CN213091574U - Mercury content measurement device based on direct sampling method - Google Patents
Mercury content measurement device based on direct sampling method Download PDFInfo
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- CN213091574U CN213091574U CN202022160971.6U CN202022160971U CN213091574U CN 213091574 U CN213091574 U CN 213091574U CN 202022160971 U CN202022160971 U CN 202022160971U CN 213091574 U CN213091574 U CN 213091574U
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Abstract
The application relates to the field of elemental analysis instruments, specifically discloses a mercury assay device based on direct sampling method for mercury content in survey detection object includes: a combustion module which combusts the detection object to cause thermal decomposition and catalytic reaction; the leveling module is connected with the combustion module to enable the elemental mercury generated by combustion to generate gold amalgam; the detection module is connected with the alignment module and used for detecting the content of the elemental mercury released by the alignment module after the temperature is raised. The method for directly feeding the solid sample is adopted for measuring the mercury content, atomization of mercury is realized through thermal decomposition and catalytic reaction, experimental errors and health hazards caused by improper pretreatment in the existing measuring method are avoided, measuring time is greatly shortened through the method for directly feeding the sample, and detection efficiency is improved.
Description
Technical Field
The application relates to the field of elemental analysis instruments, in particular to a mercury content measuring device based on a direct sample introduction method.
Background
The method for measuring the mercury content in a solid sample mainly comprises analysis methods such as cold atomic absorption spectrometry (CVAAS), inductively coupled plasma mass spectrometry (I CP-MS) and Atomic Fluorescence Spectrometry (AFS) solid sample introduction mercury measurement. At present, the mercury content in a solid sample is measured by an atomic fluorescence spectrometry method commonly used in laboratories, and the principle is that after a sample is heated and digested by acid, mercury in the sample is reduced into atomic mercury by potassium borohydride or sodium borohydride in an acidic medium, the atomic mercury is carried into an atomizer by carrier gas, ground-state mercury atoms are excited to a high-energy state under the irradiation of a mercury hollow cathode lamp, fluorescence with characteristic wavelength is emitted when the ground state is returned from the high-energy state, and the fluorescence intensity is proportional to the mercury content, so that the mercury content is measured. However, the method needs wet pretreatment of the solid sample, so that mercury elements in the sample are completely converted into digestion solution, and then the on-machine test is carried out. The operation flow of the process is long, and the operation is complicated. In addition, in the pretreatment process of the sample, due to the volatile characteristic of mercury, the accuracy of the measurement result and the physical health of experimenters are easily affected, and certain harm is caused.
SUMMERY OF THE UTILITY MODEL
In order to solve the problems of long operation process, complicated treatment and the like in the process of measuring the mercury content in the prior art, the method aims at measuring the mercury, combines an element analysis principle and an atomic fluorescence spectrometry principle, directly samples a measuring sample for measurement, removes a preposed processing flow of measurement through the structural arrangement of measuring equipment, and greatly reduces the measuring time.
In order to achieve the purpose, the technical scheme adopted by the application is as follows:
a mercury content measuring device based on a direct injection method is used for measuring the mercury content in a detection object and comprises the following components: a combustion module which combusts the detection object to cause thermal decomposition and catalytic reaction; the leveling module is connected with the combustion module to enable the elemental mercury generated by combustion to generate gold amalgam; the detection module is connected with the alignment module and used for detecting the content of the elemental mercury released by the alignment module after the temperature is raised.
The working principle of the existing element analyzer is that a sample is placed in a combustion device, and under the action of high-purity oxygen, catalytic oxidant and high temperature, the sample is decomposed and converted into H2O、N2、NOX、SO2、SO3After the gas product is generated, the mixed gas is carried into the reduction tube by high-purity helium gas as carrier gas, and NO is generated under the action of the reduction copper filled in the reduction tubeX、SO3Is reduced to N2、SO2While excess oxygen is removed. CO 22、H2O、SO2The gas products are respectively adsorbed on a special adsorption column after being taken out of the reduction tube by helium, and N is2It is first detected by helium brought directly into the Thermal Conductivity Detector (TCD). Then, the temperature of the adsorption-desorption column is sequentially raised according to the program to make CO2、H2O、SO2After desorption, the mixture enters a thermal conductivity detector in sequence for detection.
