CN216525760U - Automatic analysis device for analyzing gaseous total mercury - Google Patents

Automatic analysis device for analyzing gaseous total mercury Download PDF

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CN216525760U
CN216525760U CN202122704680.3U CN202122704680U CN216525760U CN 216525760 U CN216525760 U CN 216525760U CN 202122704680 U CN202122704680 U CN 202122704680U CN 216525760 U CN216525760 U CN 216525760U
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mercury
gaseous
gas
pipe
automatic
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张辉
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Institute of Geochemistry of CAS
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Institute of Geochemistry of CAS
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Abstract

The utility model relates to an automatic analysis device for analyzing gaseous total mercury, which comprises an automatic gas inlet mechanism, a gas inlet mechanism and a gas outlet mechanism, wherein the automatic gas inlet mechanism is provided with a first pipeline for conveying sample gas to be detected; the condensation and cracking mechanism is used for receiving the sample gas to be detected, enriching gaseous total mercury in the sample gas to be detected at low temperature, and resolving all gaseous total mercury in the sample gas to be detected into gaseous elemental mercury at high temperature; the automatic gas transmission mechanism is provided with a second pipeline for transmitting gaseous elemental mercury; the detection and analysis mechanism is used for analyzing the total concentration of the gaseous elemental mercury; and the controller is used for controlling the automatic operation of the automatic air inlet mechanism, the condensation and cracking mechanism and the automatic air conveying mechanism. The utility model can realize complete collection of the gaseous total mercury in the sample gas to be detected, and improves the accuracy of the total mercury concentration analysis of the sample gas to be detected, thereby really realizing the measurement of the total mercury content of the gas in the sample 0, simultaneously realizing simple, convenient and reliable online analysis technology, and reducing the analysis cost.

Description

Automatic analysis device for analyzing gaseous total mercury
Technical Field
The utility model relates to the field of sewage monitoring, in particular to an automatic analysis device for analyzing total mercury in water quality.
Background
Mercury is a toxic and harmful heavy metal element which exists only in a liquid state at normal temperature and normal pressure, and has volatility, so the element generally exists in nature, and can bring huge ecological risks to the ecological environment and cause human poisoning. Therefore, the united nations issued a global mercury public convention water guarantee with legal effectiveness after multiple rounds of negotiations and took effect on the global guarantee on 8/16/2017, aiming at reducing emission control and controlling mercury pollution. According to the requirements of the convention, environmental mercury needs to be monitored so as to evaluate the performance effect, so that the monitoring of the environmental mercury, especially the long-term monitoring of atmospheric mercury, is very important for evaluating the control measures and emission reduction effect of mercury pollution in China. In the case of atmospheric mercury, the physical and chemical forms of mercury are mainly divided into Gaseous Elemental Mercury (GEM), active gaseous mercury (GOM) and particulate mercury (PBM), and the sum of the three forms of mercury generally forms atmospheric gaseous total mercury (TGM). Atmospheric mercury is primarily from mercury emissions from man-made activities (man-made sources) and natural processes (natural sources). The man-made sources mainly include fossil fuel combustion, municipal and medical waste incineration, non-ferrous metal smelting, cement production, gold-smelting activities, chlor-alkali industry and the like, and the natural sources mainly include volcanic geothermal activities, soil and water surface volatilization, plant transpiration, forest fires and the like. The monitoring of the atmospheric mercury can know the distribution characteristics and the transmission rule of the atmospheric mercury, analyze the source of atmospheric mercury pollution, optimize the emission list of the atmospheric mercury, evaluate the long-term change trend of the atmospheric mercury, provide data support for mercury contract performance evaluation and the like. At present, the global measurement of gaseous mercury is mainly to remove air particles by using a Teflon filter membrane (the aperture is larger than 2 microns), then to enrich through a gold amalgam, then to carry the gas into an atomic fluorescence or atomic absorption mercury detector for analysis after heating and resolving. The method can only measure elemental mercury, a part of active mercury and granular mercury in the air, and cannot completely measure true gaseous total mercury.
In order to prevent the influence of large particles in a gas sample on a mercury enrichment tube and a detector, the traditional gaseous total mercury analysis needs to remove the large particles in the gas sample before mercury enrichment, only the particles smaller than PM2.5 are allowed to enter, so that most of the particulate mercury in the gas sample is removed, the analyzed gaseous total mercury does not contain most of the particulate mercury, in addition, the particles adsorbed on a filter membrane can also absorb elemental mercury and active mercury in the gas sample, and therefore, the measured gaseous total mercury concentration can be lower than the real total mercury concentration due to the reasons.
