CN117129618A - Online measurement and analysis method for atmospheric organic amine - Google Patents

Online measurement and analysis method for atmospheric organic amine Download PDF

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Publication number
CN117129618A
CN117129618A CN202211079377.1A CN202211079377A CN117129618A CN 117129618 A CN117129618 A CN 117129618A CN 202211079377 A CN202211079377 A CN 202211079377A CN 117129618 A CN117129618 A CN 117129618A
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China
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liquid
gas
organic amine
absorption
atmospheric
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CN202211079377.1A
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Chinese (zh)
Inventor
温天雪
刘广仁
刘子锐
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Institute of Atmospheric Physics of CAS
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Institute of Atmospheric Physics of CAS
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Priority to CN202211079377.1A priority Critical patent/CN117129618A/en
Publication of CN117129618A publication Critical patent/CN117129618A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/96Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation using ion-exchange
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

Abstract

The application provides an on-line measuring and analyzing method for atmospheric organic amine, wherein an air pump pumps gas to be measured into an absorption tube after passing through a particle filter; the peristaltic pump pumps the absorption liquid out of the absorption bottle into the absorption tube; the gas to be tested and the absorption liquid are respectively introduced from the horizontal end and the vertical end of the tee joint and then are mixed in the absorption pipe in a same-direction circulation manner; the mixed gas and liquid are respectively sent to the gas-liquid separator under the flow rate control of a mass flow controller and a peristaltic pump stepping motor controller, and the peristaltic pump sends the liquid from which the gas is stripped by the gas-liquid separator to the ion chromatographic analysis device, and the device automatically analyzes the content of the organic amine. The successful research and development of the technical scheme can realize the automatic measurement of the organic amine gaseous substances in the atmosphere polluted by the indoor and outdoor atmospheric environments and the periphery of the emission source, can be used for emission control monitoring of the atmospheric organic amine pollution sources, can also be used for concentration change monitoring of the organic amine in the atmospheric environment, and provides a favorable research means and method for the formation mechanism of the atmospheric particulate matter pollution.