The principle of the element analyzer is utilized and improved, the detection object is processed in a direct sample introduction mode to obtain the elemental mercury, and therefore the elemental mercury is detected by utilizing atomic fluorescence spectrometry equipment. Specifically, in order to improve detection device's pertinence in this application to the improvement is to the precision degree that mercury content detected in the detection object, adopts combustion module and amalgamation module to accomplish the preprocess to the detection object jointly in this scheme. The combustion module controls the temperature and the combustion condition to enable the detection object to generate thermal decomposition and catalytic reaction, so that elemental mercury existing in the form of steam is obtained. At this time, burnCO is also included in the burned product2、SO2And/or SO3And other substances, in order to reduce the interference of other combustion products to a subsequent detection module and improve the detection sensitivity, an alignment module is arranged in the combustion module and the detection module, and the principle is as follows: by utilizing the special property that gold can be dissolved in mercury, mercury vapor generated by combustion meets gold to form gold amalgam in the homogenization module, and other combustion products are directly discharged, so that low-concentration mercury vapor generated by combustion is captured and enriched in the homogenization module, and when the detection module is required to operate to detect the mercury content, the homogenization module is instantly heated to intensively release the enriched mercury vapor and input the concentrated mercury vapor into the detection module, so that the detection module only detects high-concentration elemental mercury vapor, and a more accurate detection result is obtained.
It is worth to be noted that, compared with the conventional atomic fluorescence spectrum detection method which needs wet pretreatment on the detection object, the detection time is as long as 5 hours, the method adopts the detection method combining direct sample injection and atomic fluorescence spectrum to shorten the detection time to less than 10 minutes, and the detection time is greatly shortened.
Furthermore, the combustion module is connected with the leveling module through a temperature control connecting mechanism, and the temperature control connecting mechanism has a temperature control range of 0-360 ℃.
The utility model discloses a set up the coupling mechanism between burning module and the neat module into accuse temperature coupling mechanism, accuse temperature coupling mechanism control combustion products from burning module entering neat module in-process temperature to guarantee that the mercury vapour that the burning formed keeps the gaseous state, further reduce the loss of mercury and avoid the pipeline pollution.
Furthermore, the combustion module comprises a combustion tube for accommodating a burned object and a catalyst, and a combustion furnace for heating the combustion tube and the content thereof, wherein oxygen is introduced into the combustion tube during operation.
Furthermore, the combustion module is connected with a carrier gas pipe, and the carrier gas pipe introduces inert gas into the combustion pipe to load the mercury vapor after combustion into the leveling module.
Further, the combustion module comprises a sample tray for containing a plurality of detection objects and inputting the detection objects into the combustion tube one by one.
Furthermore, accuse temperature coupling mechanism includes the quartz connecting pipe, be equipped with the heat preservation outside the quartz connecting pipe, still including the temperature control module who is used for controlling the interior ambient temperature of quartz connecting pipe.
Furthermore, the temperature control module is connected with the leveling module and controls the temperature of the leveling module. The temperature control of the leveling module mainly comprises two stages, wherein in the stage of capturing the enriched mercury vapor, the state of the mercury vapor needs to be kept at a relatively low temperature, so that the volatilization of mercury caused by overhigh temperature is avoided; when the mercury content needs to be detected, the temperature needs to be rapidly increased to a higher temperature, so that the enriched mercury is completely restored to the state of the elemental mercury vapor and enters the detection module.