SUMMERY OF THE UTILITY MODEL
(1) Technical problem to be solved
The embodiment of the utility model provides an automatic analysis device for analyzing gaseous total mercury, which is characterized in that a controller is used for controlling an automatic air inlet mechanism to automatically input sample gas to be detected, a condensation and cracking mechanism is controlled to automatically realize low-temperature enrichment and high-temperature analysis of the gaseous total mercury in the sample gas to be detected step by step to obtain all gaseous elementary mercury, the automatic gas transmission mechanism is controlled to automatically output the gaseous elementary mercury to the detection analysis mechanism, the detection analysis mechanism is used for measuring the gaseous elementary mercury to obtain the total mercury concentration of the sample gas to be detected, the gaseous total mercury in the sample gas to be detected can be completely collected, the accuracy of analyzing the total mercury concentration of the sample gas to be detected is improved, therefore, the measurement of the total mercury content of the gas in the sample is truly realized, a simple and reliable online analysis technology is realized, and the analysis cost is reduced.
(2) Technical scheme
In a first aspect, an embodiment of the present invention provides an automatic analysis apparatus for analyzing total mercury in a gaseous state, including an automatic gas inlet mechanism, provided with a first pipeline for conveying a sample gas to be detected; the condensation and cracking mechanism is used for receiving the sample gas to be detected, enriching the gaseous total mercury in the sample gas to be detected at a low temperature, and resolving all the gaseous total mercury into gaseous elementary mercury at a high temperature; the automatic gas transmission mechanism is provided with a second pipeline for transmitting the gaseous elementary mercury; the detection and analysis mechanism is used for analyzing the total concentration of the gaseous elementary mercury, and the controller is used for controlling the automatic operation of the automatic gas inlet mechanism, the condensation and cracking mechanism and the automatic gas transmission mechanism.
Further, the condensation and cracking mechanism comprises a container which is communicated with the first pipeline and the second pipeline and is used for enriching the gaseous total mercury in the sample gas to be detected, a condensation unit which is used for condensing the gaseous total mercury in the container at a low temperature and a cracking unit which is used for analyzing the gaseous total mercury in the container at a high temperature into the gaseous elementary mercury.
Further, the condensing unit is including being used for holding the condensate tank of container and through filling pipe and return line all with the condensing agent storage tank of condensate tank intercommunication, be equipped with the liquid pump on the filling pipe, be equipped with the stop valve on the return line, still be equipped with in the condensate tank and be used for detecting liquid level's level sensor and be used for detecting the thermometer of temperature in the condensate tank with be used for maintaining the temperature controller under the setting temperature in the condensate tank.
Further, the cracking unit includes a first heating wire wound on an outer wall of the container.
Furthermore, the container is filled with an enriching agent for enriching the gaseous total mercury in the sample gas to be detected, the output end of the first pipeline and the input end of the second pipeline are both arranged inside the container, the output end of the first pipeline is embedded in the enriching agent, and the input end of the second pipeline is positioned above the enriching agent.
Furthermore, the automatic air inlet mechanism further comprises a first electromagnetic valve and a second electromagnetic valve which are arranged on the first pipeline and are communicated with each other, the first electromagnetic valve is provided with a first pipeline interface used for inputting sample gas to be detected and a second pipeline interface used for being communicated with the second electromagnetic valve, and the second electromagnetic valve is further provided with a third pipeline interface used for inputting carrier gas, a fourth pipeline interface communicated with the first electromagnetic valve and a fifth pipeline interface communicated with the container.
Furthermore, a sixth pipe interface for conveying mercury standard gas and a seventh pipe interface for conveying mercury-free air are arranged on the first electromagnetic valve.
Further, the automatic gas inlet mechanism further comprises a gas pump for pumping the sample gas to be detected from the first pipeline to the second pipeline, the automatic gas transmission mechanism comprises a mass flow controller, a third electromagnetic valve, a drying pipe, a fourth electromagnetic valve, an enrichment assembly and a fifth electromagnetic valve, the mass flow controller is arranged on the second pipeline and communicated with the drying pipe and used for controlling the flow rate of carrier gas, the drying pipe is used for drying the gaseous elemental mercury, the enrichment assembly is used for secondarily purifying the gaseous elemental mercury, the fifth electromagnetic valve is arranged between the mass flow controller and the drying pipe, the fourth electromagnetic valve is arranged between the drying pipe and the enrichment assembly, the fifth electromagnetic valve is arranged between the enrichment assembly and the detection and analysis mechanism, and an eighth pipe interface is arranged on the third electromagnetic valve and used for being communicated with the gas pump.
