gases instead of SF 6 as insulating media. However, in the current experiment process, there is a problem of doping with other gases. The mixed gas after doping with other gases interferes with the qualitative analysis of the infrared spectrum, which seriously affects the accuracy of the experimental results.
发明内容Contents of the invention
针对上述现有技术的不足，本专利设置了一种涉及红外光谱对环保气体热解后混合气体检测方法，该方法减少了产物种类繁多对红外光谱图定性分析的干扰，以满足科研人员在限有测量仪器下对产物进行分析研究。In view of the shortcomings of the above-mentioned prior art, this patent sets up a method for detecting mixed gases after pyrolysis of environmentally friendly gases involving infrared spectroscopy. This method reduces the interference of various types of products on the qualitative analysis of infrared spectrograms, and satisfies scientific research personnel. Analysis and research on products under limited measuring instruments.
为了实现上述目的，本发明为一种涉及红外光谱对环保气体热解后混合气体检测方法，该涉及红外光谱对环保气体热解后混合气体检测方法包括以下步骤：In order to achieve the above object, the present invention relates to a method for detecting mixed gas after pyrolysis of environmental protection gas by infrared spectroscopy, which involves the detection method of mixed gas after pyrolysis of environmental protection gas by infrared spectroscopy, comprising the following steps:
重复使用真空泵抽离第一气室、第二气室、第三气室和第四气室中的气体杂质；Repeatedly use the vacuum pump to extract the gas impurities in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber;
被测样品气体通入所述第一气室，并且打开载气阀门往所述第二气室、所述第三气室和所述第四气室中通入氦气使气压达到平衡；The sample gas to be measured is passed into the first gas chamber, and the carrier gas valve is opened to feed helium into the second gas chamber, the third gas chamber and the fourth gas chamber to balance the pressure;
打开第一阀门将所述第一气室中的气体通入样品池进行红外检测，再打开第二阀门对所述第二气室中的气体进行红外检测，重复此操作直至所述第一气室、所述第二气室、所述第三气室和所述第四气室里的气体红外检测完为止；Open the first valve to pass the gas in the first gas chamber into the sample cell for infrared detection, then open the second valve to carry out infrared detection for the gas in the second gas chamber, repeat this operation until the infrared detection of the gas in the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber is completed;
分别对所述第一气室、所述第二气室、所述第三气室和所述第四气室所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质；Comparatively analyze the infrared spectrograms measured in the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber respectively, and qualitatively analyze the specific substances in the mixed gas by calibration gas;
通过所述真空泵对所述第一气室、所述第二气室、所述第三气室和所述第四气室内的气体进行抽取；extracting the gas in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber by the vacuum pump;
将氦气通入所述第一气室、所述第二气室、所述第三气室和所述第四气室并达到平衡后干燥保存。The helium gas is passed into the first air chamber, the second air chamber, the third air chamber and the fourth air chamber to reach equilibrium and then be stored in a dry place.
作为本发明的一种优选技术方案，所述重复使用真空泵抽离第一气室、第二气室、第三气室和第四气室中的气体杂质，其中还包括：As a preferred technical solution of the present invention, the reusable vacuum pump is used to extract the gas impurities in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber, which also includes:
打开自动控制阀，使用所述真空泵抽离所述第一气室、所述第二气室、所述第三气室和所述第四气室中的氦气直至气压表示数为负的标准大气压为止，Open the automatic control valve, use the vacuum pump to evacuate the helium in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber until the air pressure indicates a negative standard atmospheric pressure,
作为本发明的一种优选技术方案，所述第一节管的顶端、所述第二节管的底端、所述第二节管的顶端、所述第三节管的底端、所述第三节管的顶端、所述第四节管的底端、所述第四节管的顶端和第五节杆的底端分别对称设置有两个弹性滚轮。As a preferred technical solution of the present invention, two elastic rollers are symmetrically arranged on the top of the first pipe, the bottom of the second pipe, the top of the second pipe, the bottom of the third pipe, the top of the third pipe, the bottom of the fourth pipe, the top of the fourth pipe and the bottom of the fifth rod.
