Morphological analysis device for mercury in mercury-containing polluted soil

Abstract

The utility model relates to the technical field of environmental science and soil pollution analysis, and discloses a form analysis device for mercury in mercury-containing polluted soil, which comprises a rack, a sample treatment mechanism, a mercury form extraction module and a detection module, the sample treatment mechanism comprises a feed port, a heating cavity and a discharge port, the feed port is communicated with the heating cavity through a feed channel, and the discharge port is communicated with the heating cavity through a discharge channel. A grinding roller is arranged in the feeding channel, a screening net is arranged between the feeding channel and the heating cavity, and a heating wire set is arranged in the heating cavity. Samples are processed through the sample processing mechanism, so that uniform and stable soil samples can be obtained, and the accuracy of mercury form analysis is improved; mercury in an acid exchange state, an iron-manganese oxidation state, an organic-sulfuration state and a residue state in the soil can be obtained through the mercury form extraction module, so that different forms of mercury in the soil can be comprehensively analyzed; and through a detection technology in the detection module, the content of mercury in various forms can be detected.

Description

Technical Field

[0001] This utility model relates to the field of environmental science and soil pollution analysis technology, and in particular to a device for analyzing the speciation of mercury in mercury-contaminated soil. Background Technology

[0002] Mercury is a highly toxic heavy metal, and its speciation in soil determines its mobility, bioavailability, and toxicity. Studies have shown that soil pH, organic matter content, moisture content, and temperature all affect the speciation of mercury. Traditional mercury speciation analysis methods primarily focus on total mercury content, neglecting the influence of different mercury speciations on toxicity. Therefore, developing a mercury speciation analysis device that can comprehensively consider these factors is of great significance. Utility Model Content

[0003] The present invention aims to improve at least one technical problem in the prior art.

[0004] This utility model provides a device for analyzing the speciation of mercury in mercury-contaminated soil, comprising:

[0005] frame;

[0006] A sample processing mechanism includes an inlet, a heating chamber, and an outlet. The heating chamber is mounted on a frame. The inlet is connected to the heating chamber via a feeding channel. A grinding roller is provided in the feeding channel. A sieve screen is provided between the feeding channel and the heating chamber. A heating wire assembly is provided in the heating chamber. The bottom of the heating chamber is concave, and the outlet is located at the lowest point of the bottom.

[0007] A mercury speciation extraction module is used to extract acid-exchangeable mercury, iron-manganese oxide mercury, organic-sulfide mercury and residual mercury from soil samples.

[0008] The detection module acquires the content of mercury in the extracted acid-exchange state, iron-manganese oxide state, organic-sulfide state, and residue state, respectively.

[0009] As a further improvement to the above technical solution, the screening mesh includes a first screening mesh and a second screening mesh, which are fitted together vertically. The first screening mesh is provided with a first push-pull rod, and the second screening mesh is provided with a second push-pull rod. The feeding channel is provided with a first clearance hole and a second clearance hole. The first push-pull rod passes through the first clearance hole, and the second push-pull rod passes through the second clearance hole. The first push-pull rod is provided with a first adjustment groove, and the second push-pull rod is provided with a second adjustment groove. The frame is provided with a first fixing hole and a second fixing hole. The sample processing mechanism further includes a first fixing nail and a second fixing nail. The first fixing nail passes through the first adjustment groove and is threadedly connected to the first fixing hole, and the second fixing nail passes through the first adjustment groove and is threadedly connected to the second fixing hole.

[0010] As a further improvement to the above technical solution, the heating chamber is hinged to the frame, and the heating chamber is connected to the frame by a tension spring.

[0011] As a further improvement to the above technical solution, the mercury speciation extraction module includes an acid-exchange mercury extraction group, an iron-manganese oxide mercury extraction group, an organic-sulfide mercury extraction group, and a residual mercury extraction group.

[0012] As a further improvement to the above technical solution, the acid-exchangeable mercury extraction device includes a first centrifuge tube and a hydrochloric acid solution addition device. The first centrifuge tube is used to hold the conditioned soil sample, and the hydrochloric acid solution addition device is used to add hydrochloric acid solution to the first centrifuge tube to extract acid-exchangeable mercury.