Furthermore, a ninth pipe interface for inputting carrier gas is arranged on the fourth electromagnetic valve, and a tenth pipe interface for discharging waste gas and an eleventh pipe interface communicated with the detection and analysis mechanism are arranged on the fifth electromagnetic valve.
Further, the enrichment subassembly includes mercury enrichment pipe and around locating the outside second heater strip of mercury enrichment pipe, still be equipped with on the third solenoid valve and be used for the intercommunication twelfth pipe interface and the intercommunication of mass flow controller the thirteenth pipe interface of drying tube, still be equipped with on the fourth solenoid valve and be used for the intercommunication the fourteenth pipe interface of drying tube other end and be used for the intercommunication the fifteenth pipe interface of mercury enrichment pipe, still be equipped with on the fifth solenoid valve and be used for the intercommunication the sixteenth pipe interface of mercury enrichment pipe other end.
(3) Advantageous effects
In conclusion, the controller controls the automatic gas inlet mechanism to automatically input the sample gas to be detected, controls the condensation and cracking mechanism to automatically realize low-temperature enrichment and high-temperature analysis of the total gaseous mercury in the sample gas to be detected step by step to obtain all gaseous elementary mercury, controls the automatic gas conveying mechanism to automatically output the gaseous elementary mercury to the detection and analysis mechanism, measures the gaseous elementary mercury by using the detection and analysis mechanism to obtain the total mercury concentration of the sample gas to be detected, can realize complete collection of various forms of mercury (containing gaseous elementary mercury, active gaseous mercury and granular mercury) in the sample gas to be detected, improves the accuracy of analysis of the total mercury concentration of the sample gas to be detected, thereby truly realizing the measurement of all the total mercury content of the gas in the sample, simultaneously realizing simple and reliable online analysis technology, and being more suitable for long-term online monitoring, and the maintenance is simple, the whole detection and analysis process does not need to adopt the prior art to regularly replace a filter membrane to filter sample gas, and does not need a chemical reagent to enrich a sample, thereby reducing the detection and analysis cost.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic structural view of the present invention.
In the figure:
1-a first pipeline; 11-a first solenoid valve; 12-a second solenoid valve; 111-a first tubing interface; 112-a sixth pipe interface; 113-a seventh pipe interface; 114-a second tubing interface; 121-a third tube interface; 122-a fourth tube interface; 123-fifth pipe interface
2-a second pipeline; 21-mass flow controllers; 22-a third solenoid valve; 23-a fourth solenoid valve; 25-a drying tube; 26-an enrichment module; 27-a suction pump; 221-twelfth tube interface; 222-a thirteenth tubing interface; 223-eighth pipe interface; 231-ninth pipe interface; 232-fourteenth pipe interface; 233-a fifteenth pipe interface; 241-tenth pipe interface; 242-sixteenth tube interface; 243-eleventh pipe interface; 261-a mercury enrichment tube; 262-a second heating wire;
3-a container; 31-an enriching agent;
41-a condensation tank; 42-an injection line; 43-return line; 44-a condensate storage tank; 45-liquid pump; 46-a shut-off valve; 47-thermometer; 48-temperature controller; 49-a first heating wire;
5-mercury analyzer.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the utility model and are not intended to limit the scope of the utility model, i.e., the utility model is not limited to the embodiments described, but covers any modifications, alterations, and improvements in the parts, components, and connections without departing from the spirit of the utility model.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Fig. 1 is a schematic structural diagram of an automatic analysis device for analyzing total mercury in a gaseous state according to an embodiment of the present invention, and as shown in fig. 1, the automatic analysis device includes an automatic gas inlet mechanism having a first pipeline 1 for conveying a sample gas to be detected; the condensation and cracking mechanism is used for receiving the sample gas to be detected, enriching the gaseous total mercury in the sample gas to be detected at a low temperature and resolving all the gaseous total mercury into gaseous elementary mercury at a high temperature; the automatic gas transmission mechanism is provided with a second pipeline 2 for transmitting gaseous elementary mercury; the detection and analysis mechanism is used for analyzing the total concentration of the gaseous elementary mercury; and the controller is used for controlling the automatic operation of the automatic air inlet mechanism, the condensation and cracking mechanism and the automatic air conveying mechanism.