作为本发明的一种优选技术方案，所述被测样品气体通入所述第一气室，并且打开载气阀门往所述第二气室、所述第三气室和所述第四气室中通入氦气使气压达到平衡，其中还包括：As a preferred technical solution of the present invention, the measured sample gas is passed into the first gas chamber, and the carrier gas valve is opened to feed helium gas into the second gas chamber, the third gas chamber and the fourth gas chamber so that the air pressure reaches equilibrium, which also includes:
关闭所述自动控制阀，再打开所述载气气阀通入氦气，通入一段时间后关闭所述载气气阀，待第一气压表、第二气压表、第三气压表和第四气压表示数达到平衡时再进行抽真空处理，重复以上步骤三次，实现去除离所述第一气室、所述第二气室、所述第三气室和所述第四气室和分子筛表面气体杂质的目的。Close the automatic control valve, open the carrier gas valve to feed helium, and close the carrier gas valve after a period of time, and then perform vacuum pumping when the first air pressure gauge, the second air pressure gauge, the third air pressure gauge and the fourth air pressure indicator reach a balance, and repeat the above steps three times to achieve the purpose of removing gas impurities from the surface of the first gas chamber, the second gas chamber, the third gas chamber, the fourth gas chamber and the molecular sieve.
作为本发明的一种优选技术方案，所述打开第一阀门将所述第一气室中的气体通入样品池进行红外检测，再打开第二阀门对所述第二气室中的气体进行红外检测，重复此操作直至所述第一气室、所述第二气室、所述第三气室和所述第四气室里的气体红外检测完为止，其中还包括：As a preferred technical solution of the present invention, the first valve is opened to pass the gas in the first gas chamber into the sample cell for infrared detection, and then the second valve is opened to conduct infrared detection for the gas in the second gas chamber, and this operation is repeated until the infrared detection of the gas in the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber is completed, which also includes:
打开所述第一阀门将所述第一气室中的气体通入样品池进行红外检测，检测完毕后再打开所述第二阀门对所述第二气室中的气体进行红外检测，打开所述第三阀门将所述第三气室中的气体通入样品池进行红外检测，检测完毕后再打开所述第四阀门对所述第四气室中的气体进行红外检测。Open the first valve to pass the gas in the first gas chamber into the sample cell for infrared detection, open the second valve to conduct infrared detection for the gas in the second gas chamber after the detection, open the third valve to pass the gas in the third gas chamber into the sample cell for infrared detection, and then open the fourth valve to perform infrared detection for the gas in the fourth gas chamber.
作为本发明的一种优选技术方案，所述分别对所述第一气室、所述第二气室、所述第三气室和所述第四气室所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质，其中还包括：As a preferred technical solution of the present invention, the infrared spectrograms of the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber are compared and analyzed respectively, and the specific substances in the mixed gas are qualitatively analyzed by calibration gas, which also includes:
对所述第一气室、所述第二气室、所述第三气室和所述第四气室里的气体所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质。The infrared spectrograms of the gas in the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber are compared and analyzed, and the specific substances in the mixed gas are qualitatively analyzed by calibration gas.
作为本发明的一种优选技术方案，所述通过所述真空泵对所述第一气室、所述第二气室、所述第三气室和所述第四气室内的气体进行抽取，其中还包括：As a preferred technical solution of the present invention, the vacuum pump is used to extract the gas in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber, which also includes:
检测完成后打开所述自动控制阀对所述第一气室、所述第二气室、所述第三气室和所述第四气室进行抽真空处理。After the detection is completed, the automatic control valve is opened to vacuumize the first air chamber, the second air chamber, the third air chamber and the fourth air chamber.
作为本发明的一种优选技术方案，所述将氦气通入所述第一气室、所述第二气室、所述第三气室和所述第四气室并达到平衡后干燥保存，其中还包括：As a preferred technical solution of the present invention, the helium gas is passed into the first air chamber, the second air chamber, the third air chamber and the fourth air chamber and stored in a dry state after reaching equilibrium, which also includes:
打开所述载气气阀往气室中通入氦气，待各级气室气压表达到平衡时即可将气体分离装置放入干燥的环境保存。Open the carrier gas valve to feed helium into the gas chamber, and put the gas separation device into a dry environment for storage when the air pressure of each level of the gas chamber reaches equilibrium.