Description

Online measurement and analysis method for atmospheric organic amine
Technical Field
The application relates to an atmospheric quality detection technology, in particular to an online analysis method of atmospheric organic amine.
Background
The liquid organic amine substance is mainly measured by spectrophotometry, gas chromatography, high performance liquid chromatography and ion chromatography. When the methods are used for measuring the atmospheric gaseous organic amine, most of the methods need to collect an atmospheric amine sample by a collector, and then analyze the atmospheric amine sample by an analysis instrument after a complex pretreatment process.
On-line measurement analysis refers to an analysis technique that adopts an automatic sampling system to automatically sample a sample and then inputs the sample into an analysis instrument for continuous or intermittent continuous analysis. The analysis method can not automatically collect and analyze online, and needs to collect offline and analyze. The best detection mode capable of realizing automatic acquisition and online analysis is time-of-flight mass spectrometry, but the instrument equipment is very expensive and less.
Ion chromatography is a method for continuously separating, qualitatively and quantitatively determining a plurality of coexisting anions or cations by utilizing the ion exchange principle, and the method is accurate, efficient and sensitive. Ion chromatography is a conventional analytical instrument in most laboratories, and can accurately and quantitatively analyze organic amine in a liquid sample, but the analysis of gaseous organic amine can be performed only after the sample is absorbed into an absorption liquid, and automatic online analysis of atmospheric organic amine cannot be realized.
Disclosure of Invention
Aiming at the defects in the prior art, the application aims to provide an on-line measurement and analysis method for atmospheric organic amine, which is used for measuring the concentration of gaseous organic amine in the atmosphere based on ion chromatography analysis and specifically comprises the following steps:
pumping air by an air pump, filtering out atmospheric particulate matters by passing the air to be detected through a particle filter, and then guiding the air to an absorption pipe;
pumping liquid by a peristaltic pump, pumping the absorption liquid in an absorption liquid bottle into an absorption pipe, and mixing the filtered gas with the absorption liquid;
a temperature control device for heating the absorption tube to enable the absorption liquid to fully absorb the organic amine in the filtered gas;
the mixed gas-liquid enters a gas-liquid separator and is stripped into liquid to be detected and gas after adsorption, one end of the air pump, which is connected with a mass flow controller and the air pump, of the gas-liquid separator is used for pumping the gas after adsorption separated in the gas-liquid separator;
the peristaltic pump continuously pumps the liquid to be detected into ion chromatography, and automatic quantitative detection and analysis are carried out; when analysis starts, the peristaltic pump continuously pumps the liquid to be detected into the ion chromatography six-way valve sample inlet from the sample inlet, and the sample to be detected is directly pumped out from the waste liquid outlet; after 1 minute, the peristaltic pump continuously pumps the liquid to be measured into the ion chromatography six-way valve sample inlet from the sample inlet, and after the ion chromatography quantitative ring is continuously filled, the sample to be measured is pumped out from the liquid outlet until the analysis is finished; .
Further, a mass flow controller is arranged between the air pump and the vent hole of the gas-liquid separator to control the flow rate of the filtered gas.
Further, the ratio of the flow rate of the absorption liquid to the flow rate of the filtered gas is in the range of 0.1-1×10 -3 . The flow rate of the absorption liquid in the ambient atmosphere is 0.2-0.5 ml.min -1 The flow rate of the filtered gas is 1-2 L.min -1 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the absorption liquid in the polluted atmosphere is 0.5-1 ml.min -1 The gas flow rate is 0.5-1 L.min -1 。。
Further, the absorption liquid is water or methane sulfonic acid with the concentration of 20-40 mM.
Further, in the case where the absorption liquid is water, the length of the absorption tube is 1.5 meters.
Further, the absorber tube is a standard stainless steel tube of one eighth the length.
Further, the time for the ion chromatography device to analyze the sample in a single time is 30 minutes or longer.
Further, the absorption liquid and the gas to be detected flow in the same direction in the absorption tube, and are fully contacted and mixed.
An on-line measuring device for atmospheric organic amine, wherein a controller controls the device to measure the concentration of gaseous organic amine in the atmosphere based on ion chromatography, and the device comprises a power device, a control device, a sampling unit, a mixing unit, a separation unit and a detection unit;
the power device comprises an air extracting pump and a peristaltic pump and is used for providing power support for the flow of gas and liquid;
the control device includes: the temperature control device is used for controlling the temperature of the absorption tube, and the flow control device is used for controlling the flow rate of the air pump;
the sampling unit comprises a particle filter for filtering particulate matters possibly containing organic amine in the atmosphere;
the mixing unit comprises an absorption pipe for absorbing organic amine in the gas to be detected;
the separation unit comprises a gas-liquid separator for separating the absorption liquid and the gas flow after passing through the absorption pipe;
the detection unit comprises an ion chromatography analysis device and a peristaltic pump, wherein the peristaltic pump is used for conveying absorption liquid into ion chromatography; the ion chromatographic analysis device is provided with a sample inlet, a sample outlet, a six-way valve and a quantitative ring;
the air pump pumps the air to be detected into the absorption tube after passing through the particle filter; pumping the absorption liquid from the absorption bottle into the absorption tube by the peristaltic pump; the gas to be detected and the absorption liquid are mixed together after flowing in the same direction in the absorption tube; the mixed gas and liquid are sent to the gas-liquid separator under the control of the flow rate of the mass flow controller and the peristaltic pump stepping motor controller, and the peristaltic pump sends the liquid from which the gas is stripped by the gas-liquid separator to the ion chromatographic analysis device, and the device automatically analyzes the content of the organic amine.
Further, the ion chromatographic analysis device comprises a sample outlet, a sample inlet, a six-way valve and a quantitative ring, wherein the liquid to be detected enters the six-way valve from the sample inlet, and is pumped out from the sample outlet or directly pumped out from the sample outlet after being filled and quantified by the quantitative ring.
Further, the gas-liquid separator comprises a sample inlet, a vent hole and a sample outlet, the air pump is connected with the vent hole, after the sample to be tested enters the gas-liquid separator from the sample inlet, the air pump pumps the gas in the liquid away through the vent hole, and the sample to be tested flows out from the sample outlet.