The utility model controls the automatic input of the automatic gas inlet mechanism to the sample gas to be detected through the controller, controls the condensation and cracking mechanism to automatically realize low-temperature enrichment and high-temperature analysis of the gaseous total mercury in the sample gas to be detected step by step to obtain all gaseous elementary mercury, the automatic gas transmission mechanism is controlled to automatically output the gaseous elementary mercury to the detection analysis mechanism, the detection analysis mechanism is used for measuring the gaseous elementary mercury to obtain the total mercury concentration of the sample gas to be detected, the complete collection of all forms of mercury in the gaseous total mercury (containing gaseous elementary mercury, active gaseous mercury and granular mercury) in the sample gas to be detected can be realized, the accuracy of the analysis of the total mercury concentration of the sample gas to be detected is improved, therefore, the measurement of the total mercury content of the gas in the sample is truly realized, a simple and reliable online analysis technology is realized, and the analysis cost is reduced.
As a preferred embodiment, as shown in fig. 1, the condensation and cracking mechanism includes a container 3 communicating with a first pipeline 1 and a second pipeline 2 and used for enriching gaseous total mercury in a sample gas to be detected, a condensation unit used for condensing gaseous total mercury in the container 3 at a low temperature, and a cracking unit used for resolving gaseous total mercury in the container 3 at a high temperature into gaseous elemental mercury, an enriching agent 31 used for enriching gaseous total mercury in the sample gas to be detected is filled inside the container 3, the enriching agent can be quartz sand or silicon carbide particles and a combination of the two, an output end of the first pipeline 1 is embedded in the enriching agent 31, and an input end of the second pipeline 2 is located above the enriching agent 31. By utilizing the characteristic of the melting point of mercury, the enrichment of various forms of gaseous mercury (containing gaseous elementary mercury, active gaseous mercury and granular mercury) in the sample gas to be detected input in the container 3 is realized by carrying out low-temperature treatment on the container 3, the gaseous total mercury in the sample to be detected is not required to be filtered by a Teflon filter membrane, so that the granular mercury in a large granular state is removed to influence the accuracy of the total mercury concentration analysis, the container 3 is heated to raise the temperature, the gaseous total mercury enriched on the enriching agent 31 can be re-volatilized to form gaseous elementary mercury, carrier gas (high-purity nitrogen gas) is injected into a third pipe interface 121 of a second electromagnetic valve 12 (detailed later) to convey the gaseous elementary mercury from the container 3 into a detection analysis mechanism, and the purification of the gaseous total mercury in the sample gas to be detected is realized.
As another preferred embodiment, as shown in fig. 1, the condensing unit includes a condensing tank 41 for accommodating the container 3 and a refrigerant storage tank 44 communicated with the condensing tank 41 through both an injection line 42 and a return line 43, the condensing agent storage tank 44 is filled with condensing agent (methanol or glycol hydrate or mixture of methanol and glycol hydrate), the injection pipeline 42 is provided with a liquid pump 45, the return pipeline 43 is provided with a stop valve 46, the condensing tank 41 is also provided with a liquid level sensor (not shown) for detecting the liquid level height, a thermometer 47 for detecting the temperature in the condensing tank 41 and a temperature controller 48 for maintaining the temperature in the condensing tank 41 at a set temperature (preferably-50 ℃ and lower than the melting point of mercury), the cracking unit comprises a first heating wire 49 wound on the outer wall of the container 3, and the output end of the first pipeline 1 and the input end of the second pipeline 2 are both arranged inside the container 3. By the mutual matching of the liquid pump 45 and the stop valve 46, the condensing agent in the condensing agent storage tank 44 is pumped into the condensing tank 41 from the condensing agent storage tank 44 through the injection pipeline 42 when the container 3 needs to be subjected to low-temperature treatment, and the stop valve 46 is opened to re-flow the condensing agent in the condensing tank 41 into the condensing agent storage tank 44 through the return pipeline 43 during high-temperature analysis treatment, so that the automatic conveying and backflow of the condensing agent can be realized; the rising liquid level of the condensate in the condensation tank 41 is detected by a liquid level sensor, and when the liquid level of the condensate is slightly higher than the height of the enriching agent 31 in the container 3, the liquid pump 45 is controlled to stop injecting the condensate into the condensation tank 41, so that the condensate is prevented from overflowing due to excessive injection, and the cost of low-temperature treatment on the condensate is increased; the temperature of the condensing agent in the condensing tank 41 is cooled to a preset temperature value (50 ℃ below zero) by using the temperature controller 48, so that the gaseous mercury in various forms of the sample gas to be detected in the container 3 can be effectively ensured to be fully condensed at low temperature, and the comprehensive collection of mercury elements is improved; by using the real-time monitoring of the thermometer 47, the temperature controller 48 can maintain the temperature of the condensing agent in the condensing tank 41 at a preset temperature value in a dynamic balance manner, thereby ensuring the condensing effect on the gaseous mercury in various forms of the sample gas to be detected in the container 3.