[0013] As a further improvement to the above technical solution, the iron-manganese oxide mercury extraction device includes a second centrifuge tube and a hydroxylamine hydrochloride solution addition device. The second centrifuge tube is used to hold the adjusted soil sample, and the hydroxylamine hydrochloride solution addition device is used to add hydrochloric acid solution to the second centrifuge tube to extract iron-manganese oxide mercury.

[0014] As a further improvement to the above technical solution, the organic-sulfide mercury extraction kit includes a third centrifuge tube and an acetic acid solution addition device. The third centrifuge tube is used to hold the conditioned soil sample, and the acetic acid solution addition device is used to add acetic acid solution to the third centrifuge tube to extract organic-sulfide mercury.

[0015] As a further improvement to the above technical solution, the mercury speciation extraction module also includes a pH testing device and a shaking device.

[0016] As a further improvement to the above technical solution, the residual mercury extraction assembly includes a crucible, a concentrated nitric acid addition device, a hydrofluoric acid addition device, a perchloric acid addition device, a heating device, a cleaning device, and a volume-fixing device.

[0017] As a further improvement to the above technical solution, the volume-fixing device includes a liquid injection mechanism, a shaking mechanism, and a vision sensor. The liquid injection mechanism is used to inject water, the shaking mechanism is used to shake the volume-fixing reagent, and the vision sensor is used to determine the height of the volume-fixing liquid level through acquired image data.

[0018] The beneficial effects of this invention are as follows: by processing the sample through the sample processing mechanism, uniform and stable soil samples can be obtained, improving the accuracy of mercury speciation analysis; through the mercury speciation extraction module, mercury in acid-exchange state, iron-manganese oxide state, organic-sulfide state and residue state in the soil can be obtained, thereby comprehensively analyzing different speciations of mercury in the soil; through the detection technology in the detection module, the content of each speciation of mercury can be detected. Attached Figure Description

[0019] The above and / or additional aspects and advantages of this utility model will become apparent and readily understood from the description of the embodiments taken in conjunction with the following drawings, in which:

[0020] Figure 1 This is a schematic diagram of the structure of a mercury speciation analysis device in mercury-contaminated soil according to an embodiment of the present invention;

[0021] Figure 2 This is an isometric view of a sample processing mechanism according to an embodiment of the present invention;

[0022] Figure 3 This is a cross-sectional view of a sample processing mechanism according to an embodiment of the present invention.

[0023] Figure 4 for Figure 3 Enlarged view of point A in the middle;

[0024] Figure 5 This is a schematic diagram of the structure of a screening screen according to an embodiment of the present invention.

[0025] In the attached diagram: 1-Frame; 101-Feed inlet; 1011-Feed channel; 102-Heating chamber; 1021-Heating wire assembly; 103-Discharge outlet; 104-Grinding drum; 105-Screening screen; 1051-First screening screen; 1052-Second screening screen; 1053-First adjusting groove; 1054-Second adjusting groove; 1055-First fixing pin; 1056-Second fixing pin; 106-Tension spring. Detailed Implementation

[0026] The embodiments of this utility model are described in detail below. Examples of these embodiments are shown in the accompanying drawings, wherein the same or similar reference numerals denote the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the accompanying drawings are exemplary and are only used to explain this utility model, and should not be construed as limiting this utility model.

[0027] In the description of this utility model, it should be understood that the directional descriptions, such as up, down, front, back, left, right, etc., indicate the directional or positional relationship based on the directional or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0028] In the description of this utility model, unless otherwise explicitly defined, terms such as "setting," "installation," and "connection" should be interpreted broadly, and those skilled in the art can reasonably determine the specific meaning of the above terms in this utility model in conjunction with the specific content of the technical solution.

[0029] The following is combined with Figures 1 to 5 The embodiments of this utility model are described below.