Further, the detection module is an atomic fluorescence spectrum detector. The mercury vapor is excited to a high energy state by radiant energy in an atomic fluorescence spectrum detector, and emits fluorescence of a characteristic wavelength when returning to a ground state from the high energy state, and the mercury content is determined by detecting the intensity of the fluorescence. Wherein the higher the mercury content, the higher the fluorescence intensity.
The beneficial effect of this application is:
(1) the method for directly feeding the solid sample is adopted for measuring the mercury content, atomization of mercury is realized through thermal decomposition and catalytic reaction, and experimental errors and health hazards caused by improper pretreatment in the conventional measuring method are avoided.
(2) The amalgam is arranged to enrich the slowly released mercury in the form of gold amalgam, then the mercury is resolved out by instant heating, and then quantitative determination is carried out by an atomic fluorescence spectrometer, and the detection sensitivity is improved by enrichment.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic structural diagram of the present application;
FIG. 2 is a schematic diagram of a prior art elemental analyzer;
in the figure: 1-sample tray; 2-a combustion tube; 3-a combustion furnace; 4-a catalyst; 5-insulating layer; 6-quartz connecting tube; 7-leveling module; 8-detection module.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are some embodiments of the present application, but not all embodiments. The components of the embodiments of the present application, generally described and illustrated in the figures herein, can be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present application, presented in the accompanying drawings, is not intended to limit the scope of the claimed application, but is merely representative of selected embodiments of the application. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present application, it should be noted that if the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. are used for indicating the orientation or positional relationship based on the orientation or positional relationship shown in the drawings or the orientation or positional relationship which is usually placed when the product of the application is used, the description is only for convenience and simplicity, and the indication or suggestion that the referred device or element must have a specific orientation, be constructed in a specific orientation and be operated, and thus, should not be construed as limiting the present application. Furthermore, the appearances of the terms "first," "second," and the like in the description herein are only used for distinguishing between similar elements and are not intended to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical" and the like when used in the description of the present application do not require that the components be absolutely horizontal or overhanging, but may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present application, it should also be noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," "connected," and "connected" should be interpreted broadly, e.g., as being fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present application can be understood in a specific case by those of ordinary skill in the art.
Example 1:
a mercury content measuring device based on a direct injection method as shown in fig. 1, for measuring the mercury content in a detection object, comprising: a combustion module which combusts the detection object to cause thermal decomposition and catalytic reaction; the leveling module 7 is connected with the combustion module to enable the elemental mercury generated by combustion to generate gold amalgam; and the detection module 8 is connected with the alignment module 7, and the content of the elemental mercury released after the temperature of the alignment module 7 is raised is detected.
The working principle is as follows:
the detection principle of the application refers to the adsorption-desorption principle adopted by the existing element analyzer, the schematic diagram of the test principle of the existing element analyzer is shown in fig. 2, a detected object is completely decomposed through high-temperature combustion, a generated gas mixture is effectively separated by a special adsorption-desorption device after interference substances are eliminated, and finally, all components are detected by the detection device.
Detected object is in burning moduleThe mercury in various forms is reduced into simple substance mercury under the action of high temperature and catalysis, and other substances in the detection object are also oxidized and reduced to generate CO2Or SO2And other combustion products. All combustion products enter the leveling module 7, only mercury vapor is captured and enriched in the leveling module 7, the mercury vapor meets gold in the leveling module 7 to generate gold amalgam by utilizing the principle that gold can be dissolved in mercury, and after the mercury vapor is enriched, the leveling module 7 is heated again to release the enriched mercury uniformly, so that the detection module 8 detects the mercury content.
It is worth mentioning that the leveling module 7 is arranged between the combustion module and the detection module 8 to enrich elemental mercury, so that the detection sensitivity can be improved besides the detection result can be prevented from being interfered by other combustion products. The principle is as follows: during actual detection, if the generated mercury vapor directly enters the detection module 8 to be detected, the atomic fluorescence detection has the trailing phenomenon or the steamed bun peak or even the situation that the detection cannot be performed due to the long thermal decomposition and catalytic reaction processes of the solid sample, while the leveling module 7 can quickly release the enriched mercury to form mercury vapor with relatively high concentration, so that the detection sensitivity is improved.