As another preferred embodiment, as shown in fig. 1, the automatic air intake mechanism further includes a first electromagnetic valve 11 and a second electromagnetic valve 12 which are disposed on the first pipeline 1 and are communicated with each other, the first electromagnetic valve 11 is provided with a first pipe interface 111 for inputting a sample gas to be measured and a second pipe interface 114 for communicating with the second electromagnetic valve 12, and the second electromagnetic valve 12 is further provided with a third pipe interface 121 for inputting a carrier gas, a fourth pipe interface 122 for communicating with the first electromagnetic valve 11, and a fifth pipe interface 123 for communicating with the container 3. The controller controls the first tube interface 111, the second tube interface 114, the fourth tube interface 122, the fifth tube interface 123 to open and the third tube interface 121 to close, so that the sample gas to be detected can be automatically conveyed into the container 3, and controls the first tube interface 111, the fourth tube interface 122 to close and the third tube interface 121, the fifth tube interface 123 to open, so that the carrier gas (high-purity nitrogen) is injected into the container 3, and the gaseous elemental mercury after high-temperature analysis or high-temperature cracking is discharged from the container 3 into the second tube 2. It should be noted that, the opening and closing of the first pipe joint, the second pipe joint, the third pipe joint, the fourth pipe joint and the fifth pipe joint are controlled, and actually, the opening and closing of a corresponding valve (not shown in the drawings) arranged on a corresponding electromagnetic valve in each of the pipe joints are controlled, and the opening and closing of each pipe joint described in this application refers to the opening and closing of a corresponding valve on a corresponding electromagnetic valve, which is not described in detail later.
As other alternative embodiments.
Preferably, as shown in fig. 1, the first solenoid valve 11 is further provided with a sixth pipe interface 112 for delivering the mercury standard gas and a seventh pipe interface 113 for delivering the mercury-free air. Through arranging the sixth pipe interface 112 for conveying the mercury standard gas and the seventh pipe interface 113 for conveying the mercury-free air on the first electromagnetic valve 11, the mercury-free air can be introduced into the first pipeline 1, the container 3 and the second pipeline 2 until the total mercury concentration value measured by the detection and analysis mechanism is zero before the total mercury concentration measurement and analysis of the sample gas to be detected is performed, so as to prevent the gaseous mercury remaining in the whole analysis device from influencing the accuracy of the total mercury concentration during the normal measurement or the next measurement, on the other hand, the mercury standard gas can be introduced into the first pipeline 1, the container 3 and the second pipeline 2 before the total mercury concentration measurement and analysis of the sample gas to be detected, so as to calibrate and calibrate the total mercury concentration of the whole analysis device, thereby accurately detecting the recovery rate of the sample gas to be detected (that when the difference degree between the total mercury concentration value of the sample gas to be detected and the total mercury concentration value of the mercury standard gas is detected, can be used as a reference basis for recovering the sample gas to be detected).