作为本发明的一种优选技术方案，所述涉及红外光谱对环保气体热解后混合气体检测方法还包括：As a preferred technical solution of the present invention, the method for detecting mixed gas after pyrolysis of environment-friendly gas involving infrared spectroscopy also includes:
去除杂质系统，所述去除杂质系统用于重复使用真空泵抽离第一气室、第二气室、第三气室和第四气室中的气体杂质；The impurity removal system is used to repeatedly use the vacuum pump to remove the gaseous impurities in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber;
稳定气压系统，所述稳定气压系统用于被测样品气体通入所述第一气室，并且打开载气阀门往所述第二气室、所述第三气室和所述第四气室中通入氦气使气压达到平衡；Stable air pressure system, the stable air pressure system is used to pass the measured sample gas into the first air chamber, and open the carrier gas valve to feed helium into the second air chamber, the third air chamber and the fourth air chamber to balance the air pressure;
红外检测系统，所述红外检测系统用于打开第一阀门将所述第一气室中的气体通入样品池进行红外检测，再打开第二阀门对所述第二气室中的气体进行红外检测，重复此操作直至所述第一气室、所述第二气室、所述第三气室和所述第四气室里的气体红外检测完为止；An infrared detection system, the infrared detection system is used to open the first valve to pass the gas in the first gas chamber into the sample cell for infrared detection, and then open the second valve to perform infrared detection on the gas in the second gas chamber, repeating this operation until the infrared detection of the gas in the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber is completed;
红外光谱图分析系统，所述红外光谱图分析系统用于分别对所述第一气室、所述第二气室、所述第三气室和所述第四气室所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质；An infrared spectrogram analysis system, the infrared spectrogram analysis system is used to compare and analyze the infrared spectrograms measured in the first gas chamber, the second gas chamber, the third gas chamber and the fourth gas chamber respectively, and qualitatively analyze the specific substances in the mixed gas through calibration gas;
气体回收系统，所述气体回收系统用于通过所述真空泵对所述第一气室、所述第二气室、所述第三气室和所述第四气室内的气体进行抽取；a gas recovery system, the gas recovery system is used to extract the gas in the first air chamber, the second air chamber, the third air chamber and the fourth air chamber through the vacuum pump;
保存系统，所述保存系统用于将氦气通入所述第一气室、所述第二气室、所述第三气室和所述第四气室并达到平衡后干燥保存。A preservation system, the preservation system is used to pass helium gas into the first air chamber, the second air chamber, the third air chamber and the fourth air chamber, and dry and preserve after reaching equilibrium.
综上所述，由于本发明采用了上述技术方案，本发明具有以下技术效果：通过气体样品通入气体分离装置根据其分子直径的大小进行分离，再将分离的气体依次通入样品池进行红外光谱检测得到对应气体的红外光谱图，最后对比所得红外光谱图对混合气体进行准确的定性分析，减少了产物种类繁多对红外光谱图定性分析的干扰，以满足科研人员在限有测量仪器下对产物进行分析研究。In summary, because the present invention adopts the above-mentioned technical scheme, the present invention has the following technical effects: the gas sample is passed into the gas separation device to separate according to the size of its molecular diameter, and then the separated gas is sequentially passed into the sample cell for infrared spectrum detection to obtain the infrared spectrum of the corresponding gas, and finally the obtained infrared spectrum is compared to carry out accurate qualitative analysis of the mixed gas, reducing the interference of a wide variety of products on the qualitative analysis of the infrared spectrum, so that scientific researchers can analyze and study the product under limited measuring instruments.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其它的附图。In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the accompanying drawings that are required in the description of the embodiments or prior art. Obviously, the accompanying drawings in the following description are only some embodiments of the present invention. For those of ordinary skill in the art, other accompanying drawings can also be obtained based on these drawings without creative work.
图1是本发明的涉及红外光谱对环保气体热解后混合气体检测方法的操作流程图；Fig. 1 is the operation flowchart of the present invention related to the mixed gas detection method after pyrolysis of environment-friendly gas by infrared spectroscopy;
图2是本发明的对环保混合气体热解后产物分离装置的示意图。Fig. 2 is a schematic diagram of a device for separating products after pyrolysis of an environmentally friendly mixed gas according to the present invention.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.