Further, the absorption pipes are arranged in a reciprocating manner so as to increase the mixing time of the gas to be detected and the absorption liquid, and the organic amine is fully absorbed.
Further, the detection limit of the organic amine on-line measuring device for methylamine, dimethylamine and trimethylamine can be less than 10 mu g.m -3
The successful research and development of the system can realize the automatic measurement of the organic amine gaseous substances in the indoor and outdoor atmospheric environment and the polluted atmosphere around the emission source, can be used for the emission control and monitoring of the atmospheric organic amine pollution source, can also be used for the atmospheric observation of the concentration change of the organic amine in the atmospheric environment, and provides a favorable research means and method for the formation mechanism of the atmospheric particulate matter pollution.
According to the technical scheme, the absorption tube is connected with the ion chromatography sample inlet in series, so that automatic online measurement of the atmospheric organic amine is realized, and the aging problem of offline measurement of the atmospheric organic amine is solved; the peristaltic pump and the air pump are used for respectively controlling the flow rate of the absorption liquid and the flow rate of the gas to be detected, so that the gas to be detected slowly passes through the absorption liquid and is fully mixed with the absorption liquid, the absorption efficiency of the atmospheric organic amine is enhanced, and the detection limit of the atmospheric organic amine is also improved; the detection limit of the technical scheme is close to that of an off-line analysis method of the ecological environment department HJ1076-2019, and meets the national use standard.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a schematic diagram of an on-line measuring device according to an embodiment of the present application;
in the figure: 1-a particle filter; 2-an absorption tube; 3-a temperature control device; 4-a gas-liquid separator; a 5-mass flow controller; 6-an air extracting pump; 7-peristaltic pump; 8-an absorption liquid bottle; 9-ion chromatography apparatus.
Detailed Description
The present application will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present application, but are not intended to limit the application in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept.
Specific embodiments of the present application are described below. It is to be understood that the application is not limited to the particular embodiments described above, and that various changes or modifications may be made by those skilled in the art within the scope of the appended claims without affecting the spirit of the application. The embodiments of the application and the features of the embodiments may be combined with each other arbitrarily without conflict.
The method mainly comprises the steps of collecting by an absorption tube 2, and then carrying out off-line analysis by using gas chromatography, ion chromatography and other analysis instruments. The concentration of gaseous organic amine in the atmosphere is measured based on the ion chromatography measuring and analyzing device 9, and an automatic online analysis system of the organic amine in the atmosphere is formed by combining the ion chromatography and a liquid path design of automatic sample introduction of an absorption liquid, and specifically comprises the following steps:
by combining the liquid path design of automatic sample injection of an absorption liquid with ion chromatography, an air pump 6 pumps air, and the environment atmosphere containing organic amine, namely the gas to be detected, passes through a particle filter 1, filters out the atmospheric particulate matters and then is led into an absorption pipe; the gas to be tested without particulate matters enters the atmospheric organic amine absorption tube 2 under the action of the air pump 6, and the flow rate of the gas is 2L/min.
Pumping liquid by a peristaltic pump 7, pumping the absorption liquid in an absorption liquid bottle 8 into an absorption pipe 2, and mixing the filtered gas with the absorption liquid; a temperature control device 3 for controlling the temperature of the absorption tube 2 so that the absorption liquid sufficiently absorbs the organic amine in the filtered gas; the mixed gas-liquid enters the gas-liquid separator 4 and is divided into liquid to be detected and gas after adsorption, the air pump 6 is connected with an air vent at one end of the gas-liquid separator 4, and the gas after adsorption separated in the gas-liquid separator 4 is pumped out;
the peristaltic pump 7 pumps the liquid to be measured into the ion chromatographic device 9 from the sample inlet continuously, and the flow rate is 0.2-1 ml.min -1 And (5) quantitatively detecting and analyzing the end of the cyclic sampling to finish all detection.
A flow controller is arranged between the air pump 6 and the vent hole of the gas-liquid separator 4 to control the flow rate of the filtered gas.
The technical scheme is that an online trapping and absorbing device is constructed by utilizing the alkaline and water-soluble characteristics of organic amine, the absorbing liquid is water or 20-40mM methane sulfonic acid solution, and the absorbing liquid used in the embodiment is 20mM methane sulfonic acid.
In some alternative embodiments, the absorption liquid may be water, which has low solubility, and a thin and long absorption tube is needed to mix the gas and the liquid more fully.
In some alternative embodiments, the absorption liquid may be dilute sulfuric acid or dilute hydrochloric acid
In the case that the absorption liquid is water, the length of the absorption tube is 1.5 m.
In this embodiment, the absorber tube 2 is an eighth of a standard stainless steel tube. The time for the ion chromatography device to analyze the sample once is 30 minutes or more. The absorption liquid and the gas to be detected flow in the absorption tube in the same direction, and are fully contacted and mixed.
Under the action of the detection method and the detection device of the embodiment, the organic amine online measurement device can limit the detection of methylamine, dimethylamine and trimethylamine to be less than 10 mu g.m -3
The successful research and development of the system can realize the automatic measurement of the organic amine gaseous substances in the indoor and outdoor atmospheric environment and the polluted atmosphere around the emission source, can be used for the emission control and monitoring of the atmospheric organic amine pollution source, can also be used for the atmospheric observation of the concentration change of the organic amine in the atmospheric environment, and provides a favorable research means and method for the formation mechanism of the atmospheric particulate matter pollution.
According to the technical scheme, the absorption tube is connected with the ion chromatography quantitative ring in series, so that automatic online measurement of the atmospheric organic amine is realized, and the aging problem of offline measurement of the atmospheric organic amine is solved; the peristaltic pump and the air pump are used for respectively controlling the flow rate of the absorption liquid and the flow rate of the gas to be detected, so that the gas to be detected slowly passes through the absorption liquid and is fully contacted and mixed with the absorption liquid, the absorption efficiency of the atmospheric organic amine is enhanced, and the detection limit of the atmospheric organic amine is also improved.