Example 2:
the present embodiment is further optimized and limited based on the above embodiments.
The combustion module is connected with the leveling module 7 through a temperature control connecting mechanism, and the temperature control connecting mechanism has a temperature control range of 0-360 ℃. The temperature control connecting mechanism comprises a quartz connecting pipe 6, a heat preservation layer 5 is arranged outside the quartz connecting pipe 6, and the temperature control connecting mechanism further comprises a temperature control module used for controlling the ambient temperature in the quartz connecting pipe 6.
The working principle is as follows:
the temperature control connecting mechanism is composed of a quartz connecting pipe 6, a heat insulating layer 5 wrapping the quartz connecting pipe 6 and a temperature control module controlling the temperature in the quartz connecting pipe 6. Vapor generated in the combustion module enters the leveling module 7 through the quartz connecting pipe 6, and the temperature control module is used for controlling the temperature in the mercury vapor conveying process, so that the vapor is kept in the form and enters the leveling module 7 to be conveniently captured by the leveling module 7. And the mercury vapor is not easy to adhere to the inner wall of the conveying pipeline in a high-temperature environment, so that the loss of mercury in the conveying process is effectively avoided, and the detection precision is improved.
Example 3:
on the basis of the above embodiments, the present embodiment further optimizes and defines the combustion module.
As shown, the combustion module includes a combustion tube 2 for accommodating a material to be combusted and a catalyst 4, and a combustion furnace 3 for heating the combustion tube 2 and its contents. The combustion tube 2 is connected with a gas carrying tube, and the gas carrying tube introduces inert gas into the combustion tube 2 to load the mercury vapor after combustion into the leveling module 7.
It is to be noted that, when the test object is burned in the combustion tube 2, oxygen needs to be introduced into the combustion tube 2 so that the test object can be decomposed under high temperature conditions, the redox action of oxygen, and the catalytic action of the catalyst 4, thereby converting mercury in various states into mercury vapor. Simultaneously, this application adopts inert gas to drive the mercury vapour in burning tube 2 as the carrier gas and to the module 7 of making an uproar in, can effectively avoid producing other chemical reaction and influence the testing result. Among them, helium and argon are preferable as the carrier gas.
Example 4:
in this embodiment, further optimization and limitation are performed on the basis of embodiment 2.
The temperature control connecting mechanism comprises a quartz connecting pipe 6, a heat preservation layer 5 is arranged outside the quartz connecting pipe 6, and the temperature control connecting mechanism further comprises a temperature control module used for controlling the ambient temperature in the quartz connecting pipe 6. The temperature control module is connected with the leveling module 7 and controls the temperature of the leveling module 7. In this embodiment, the combustion tube 2 and the leveling module 7 are connected by the quartz connection tube 6, and the mercury vapor enters the leveling module 7 through the quartz connection tube 6. The temperature control module is arranged to control the temperature in the quartz connecting pipe 6 to keep the mercury in a steam state, and the heat-insulating layer 5 is coated on the outer layer of the quartz connecting pipe 6 to avoid heat loss. Meanwhile, the temperature control module is also used for controlling the temperature of the leveling module 7. The temperature control of the leveling module 7 mainly comprises two stages, wherein in the stage of capturing the mercury-enriched vapor, the mercury needs to be kept in a relatively low-temperature state to avoid the volatilization of mercury caused by overhigh temperature; when the mercury content needs to be detected, the temperature needs to be rapidly increased to a higher temperature, so that the enriched mercury is completely restored to the state of the elemental mercury vapor and enters the detection module.