Preferably, as shown in fig. 1, the automatic gas transmission mechanism is disposed on the second pipeline 2 and is communicated with the mass flow controller 21 for controlling the flow rate of the carrier gas, the third electromagnetic valve 22, the drying pipe 25 for drying the gaseous elemental mercury, the fourth electromagnetic valve 23, the enrichment assembly 26 for secondarily purifying the gaseous elemental mercury, and the fifth electromagnetic valve 24, the third electromagnetic valve 22 is disposed between the mass flow controller 21 and the drying pipe 25, the fourth electromagnetic valve 23 is disposed between the drying pipe 25 and the enrichment assembly 26, the fifth electromagnetic valve 24 is disposed between the enrichment assembly 26 and the detection and analysis mechanism, the automatic gas transmission mechanism further includes a suction pump 27 for sucking the sample gas to be detected from the first pipeline 1 into the second pipeline 2, and the third electromagnetic valve 22 is provided with an eighth pipe interface 223 for communicating with the suction pump 27. The mass flow controller 21 monitors the flow of the sample gas to be detected extracted by the air extracting pump 27 in real time to automatically adjust the air inlet flow of the sample gas to be detected, so that waste caused by incapability of rapid condensation of the sample gas to be detected due to overlarge air inlet flow or influence on automatic analysis efficiency due to long air inlet time caused by undersize air inlet flow are prevented, and the total flow of the sample gas to be detected passing through the mass flow controller is recorded; the drying agent such as soda lime and the like used for adsorbing the moisture and other impurity gases mixed in the gaseous elementary mercury is arranged in the drying pipe, so that the inaccurate influence of the moisture and other impurity gases on the measurement result of the detection and analysis mechanism is avoided; through set up mercury enrichment pipe between fourth solenoid valve and fifth solenoid valve and be used for carrying out the secondary purification to gaseous state simple substance mercury after getting rid of aqueous vapor and other foreign gas, it is higher to ensure to get into the purity of gaseous state simple substance mercury among the detection and analysis mechanism for measuring result is more accurate.
Preferably, as shown in fig. 1, the fourth solenoid valve 23 is provided with a ninth pipe interface 231 for inputting carrier gas, the fifth solenoid valve 24 is provided with a tenth pipe interface 241 for discharging exhaust gas (moisture and other impurity gas except high purity nitrogen gas) and an eleventh pipe interface 243 communicated with the detection and analysis mechanism, the enrichment assembly 26 includes a mercury-rich tube 261 and a second heating wire 262 wound around the exterior of the mercury-rich tube 261, the third solenoid valve 22 is further provided with a twelfth pipe joint 221 for communicating with the mass flow controller 21 and a thirteenth pipe joint 222 for communicating with the drying pipe 25, the fourth solenoid valve 23 is further provided with a fourteenth pipe port 232 for communicating the other end of the drying pipe 25 and a fifteenth pipe port 233 for communicating the mercury-rich pipe 261, the fifth solenoid valve 24 is further provided with a sixteenth pipe interface 242 for communicating the other end of the mercury-rich pipe 261. By controlling to close the fourteenth pipe interface 232 and the eleventh pipe interface 243 and open the ninth pipe interface 231, the fifteenth pipe interface 233, the sixteenth pipe interface 242, and the tenth pipe interface 241, the purity of the gaseous elemental mercury to be measured can be improved and the accuracy of the measurement result can be ensured when the gaseous elemental mercury from which moisture and other impurity gases have been removed is subjected to secondary enrichment.
Preferably, as shown in fig. 1, the detection and analysis mechanism is a mercury analyzer 5, and the mercury analyzer 5 may be an atomic fluorescence or atomic absorption mercury detector.
To further understand the inventive step of the present invention, the operation principle of the present invention is described as follows, and as shown in fig. 1, the automatic analysis process implemented by the automatic analysis apparatus for analyzing total mercury in gaseous state of the present invention includes a first control phase (a phase of injecting the condensing agent into the condensation tank and maintaining a preset temperature), i.e., the controller controls the liquid pump 45 to open, and simultaneously closes the stop valve 46, the liquid pump 45 pumps the condensing agent in the condensing agent storage tank 44 into the condensation tank 41 until the liquid level sensor detects that the liquid level of the condensing agent in the condensation tank 41 reaches a preset position (i.e., slightly higher than the height of the enriching agent 31 formed in the container 3), and closes the liquid pump 45 and simultaneously opens the temperature controller 48 to cool the condensing agent in the condensation tank 41 and maintain the preset temperature (i.e., 50 ℃ below zero); a second control stage (automatic gas inlet and condensation enrichment stage), namely, opening the first tube interface 111, the second tube interface 114, the fourth tube interface 122, the fifth tube interface 123, the twelfth tube interface 221, the eighth tube interface 223, closing the sixth tube interface 112, the seventh tube interface 113, the third tube interface 121, and the thirteenth tube interface 222, and simultaneously starting the air pump 27 and the mass flow controller 21, so that various forms of mercury (including gaseous elemental mercury, active gaseous