需要说明的是，当一个元件被认为是“连接”另一个元件，它可以使直接连接到另一个元件或者可能同时存在居中设置的元件。当一个元件被认为是“设置在”另一个元件，它可以使直接设置在另一个元件上或者可能同时存在居中设置的元件。It should be noted that when an element is considered to be "connected" to another element, it may be directly connected to the other element or there may be an intervening element at the same time. When an element is said to be "disposed on" another element, it can be directly disposed on the other element or intervening elements may also be present.
除非另有定义，本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。本文所使用的术语“及/或”包括一个或多个相关的所列项目的任意的和所有的组合。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the technical field of the invention. The terms used herein in the description of the present invention are for the purpose of describing specific embodiments only, and are not intended to limit the present invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
下面结合附图，对本发明的实施例作详细说明。在不冲突的情况下，下述的实施例及实施例的特征可以相互组合。Embodiments of the present invention will be described in detail below in conjunction with the accompanying drawings. In the case of no conflict, the following embodiments and features of the embodiments can be combined with each other.
请参阅图1和图2，图1示出的本发明的涉及红外光谱对环保气体热解后混合气体检测方法的操作流程图；图2示出的本发明的对环保混合气体热解后产物分离装置的示意图。Please refer to Fig. 1 and Fig. 2, the operation flowchart of the present invention that Fig. 1 shows relates to infrared spectroscopy to the mixed gas detection method after the environmental protection gas pyrolysis; Fig. 2 shows the schematic diagram of the product separation device after the environmental protection mixed gas pyrolysis of the present invention.
具体的，本实验中发明实施例所示的涉及红外光谱对环保气体热解后混合气体检测方法包括一套对环保混合气体热解后产物分离装置，该装置包括第一气室11、第二气室12、第三气室13和第四气室14，第一气室11、第二气室12、第三气室13和第四气室14的底端均设置有分子筛气体分离膜17，且第一气室11、第二气室12、第三气室13和第四气室14从上到下依次叠放。Specifically, the method for detecting mixed gases after pyrolysis of environmentally friendly gases by infrared spectroscopy as shown in the embodiment of the invention includes a set of separation devices for products after pyrolysis of environmentally friendly mixed gases. The chambers 14 are stacked sequentially from top to bottom.
进一步的，第一气室11的上端设置有载气气阀15和样品气阀16，第一气室11的右侧设置有第一气压表21和第一阀门22。第一气室11经过第一阀门22与样品池19连接。Further, a carrier gas valve 15 and a sample gas valve 16 are provided on the upper end of the first gas chamber 11 , and a first air pressure gauge 21 and a first valve 22 are provided on the right side of the first gas chamber 11 . The first gas chamber 11 is connected with the sample cell 19 through the first valve 22 .
进一步的，第二气室12的右侧设置有第二气压表23和第二阀门24。第二气室12经过第二阀门24与样品池19连接。Further, a second air pressure gauge 23 and a second valve 24 are provided on the right side of the second air chamber 12 . The second air chamber 12 is connected with the sample cell 19 through the second valve 24 .
进一步的，第三气室13的右侧设置有第三气压表25和第三阀门26。第三气室13经过第三阀门26与样品池19连接。Further, a third air pressure gauge 25 and a third valve 26 are provided on the right side of the third air chamber 13 . The third air chamber 13 is connected with the sample cell 19 through the third valve 26 .
进一步的，第四气室14的右侧设置有第四气压表27和第四阀门28。第四气室14经过第四阀门28与样品池19连接。Further, a fourth air gauge 27 and a fourth valve 28 are provided on the right side of the fourth air chamber 14 . The fourth gas chamber 14 is connected to the sample cell 19 through a fourth valve 28 .
进一步的，第一气室11、第二气室12、第三气室13和第四气室14的左侧分别对应设置有自动控制阀29，基于自动控制阀29，第一气室11、第二气室12、第三气室13和第四气室14分别与真空泵18连接。Further, the left sides of the first air chamber 11, the second air chamber 12, the third air chamber 13, and the fourth air chamber 14 are respectively provided with automatic control valves 29. Based on the automatic control valves 29, the first air chamber 11, the second air chamber 12, the third air chamber 13, and the fourth air chamber 14 are respectively connected to the vacuum pump 18.