[0030] This utility model embodiment provides a device for analyzing the speciation of mercury in mercury-contaminated soil, comprising:

[0031] Rack 1;

[0032] The sample processing mechanism includes an inlet 101, a heating chamber 102, and an outlet 103. The heating chamber 102 is mounted on a frame 1. The inlet 101 is connected to the heating chamber 102 through a feeding channel 1011. A grinding roller 104 is provided in the feeding channel 1011. A sieve 105 is provided between the feeding channel 1011 and the heating chamber 102. A heating wire assembly 1021 is provided in the heating chamber 102. The bottom of the heating chamber 102 is concave downwards, and the outlet 103 is located at the lowest point of the bottom.

[0033] A mercury speciation extraction module is used to extract acid-exchangeable mercury, iron-manganese oxide mercury, organic-sulfide mercury and residual mercury from soil samples.

[0034] The detection module acquires the content of mercury in the extracted acid-exchange state, iron-manganese oxide state, organic-sulfide state, and residue state, respectively.

[0035] The sample processing steps in this implementation include:

[0036] Soil samples are fed into the sample processing mechanism through the inlet 101. The soil samples are first ground by the grinding roller 104 in the feed channel 1011, and then fall into the heating chamber 102 through the sieve 105. The soil samples are dried by the heating wire group 1021 in the heating chamber 102, and finally the processed soil samples are obtained from the outlet 103.

[0037] This embodiment uses a sample processing mechanism to process the sample, which can obtain a uniform and stable soil sample, ensuring the accuracy of mercury speciation analysis. The mercury speciation extraction module can obtain mercury in acid-exchange, iron-manganese oxide, organic-sulfide, and residual forms in the soil, thereby comprehensively analyzing the different forms of mercury in the soil. The detection technology in the detection module can quickly and accurately quantify the content of each form of mercury.

[0038] Further, the sieve 105 in this embodiment includes a first sieve 1051 and a second sieve 1052, which are fitted together vertically. The first sieve 1051 is provided with a first push-pull rod, and the second sieve 1052 is provided with a second push-pull rod. The feed channel 1011 is provided with a first clearance hole and a second clearance hole. The first push-pull rod passes through the first clearance hole, and the second push-pull rod passes through the second clearance hole. The first push-pull rod is provided with a first adjustment groove 1053, and the second push-pull rod is provided with a second adjustment groove 1054. The frame 1 is provided with a first fixing hole and a second fixing hole. The sample processing mechanism also includes a first fixing nail 1055 and a second fixing nail 1056. The first fixing nail 1055 passes through the first adjustment groove 1053 and is threadedly connected to the first fixing hole, and the second fixing nail 1056 passes through the first adjustment groove 1053 and is threadedly connected to the second fixing hole.

[0039] In this embodiment, the first sieve 1051 and the second sieve 1052 are respectively equipped with a first push-pull rod and a second push-pull rod. By pushing and pulling the first push-pull rod and the second push-pull rod, the first sieve 1051 and the second sieve 1052 can be slightly misaligned, thereby adjusting the width of the sieve holes and obtaining soil samples with different particle sizes according to the test. In addition, the setting of the adjustment groove and the fixing nail in this embodiment can facilitate the adjustment of the first push-pull rod and the second push-pull rod, and fix the first sieve 1051 and the second sieve 1052, preventing the first sieve 1051 and the second sieve 1052 from loosening or displacement due to mechanical vibration generated during the operation of the sample processing mechanism, thereby ensuring the accuracy of soil sample sieving.

[0040] Furthermore, in this embodiment, the heating cavity 102 is hinged to the frame 1, and the heating cavity 102 is connected to the frame 1 by a tension spring 106.

[0041] In this example, the grinding roller 104 is driven by a motor, which is mounted on the frame 1. When the motor is working, it will cause a certain vibration to the frame 1. Since the heating chamber 102 is connected to the frame 1 through the tension spring 106, when the frame 1 vibrates, the tension spring 106 can increase the vibration duration of the heating chamber 102, causing the heating chamber 102 to shake up and down, so that the soil sample can fall smoothly into the outlet 103 in the heating chamber 102.

[0042] In this example, the transfer of soil samples between various mechanisms / modules is carried out by human hands or robotic arms.