mercury, and particulate mercury) in the sample gas to be measured are enriched by the enrichment agent 31 condensed at low temperature while flowing through the container 3, and the mass flow controller 21 records the flow rate of the sample gas to be measured, and the preset sampling time or sampling volume is taken as a control signal for completing the enrichment); a third control stage (high temperature analysis and gas transmission detection stage), namely closing the air pump 27 and the fourth interface 122, opening the stop valve 46 to automatically flow the condensing agent in the condensing tank 41 into the condensing agent storage tank 44 through the return pipeline 43, adjusting the temperature controller 48 to heat the first heating wire 49 to a preset high temperature (900 ℃), analyzing all the mercury in the enriching agent 31 into gaseous elemental mercury, closing the sixth pipe interface 112, the eighth pipe interface 223, the ninth pipe interface 231 and the eleventh pipe interface 243, opening the third pipe interface 121, the thirteenth pipe interface 222, the fourteenth pipe interface 232, the fifteenth pipe interface 233, the sixteenth pipe interface 242 and the tenth pipe interface 241, and taking the analyzed gaseous elemental mercury out from the container 3 by the carrier gas (high purity nitrogen or argon) introduced from the third pipe interface 121 and sequentially passing through the twelfth pipe interface 221, the fifteenth pipe interface 221, the eleventh pipe interface 221, the thirteenth pipe interface 221, the eleventh pipe interface 241, The thirteenth pipe interface 222, the drying pipe 25 (for removing water gas and other impurity gases entrained in the gaseous elemental mercury), the fourteenth pipe interface 232 and the fifteenth pipe interface 233 enter the mercury enrichment pipe 261 (made of pure gold, quartz gold-plated, silicon carbide or activated carbon and other materials) to perform secondary purification and enrichment on the gaseous elemental mercury, simultaneously the formed exhaust gas (high-purity nitrogen and other impurity gases) sequentially passes through the sixteenth pipe interface 242 and the tenth pipe interface 241 and then is discharged to the external atmosphere until the enrichment process is completed (the enrichment time is controlled for 30-60 minutes, for example, by a timer), then the fourteenth pipe interface 232 and the tenth pipe interface 241 are controlled to be closed, the ninth pipe interface 231 and the eleventh pipe interface 243 are opened at the same time, and the second heating wire 262 is started to heat up to 500-600 ℃ to re-resolve the mercury elements enriched in the mercury enrichment pipe into gaseous elemental mercury, and injecting carrier gas (high-purity nitrogen or argon) into the ninth pipe interface 231, allowing the gaseous elementary mercury obtained by secondary analysis to sequentially pass through the sixteenth pipe interface 242 and the eleventh pipe interface 243 to enter the mercury detector or mercury analyzer 5, and calculating the total mercury concentration in the sample gas to be detected through the measured mercury content and the total flow or sampling volume of the sample gas to be detected recorded by the mass flow controller 21.
For injecting the mercury standard gas and the mercury-free air, the first pipe interface 111 is only required to be switched to the corresponding sixth pipe interface 112 or seventh pipe interface 113 in the second control stage, and the rest steps are the same as the analysis and measurement process of the sample gas to be measured, and are not described herein again.
It should be clear that the embodiments in this specification are described in a progressive manner, and the same or similar parts in the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. The present invention is not limited to the specific steps and structures described above and shown in the drawings. Also, a detailed description of known process techniques is omitted herein for the sake of brevity.
The above description is only an example of the present application and is not limited to the present application. Various modifications and alterations to this application will become apparent to those skilled in the art without departing from the scope of this invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.

Claims (10)

1. An automatic analysis device for analyzing gaseous total mercury, comprising: the automatic air inlet mechanism is provided with a first pipeline (1) for conveying gas of a sample to be detected;
the condensation and cracking mechanism is used for receiving the sample gas to be detected, enriching the gaseous total mercury in the sample gas to be detected at a low temperature, and resolving all the gaseous total mercury into gaseous elementary mercury at a high temperature;
the automatic gas transmission mechanism is provided with a second pipeline (2) for transmitting the gaseous elementary substance mercury; the detection analysis mechanism is used for analyzing the total concentration of the gaseous elementary mercury;
and the controller is used for controlling the automatic air inlet mechanism, the condensation and cracking mechanism and the automatic air conveying mechanism to automatically operate.
2. The automatic analysis device for analyzing gaseous total mercury according to claim 1, characterized in that the condensation and cracking mechanism comprises a container (3) communicating with the first pipeline (1) and the second pipeline (2) for enriching the gaseous total mercury in the sample gas to be tested, a condensation unit for low-temperature condensation of the gaseous total mercury in the container (3), and a cracking unit for high-temperature resolution of the gaseous total mercury in the container (3) into the gaseous elemental mercury.