进一步的，第一气室11基于载气气阀15与氦气储存罐连接；第一气室11基于样品气阀16与被测样品连接。Further, the first gas chamber 11 is connected to the helium storage tank based on the carrier gas valve 15 ; the first gas chamber 11 is connected to the sample to be measured based on the sample gas valve 16 .
进一步的，第一气室11基于载气气阀15与氦气储存罐连接，向第一气室11通入氦气，通过氦气平衡气室气压、防止气室受潮影响实验结果，每次检测完成后往气室中通入氦气，待各级气室气压表有一定的示数即可，同时在对气室进行抽真空处理去除各级气室杂质时，可以剥离分子筛上吸附残留的样品杂质。氦气是的化学性能稳定不会与样品反应，分子直径小，不易不被分子筛吸附从而能够渗透到各级气室中。Further, the first gas chamber 11 is connected to the helium storage tank based on the carrier gas valve 15, and helium gas is introduced into the first gas chamber 11, and the air pressure of the gas chamber is balanced by helium to prevent the gas chamber from being affected by moisture. Experimental results are prevented. After each detection is completed, helium gas is passed into the gas chamber, and it is sufficient to wait until the barometers of the gas chambers at all levels have a certain reading. Helium has stable chemical properties and will not react with samples. Its molecular diameter is small, and it is difficult not to be absorbed by molecular sieves, so it can penetrate into all levels of gas chambers.
进一步的，设置自动控制阀29，因为红外检测前和检测完成后需要对气室抽真空处理，将真空泵18与各气室相连接，通过继电设备对其的开断进行控制，通过继电设备控制有效避免人为的疏忽从而造成的试验失败。Further, an automatic control valve 29 is set, because the air chamber needs to be evacuated before and after the infrared detection is completed, the vacuum pump 18 is connected to each air chamber, and its switching is controlled by a relay device, and the test failure caused by human negligence is effectively avoided by the relay device control.
进一步的，通过自动控制阀29与气室相连接，真空泵18可对气室抽真空去除各级气室内残留的杂质气体，保障实验结果的准确可靠。Further, through the connection of the automatic control valve 29 to the gas chamber, the vacuum pump 18 can vacuum the gas chamber to remove the residual impurity gases in the gas chambers at all levels, so as to ensure the accuracy and reliability of the experimental results.
进一步的，本发明装置中分为第一气室11、第二气室12、第三气室13和第四气室14，混合气体在此环境中被分离，气室级数越高，气室中被分离的气体直径越小，不同气体透过分子筛气体分离膜17进入到下一级气室时前后气室中气体浓度差较大，为了使前后气室的气体浓度尽快达到平衡，将下一级气室的体积设置比上一级气室的体积要小。Further, the device of the present invention is divided into the first gas chamber 11, the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14. The mixed gas is separated in this environment. The higher the number of gas chambers, the smaller the diameter of the separated gas in the gas chamber. When different gases pass through the molecular sieve gas separation membrane 17 and enter the next gas chamber, the gas concentration difference between the front and rear gas chambers is relatively large.
进一步的，分子筛气体分离膜17为一种人工合成的具有筛选分子作用的水合硅铝酸盐或天然沸石，它在结构上有许多孔径均匀的孔道和排列整齐的孔穴，不同孔径的分子筛把不同大小和形状分子分开，根据SiO2和Al2O3的分子比不同，得到不同孔径的分子筛，本装置中采用的分子筛尺寸随气室等级的增加而减少。Further, the molecular sieve gas separation membrane 17 is a kind of artificially synthesized hydrated aluminosilicate or natural zeolite with the function of screening molecules. It has many pores with uniform apertures and neatly arranged holes in its structure. Molecular sieves with different apertures separate molecules of different sizes and shapes. Molecular sieves with different apertures are obtained according to the molecular ratios of SiO2 and Al2O3. The size of the molecular sieve used in this device decreases with the increase of the gas chamber grade.