[0043] Furthermore, the device for analyzing the speciation of mercury in mercury-contaminated soil also includes a soil condition adjustment module. The soil condition adjustment module includes a reagent addition mechanism, a heating mechanism, a pH adjustment group, an organic matter content adjustment group, a moisture content adjustment group, and a temperature control group. The reagent addition mechanism is electrically connected to the pH adjustment group, the organic matter content adjustment group, and the moisture content adjustment group, respectively. The heating mechanism is electrically connected to the moisture content adjustment group and the temperature control group.

[0044] Specifically, the soil condition adjustment steps in this embodiment include:

[0045] The pH adjustment group controls the addition of appropriate amounts of acid or alkali solutions to adjust the pH value of the soil sample to the target range (3.0-8.0).

[0046] By adding appropriate amounts of organic matter or oxidants through the organic matter content adjustment group control reagent addition mechanism, the organic matter content of the soil sample is adjusted to the target range (1%-10%).

[0047] The appropriate amount of water is added by controlling the reagent addition mechanism of the moisture content adjustment group, and the heating mechanism is controlled to dry the soil sample, so that the moisture content of the soil sample is adjusted to the target range (10%-40%).

[0048] The heating mechanism is controlled by a temperature control unit to keep the temperature of the soil sample within the target range (10℃-40℃).

[0049] This implementation includes a soil condition adjustment module that comprehensively considers the effects of soil pH, organic matter content, moisture content, and temperature on mercury speciation, making it suitable for soil mercury pollution analysis under different environmental conditions.

[0050] Furthermore, the mercury speciation extraction module includes an acid-exchange mercury extraction group, an iron-manganese oxide mercury extraction group, an organic-sulfide mercury extraction group, and a residual mercury extraction group, which can extract mercury in different forms from the soil so that the detection module can obtain the mercury content in different forms.

[0051] Furthermore, the acid-exchangeable mercury extraction assembly includes a first centrifuge tube and a hydrochloric acid solution addition device. The first centrifuge tube is used to hold the conditioned soil sample, and the hydrochloric acid solution addition device is used to add hydrochloric acid solution to the first centrifuge tube to extract the acid-exchangeable mercury. The independent arrangement of the first centrifuge tube and the hydrochloric acid solution addition device can prevent cross-contamination of reagents.

[0052] Furthermore, the iron-manganese mercury oxide extraction kit includes a second centrifuge tube and a hydroxylamine hydrochloride solution addition device. The second centrifuge tube is used to hold the conditioned soil sample, and the hydroxylamine hydrochloride solution addition device is used to add hydrochloric acid solution to the second centrifuge tube to extract iron-manganese mercury oxide. The independent setup of the second centrifuge tube and the hydroxylamine hydrochloride solution addition device can prevent cross-contamination of reagents.

[0053] Furthermore, the organic-sulfide mercury extraction kit includes a third centrifuge tube and an acetic acid solution addition device. The third centrifuge tube is used to hold the conditioned soil sample, and the acetic acid solution addition device is used to add acetic acid solution to the third centrifuge tube to extract organic-sulfide mercury. The independent setup of the third centrifuge tube and the acetic acid solution addition device can prevent cross-contamination of reagents.

[0054] Furthermore, the mercury speciation extraction module also includes a pH testing device and an oscillation device. The pH testing device can monitor the acidity and alkalinity of the reaction system in real time to ensure accurate extraction conditions for different speciations of mercury. The oscillation device accelerates the contact between the reagent and the soil sample through mechanical vibration, thereby improving the extraction rate.

[0055] Furthermore, the residual mercury extraction assembly includes a crucible, a concentrated nitric acid addition device, a hydrofluoric acid addition device, a perchloric acid addition device, a heating device, a cleaning device, and a volume-fixing device. The heating device accelerates the acidolysis reaction, the cleaning device removes residual acid, and the volume-fixing device ensures the precise volume of the final solution, thereby improving detection accuracy.

[0056] Furthermore, the volume-fixing device includes a liquid injection mechanism, a shaking mechanism, and a vision sensor. The liquid injection mechanism is used to inject water, the shaking mechanism is used to shake the volume-fixing reagent, and the vision sensor is used to determine the volume-fixing liquid level height through acquired image data, enabling automated operation.