3. The automatic analyzing apparatus for analyzing gaseous total mercury according to claim 2, wherein the condensing unit comprises a condensing tank (41) for accommodating the container (3) and a condensing agent storage tank (44) communicated with the condensing tank (41) through a filling line (42) and a return line (43), the filling line (42) is provided with a liquid pump (45), the return line (43) is provided with a stop valve (46), the condensing tank (41) is further provided with a liquid level sensor for detecting a liquid level and a thermometer (47) for detecting a temperature in the condensing tank (41) and a temperature controller (48) for maintaining a set temperature in the condensing tank (41).
4. The automatic analysis device for analyzing gaseous total mercury according to claim 2, characterized in that the cracking unit comprises a first heating wire (49) wound on the outer wall of the container (3).
5. The automatic analysis device for analyzing total mercury gaseous according to claim 2, characterized in that the container (3) is filled with an enrichment agent (31) for enriching total mercury gaseous in a sample gas to be tested, the output end of the first pipeline (1) and the input end of the second pipeline (2) are both arranged inside the container (3), and the output end of the first pipeline (1) is embedded in the enrichment agent (31), and the input end of the second pipeline (2) is located above the enrichment agent (31).
6. The automatic analysis device for analyzing total mercury vapor according to claim 2, characterized in that the automatic gas inlet mechanism further comprises a first solenoid valve (11) and a second solenoid valve (12) which are arranged on the first pipeline (1) and are communicated with each other, the first solenoid valve (11) is provided with a first pipe interface (111) for inputting a sample gas to be tested and a second pipe interface (114) for communicating with the second solenoid valve (12), and the second solenoid valve (12) is further provided with a third pipe interface (121) for inputting a carrier gas, a fourth pipe interface (122) for communicating with the first solenoid valve (11), and a fifth pipe interface (123) for communicating with the container (3).
7. The automatic analysis device for analyzing total mercury in the gaseous state according to claim 6, characterized in that the first solenoid valve (11) is further provided with a sixth pipe interface (112) for delivering mercury standard gas and a seventh pipe interface (113) for delivering mercury-free air.
8. The automatic analysis device for analyzing gaseous total mercury according to claim 6, characterized in that the automatic gas inlet mechanism further comprises a suction pump (27) for pumping the sample gas to be tested from the first pipeline (1) into the second pipeline (2), the automatic gas delivery mechanism comprises a mass flow controller (21) for controlling the flow rate of the carrier gas, a third electromagnetic valve (22), a drying pipe (25) for drying the gaseous elemental mercury, a fourth electromagnetic valve (23), an enrichment assembly (26) for secondarily purifying the gaseous elemental mercury, and a fifth electromagnetic valve (24) which are arranged on the second pipeline (2) and are communicated with each other, the third electromagnetic valve (22) is arranged between the mass flow controller (21) and the drying pipe (25), and the fourth electromagnetic valve (23) is arranged between the drying pipe (25) and the enrichment assembly (26), the fifth electromagnetic valve (24) is arranged between the enrichment assembly (26) and the detection and analysis mechanism, and an eighth pipe interface (223) used for being communicated with the air suction pump (27) is arranged on the third electromagnetic valve (22).
9. The automatic analyzing device for analyzing gaseous total mercury according to claim 8, wherein a ninth pipe interface (231) for inputting carrier gas is provided on the fourth solenoid valve (23), and a tenth pipe interface (241) for discharging exhaust gas and an eleventh pipe interface (243) communicating with the detection and analysis mechanism are provided on the fifth solenoid valve (24).
10. The automatic analysis device for analyzing gaseous total mercury according to claim 9, wherein the enrichment assembly (26) comprises a mercury-rich pipe (261) and a second heating wire (262) wound outside the mercury-rich pipe (261), a twelfth pipe joint (221) for communicating the mass flow controller (21) and a thirteenth pipe joint (222) for communicating the drying pipe (25) are further provided on the third solenoid valve (22), a fourteenth pipe joint (232) for communicating the other end of the drying pipe (25) and a fifteenth pipe joint (233) for communicating the mercury-rich pipe (261) are further provided on the fourth solenoid valve (23), and a sixteenth pipe joint (242) for communicating the other end of the mercury-rich pipe (261) is further provided on the fifth solenoid valve (24).
CN202122704680.3U 2021-11-05 2021-11-05 Automatic analysis device for analyzing gaseous total mercury Active CN216525760U (en)

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