进一步的，第一气压表21、第二气压表23、第三气压表25和第四气压表27反应气室气压的变化，当每级气室气压表值不再发生变化时可以判断混合气体已经分离完成。Further, the first air pressure gauge 21, the second air pressure gauge 23, the third air pressure gauge 25 and the fourth air pressure gauge 27 reflect the change of air pressure in the air chamber, and when the air pressure gauge value of each air chamber no longer changes, it can be judged that the mixed gas has been separated.
进一步的，第一阀门22、第二阀门24、第三阀门26和第四阀门28按照顺序依次打开阀门将各气室的气体通入样品池19进行红外检测，每检测完一个气室的气体样品再打开下一个阀进行样品检测，每次阀门打开的时间不能太长，长时间的往样品池19进气会导致相邻两个等级的气室形成较高的气压差损坏分子筛气体分离膜17。Further, the first valve 22, the second valve 24, the third valve 26, and the fourth valve 28 are opened in order to pass the gas in each gas chamber into the sample cell 19 for infrared detection. After each gas sample in a gas chamber is detected, the next valve is opened for sample detection. The time for each valve to be opened should not be too long. Long-term intake of air into the sample cell 19 will cause a relatively high pressure difference between two adjacent levels of gas chambers and damage the molecular sieve gas separation membrane 17.
本发明装置基于膜分离技术可以对混合气体进行选择性分离，根据不同尺寸分子筛膜对不同直径大小气体分子具有选择透过作用。通过本装置的运行可以将不同大小的气体分子进行分离，将分离的气体依次通入样品池19进行红外检测，这样能够降低所得红外光谱图中峰重叠的概率，方便定性分析。The device of the invention can selectively separate the mixed gas based on the membrane separation technology, and the molecular sieve membranes of different sizes can selectively permeate gas molecules with different diameters. Through the operation of the device, gas molecules of different sizes can be separated, and the separated gases are sequentially passed into the sample cell 19 for infrared detection, which can reduce the probability of peak overlap in the obtained infrared spectrum and facilitate qualitative analysis.
具体的，所述涉及红外光谱对环保气体热解后混合气体检测方法包括以下步骤：Specifically, the method for detecting the mixed gas after pyrolysis of the environment-friendly gas involving infrared spectroscopy includes the following steps:
重复使用真空泵18抽离第一气室11、第二气室12、第三气室13和第四气室14中的气体杂质1；Reuse the vacuum pump 18 to extract the gas impurities 1 in the first air chamber 11, the second air chamber 12, the third air chamber 13 and the fourth air chamber 14;
被测样品气体通入所述第一气室11，并且打开载气阀门往所述第二气室12、所述第三气室13和所述第四气室14中通入氦气使气压达到平衡2；The measured sample gas is passed into the first gas chamber 11, and the carrier gas valve is opened to feed helium gas into the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14 to make the air pressure reach equilibrium 2;
打开第一阀门22将所述第一气室11中的气体通入样品池19进行红外检测，再打开第二阀门24对所述第二气室12中的气体进行红外检测，重复此操作直至所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14里的气体红外检测完为止3；Open the first valve 22 to pass the gas in the first gas chamber 11 into the sample cell 19 for infrared detection, then open the second valve 24 to carry out infrared detection for the gas in the second gas chamber 12, repeat this operation until the infrared detection of the gas in the first gas chamber 11, the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14 is completed;
分别对所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质4；Carry out comparative analysis of the infrared spectrograms measured by the first gas chamber 11, the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14, and qualitatively analyze the specific substance 4 in the mixed gas by calibration gas;
通过所述真空泵18对所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14内的气体进行抽取5；The gas in the first air chamber 11, the second air chamber 12, the third air chamber 13 and the fourth air chamber 14 is extracted 5 by the vacuum pump 18;
将氦气通入所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14并达到平衡后干燥保存6。Pass helium gas into the first air chamber 11 , the second air chamber 12 , the third air chamber 13 and the fourth air chamber 14 and keep it dry after reaching equilibrium.