It should be noted that since the temperature of the leveling module 7 depends on the operating stage, the temperature control module needs to control the temperature of the quartz connecting tube 6 and the leveling module 7 in stages to make the two modules work in cooperation for better mercury vapor capture. During detection, about 240 seconds are needed from the beginning of combustion of a detection object to the complete enrichment in the homogenization module 7, during the period, the temperature control module needs to maintain the temperature of the quartz tube to enable mercury to maintain a vapor state, the temperature in the homogenization module 7 is controlled not to be too high to enrich mercury vapor, then, the homogenization module 7 needs to be rapidly heated within 20 seconds to release mercury vapor, and the temperature is reduced after the release is completed. The detection module 8 has a detection and reading time of 20-30 seconds at the time of detection.
Example 5:
the present embodiment is further optimized and limited based on the above embodiments.
As shown in fig. 1, in order to allow the test object to be more sufficiently thermally decomposed in the combustion tube having a limited volume, the combustion module includes a sample tray 1 for holding a plurality of test objects and inputting them one by one to a combustion tube 2. When the device is used, a detection object is divided and uniformly placed in the sample tray 1, and the sample tray 1 conveys the detection object to the combustion pipe 2 one by one in batches. In practice, in order to cooperate with the leveling module 7 and the detection module 8, after the first sample has completely completed the detection process, a second sample is introduced into the combustion tube 2. Preferably, a certain time interval may be set after the first sample is completely detected, and the second sample may be put into the combustion tube 2.
Example 6:
in this embodiment, based on the above embodiments, the detection module 8 is further optimized and defined.
The detection module 8 is an atomic fluorescence spectrum detector, mercury vapor is excited to a high energy state by radiant energy in the atomic fluorescence spectrum detector, and emits fluorescence with characteristic wavelength when returning to a ground state from the high energy state, and the mercury content is measured by detecting the intensity of the fluorescence. Wherein the higher the mercury content, the higher the fluorescence intensity.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (8)
1. The utility model provides a mercury content survey device based on direct injection method for survey mercury content in the detection object, its characterized in that: the method comprises the following steps:
a combustion module which combusts the detection object to cause thermal decomposition and catalytic reaction;
the amalgam module (7) is connected with the combustion module to enable the elemental mercury generated by combustion to generate gold amalgam;
and the detection module (8) is connected with the alignment module (7), and the content of the elemental mercury released after the temperature of the alignment module (7) is raised is detected.
2. The mercury content measuring device based on the direct injection method according to claim 1, characterized in that: the combustion module is connected with the leveling module (7) through a temperature control connecting mechanism, and the temperature control connecting mechanism has a temperature control range of 0-360 ℃.
3. The mercury content measuring device based on the direct injection method according to claim 1, characterized in that: the combustion module comprises a combustion tube (2) for accommodating a substance to be combusted and a catalyst (4), and a combustion furnace (3) for heating the combustion tube (2) and the content thereof.
4. The mercury content measuring device based on the direct injection method according to claim 3, characterized in that: the combustion tube (2) is connected with a gas carrying tube, and the gas carrying tube introduces inert gas into the combustion tube (2) to load the mercury vapor after combustion into the leveling module (7).
5. The mercury content measuring device based on the direct injection method according to claim 1, characterized in that: the combustion module comprises a sample plate (1) which is used for containing a plurality of detection objects and inputting the detection objects into a combustion tube (2) one by one.
6. The mercury content measuring device based on the direct injection method according to claim 2, characterized in that: the temperature control connecting mechanism comprises a quartz connecting pipe (6), wherein a heat insulation layer (5) is arranged outside the quartz connecting pipe (6), and the temperature control connecting mechanism further comprises a temperature control module for controlling the ambient temperature in the quartz connecting pipe (6).
7. The mercury content measuring device based on the direct injection method according to claim 6, characterized in that: the temperature control module is connected with the leveling module (7) and controls the temperature of the leveling module (7).
8. The mercury content measuring device based on the direct injection method according to any one of claims 1 to 7, wherein: the detection module (8) is an atomic fluorescence spectrum detector.
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