Claims (10)

1. An on-line measuring and analyzing method for atmospheric organic amine, which is based on ion chromatography measuring and analyzing to determine the concentration of gaseous organic amine in the atmosphere, comprises the following steps:
pumping air by an air pump, filtering out atmospheric particulate matters by passing the air to be detected through a particle filter, and then guiding the air to an absorption pipe;
pumping liquid by a peristaltic pump, pumping the absorption liquid in an absorption liquid bottle into an absorption pipe, and mixing the filtered gas with the absorption liquid;
three-way drainage, introducing gas and liquid into the absorption tube simultaneously
A temperature control device for controlling the temperature of the absorption tube so that the absorption liquid fully absorbs the organic amine in the gas at a set temperature;
the mixed gas-liquid enters a gas-liquid separator and is stripped into liquid to be detected and gas after adsorption, one end of the air pump and one end of the gas-liquid separator are connected with a mass flow control and air pump, and the gas after adsorption separated in the gas-liquid separator is pumped out;
the peristaltic pump continuously pumps the liquid to be detected into ion chromatography, and automatic quantitative detection and analysis are carried out; when analysis starts, the peristaltic pump continuously pumps the liquid to be detected into the ion chromatography six-way valve sample inlet from the sample inlet, and the sample to be detected is directly pumped out from the waste liquid outlet; after 1 minute, the peristaltic pump continuously pumps the liquid to be measured into the ion chromatography six-way valve sample inlet from the sample inlet, and after the ion chromatography quantitative ring is continuously filled, the sample to be measured is pumped out from the liquid outlet until the analysis is finished; and (5) cycling until the sampling is finished and all detection is finished.
2. The method for on-line measurement and analysis of an atmospheric organic amine according to claim 1, wherein the temperature control device controls the temperature of the absorption tube in a range of 20 to 30 degrees.
3. The method according to claim 1, wherein a flow controller is provided between the suction pump and the vent hole of the gas-liquid separator to control the flow rate of the filtered gas.
4. The method for on-line measurement and analysis of an atmospheric organic amine according to claim 3, wherein a ratio of a flow rate of the absorption liquid to a flow rate of the filtered gas is in a range of 0.1 to 1X 10 -3 . The flow rate of the absorption liquid in the ambient atmosphere is 0.2-0.5 ml.min -1 The flow rate of the filtered gas is 1-2 L.min -1 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the absorption liquid in the polluted atmosphere is 0.5-1 ml.min -1 The gas flow rate is 0.5-1 L.min -1
5. The method for on-line measurement and analysis of atmospheric organic amine according to claim 1, wherein the absorption liquid is water or a methane sulfonic acid solution of 20-40 mM.
6. The method for on-line measurement and analysis of an atmospheric organic amine according to claim 1, wherein in the case where the absorption liquid is water, the length of the absorption tube is 1.5 m.
7. The method for on-line measurement and analysis of atmospheric organic amine according to claim 1, wherein the absorption tube is one eighth of a standard stainless steel tube.
8. The method according to claim 1, wherein the time for the ion chromatography device to analyze the sample in a single pass is 30 minutes or longer.
9. The method for on-line measurement and analysis of an atmospheric organic amine according to claim 1, wherein the absorption liquid and the gas to be measured flow in the same direction in the absorption tube, are fully contacted and mixed.
10. The device for on-line measurement of atmospheric organic amine according to claim 1, wherein the detection limit of methylamine, dimethylamine and trimethylamine by the device for on-line measurement of organic amine is less than 10. Mu.g.m -3
CN202211079377.1A 2022-09-05 2022-09-05 Online measurement and analysis method for atmospheric organic amine Pending CN117129618A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211079377.1A CN117129618A (en) 2022-09-05 2022-09-05 Online measurement and analysis method for atmospheric organic amine

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211079377.1A CN117129618A (en) 2022-09-05 2022-09-05 Online measurement and analysis method for atmospheric organic amine

Publications (1)

Publication Number Publication Date
CN117129618A true CN117129618A (en) 2023-11-28

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Family Applications (1)

Application Number Title Priority Date Filing Date
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