具体的，所述重复使用真空泵18抽离第一气室11、第二气室12、第三气室13和第四气室14中的气体杂质1，其中还包括：Specifically, the reusable vacuum pump 18 is used to extract the gaseous impurities 1 in the first air chamber 11, the second air chamber 12, the third air chamber 13 and the fourth air chamber 14, which also includes:
打开自动控制阀29，使用所述真空泵18抽离所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14中的氦气直至气压表示数为负的标准大气压为止。Open the automatic control valve 29, use the vacuum pump 18 to evacuate the helium in the first air chamber 11, the second air chamber 12, the third air chamber 13 and the fourth air chamber 14 until the air pressure is negative standard atmospheric pressure.
具体的，所述被测样品气体通入所述第一气室11，并且打开载气阀门往所述第二气室12、所述第三气室13和所述第四气室14中通入氦气使气压达到平衡2，其中还包括：Specifically, the measured sample gas is passed into the first gas chamber 11, and the carrier gas valve is opened to feed helium gas into the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14 to make the air pressure reach equilibrium 2, which also includes:
关闭所述自动控制阀29，再打开所述载气气阀15通入氦气，通入一段时间后关闭所述载气气阀15，待第一气压表21、第二气压表23、第三气压表25和第四气压表27示数达到平衡时再进行抽真空处理，重复以上步骤三次，实现去除离所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14和分子筛表面气体杂质的目的。Close the automatic control valve 29, open the carrier gas valve 15 to feed helium, and close the carrier gas valve 15 after a period of time. When the first air gauge 21, the second air gauge 23, the third air gauge 25, and the fourth air gauge 27 show a balance, then perform the vacuuming process. Repeat the above steps three times to achieve the purpose of removing gas impurities from the first gas chamber 11, the second gas chamber 12, the third gas chamber 13, the fourth gas chamber 14 and the molecular sieve surface.
具体的，所述打开第一阀门22将所述第一气室11中的气体通入样品池19进行红外检测，再打开第二阀门24对所述第二气室12中的气体进行红外检测，然后到下个气室重复此操作直至所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14里的气体红外检测完为止3，其中还包括：Specifically, the first valve 22 is opened to pass the gas in the first gas chamber 11 into the sample cell 19 for infrared detection, and then the second valve 24 is opened to conduct infrared detection for the gas in the second gas chamber 12, and then this operation is repeated in the next gas chamber until the infrared detection of the gas in the first gas chamber 11, the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14 is completed. 3, which also includes:
打开所述第一阀门22将所述第一气室11中的气体通入样品池19进行红外检测，检测完毕后再打开所述第二阀门24对所述第二气室12中的气体进行红外检测，打开所述第三阀门26将所述第三气室13中的气体通入样品池19进行红外检测，检测完毕后再打开所述第四阀门28对所述第四气室14中的气体进行红外检测。Open the first valve 22 to pass the gas in the first gas chamber 11 into the sample cell 19 for infrared detection. After the detection, open the second valve 24 to carry out infrared detection for the gas in the second gas chamber 12. Open the third valve 26 to pass the gas in the third gas chamber 13 into the sample cell 19 for infrared detection. After the detection, open the fourth valve 28 to carry out infrared detection for the gas in the fourth gas chamber 14.
具体的，所述分别对所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质4，其中还包括：Specifically, the infrared spectrograms of the first gas chamber 11, the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14 are compared and analyzed respectively, and the specific substance 4 in the mixed gas is qualitatively analyzed by calibration gas, which also includes:
对所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14里的气体所测得红外光谱图进行对比分析，通过标气定性分析混合气体中的具体物质。The infrared spectrograms of the gas in the first gas chamber 11, the second gas chamber 12, the third gas chamber 13 and the fourth gas chamber 14 are compared and analyzed, and the specific substances in the mixed gas are qualitatively analyzed by calibration gas.
具体的，所述通过所述真空泵18对所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14内的气体进行抽取5，其中还包括：Specifically, the gas in the first air chamber 11, the second air chamber 12, the third air chamber 13 and the fourth air chamber 14 is extracted 5 by the vacuum pump 18, which also includes:
检测完成后打开所述自动控制阀29对所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14进行抽真空处理。After the detection is completed, the automatic control valve 29 is opened to vacuumize the first air chamber 11 , the second air chamber 12 , the third air chamber 13 and the fourth air chamber 14 .
具体的，所述将氦气通入所述第一气室11、所述第二气室12、所述第三气室13和所述第四气室14并达到平衡后干燥保存6，其中还包括：Specifically, the said helium gas is passed into the first air chamber 11, the second air chamber 12, the third air chamber 13 and the fourth air chamber 14 and reaches equilibrium and then dried and stored 6, which also includes:
打开所述载气气阀15往气室中通入氦气，待各级气室气压表达到平衡时即可将气体分离装置放入干燥的环境保存。Open the carrier gas valve 15 to feed helium into the gas chamber. When the air pressures of the gas chambers at all levels are balanced, the gas separation device can be stored in a dry environment.
本发明，通过气体样品通入气体分离装置根据其分子直径的大小进行分离，再将分离的气体依次通入样品池进行红外光谱检测得到对应气体的红外光谱图，最后对比所得红外光谱图对混合气体进行准确的定性分析，减少了产物种类繁多对红外光谱图定性分析的干扰，以满足科研人员在限有测量仪器下对产物进行分析研究。In the present invention, the gas sample is passed into the gas separation device to separate according to the size of its molecular diameter, and then the separated gas is sequentially passed into the sample cell for infrared spectrum detection to obtain the infrared spectrum diagram of the corresponding gas, and finally the infrared spectrum diagram obtained is compared for accurate qualitative analysis of the mixed gas, which reduces the interference of various products on the qualitative analysis of the infrared spectrum diagram, and satisfies the needs of scientific researchers to analyze and study products under limited measuring instruments.
以上对本发明的实施例所提供的一种涉及红外光谱对环保气体热解后混合气体检测方法进行了详细介绍，本文中应采用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上，本说明书内容不应理解为对本发明的限制。The method for detecting mixed gases after pyrolysis of environmentally friendly gases by infrared spectroscopy provided by the embodiments of the present invention has been described in detail above. In this paper, specific examples should be used to illustrate the principles and implementation methods of the present invention. The descriptions of the above embodiments are only used to help understand the methods and core ideas of the present invention; meanwhile, for those of ordinary skill in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008298452A (en) * | 2007-05-29 | 2008-12-11 | Yokogawa Electric Corp | Infrared gas analyzer |
| CN202305402U (en) * | 2011-08-10 | 2012-07-04 | 重庆川仪分析仪器有限公司 | Infrared gas analyzer |
| CN102872689A (en) * | 2012-08-20 | 2013-01-16 | 中国计量学院 | Infrared differential spectroscopy-based biogas detection and purification control system |
| CN106970182A (en) * | 2017-04-21 | 2017-07-21 | 上海纳晶科技有限公司 | A kind of apparatus and method of on-line checking mixed gas concentration |
| CN107389585A (en) * | 2017-08-21 | 2017-11-24 | 湖北锐意自控系统有限公司 | A kind of gas analyzer and analysis method for gases |
-
2020
- 2020-11-27 CN CN202011362994.3A patent/CN112666108B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008298452A (en) * | 2007-05-29 | 2008-12-11 | Yokogawa Electric Corp | Infrared gas analyzer |
| CN202305402U (en) * | 2011-08-10 | 2012-07-04 | 重庆川仪分析仪器有限公司 | Infrared gas analyzer |
| CN102872689A (en) * | 2012-08-20 | 2013-01-16 | 中国计量学院 | Infrared differential spectroscopy-based biogas detection and purification control system |
| CN106970182A (en) * | 2017-04-21 | 2017-07-21 | 上海纳晶科技有限公司 | A kind of apparatus and method of on-line checking mixed gas concentration |
| CN107389585A (en) * | 2017-08-21 | 2017-11-24 | 湖北锐意自控系统有限公司 | A kind of gas analyzer and analysis method for gases |
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Application publication date: 20210416 Assignee: Guangxi Power Grid Energy Technology Co.,Ltd. Assignor: ELECTRIC POWER SCIENCE & RESEARCH INSTITUTE OF GUANGXI POWER GRID Corp. Contract record no.: X2024980029037 Denomination of invention: A method for detecting mixed gases after pyrolysis of environmentally friendly gases using infrared spectroscopy Granted publication date: 20230725 License type: Common License Record date: 20241202 |