[0057] Specifically, the mercury speciation extraction step in this embodiment includes:

[0058] Soil samples were placed into a first centrifuge tube, a second centrifuge tube, a third centrifuge tube, and a crucible, respectively.

[0059] 0.1 mol / L hydrochloric acid solution was added to the first centrifuge tube using a hydrochloric acid solution adding device, while the pH value was controlled (to 2.0 ± 0.1) using a pH testing device. The tube was shaken using a shaking device (for 1 hour) and then centrifuged using a centrifuge device (centrifugation speed of 3000 rpm and centrifugation time of 10 minutes) to extract acid-exchangeable mercury.

[0060] 0.04 mol / L hydroxylamine hydrochloride solution was added to the second centrifuge tube using a hydroxylamine hydrochloride solution adding device, while the pH value was controlled (to 1.5 ± 0.1) using a pH testing device. The tube was shaken using a shaking device (6 hours) and then centrifuged using a centrifuge device (centrifugation speed of 3000 rpm, centrifugation time of 10 minutes) to extract iron-manganese mercury oxide.

[0061] 0.02 mol / L acetic acid solution was added to the third centrifuge tube using an acetic acid solution adding device, while the pH value was controlled (to 2.0 ± 0.1) using a pH testing device. The tube was shaken using a shaking device (for 1 hour) and then centrifuged using a centrifuge device (centrifugation speed of 3000 rpm and centrifugation time of 10 minutes) to extract organic-sulfide mercury.

[0062] Add 10 mL of concentrated nitric acid, 10 mL of hydrofluoric acid, and 3 mL of perchloric acid to the crucible using a concentrated nitric acid addition device, a hydrofluoric acid addition device, and a perchloric acid addition device, respectively. Cover the crucible and heat it using a heating device (first at 80°C for 1 hour, then at 120°C for 1 hour). Open the crucible lid to remove silicon, repeating the process until white fumes cease and the contents of the crucible become viscous. Clean the crucible lid and inner wall using a cleaning device. Add 1 mL of nitric acid solution (V(HNO3)∶V(H2O)=1∶1) to the crucible using a nitric acid solution addition device. Transfer the solution to a volume-fixing device to achieve volume fixation, obtaining residual mercury.

[0063] In this process, water is injected into the volume-fixing device through a liquid injection mechanism, while a visual sensor ensures that the water is injected to the required volume-fixing liquid level. Finally, the volume-fixing reagent is shaken evenly by a shaking mechanism.

[0064] Furthermore, in this embodiment, the detection module is a hydrogenation generation-atomic fluorescence spectrometer, which is used to obtain mercury content information so as to more quickly and accurately quantify the content of various forms of mercury.

[0065] The preferred embodiments of the present invention have been described in detail above, but the present disclosure is not limited to the embodiments described. Those skilled in the art can make various equivalent modifications or substitutions without departing from the spirit of the present invention, and these equivalent modifications or substitutions are all included within the scope defined by the claims of the present disclosure.

Claims

1. A device for analyzing the speciation of mercury in mercury-contaminated soil, characterized in that, include: frame; A sample processing mechanism includes an inlet, a heating chamber, and an outlet. The heating chamber is mounted on a frame. The inlet is connected to the heating chamber via a feeding channel. A grinding roller is provided in the feeding channel. A sieve screen is provided between the feeding channel and the heating chamber. A heating wire assembly is provided in the heating chamber. The bottom of the heating chamber is concave, and the outlet is located at the lowest point of the bottom. A mercury speciation extraction module is used to extract acid-exchangeable mercury, iron-manganese oxide mercury, organic-sulfide mercury and residual mercury from soil samples. The detection module acquires the content of mercury in the extracted acid-exchange state, iron-manganese oxide state, organic-sulfide state, and residue state, respectively.

2. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 1, characterized in that, The screening mesh includes a first screening mesh and a second screening mesh, which are fitted together vertically. The first screening mesh is provided with a first push-pull rod, and the second screening mesh is provided with a second push-pull rod. The feed channel is provided with a first clearance hole and a second clearance hole. The first push-pull rod passes through the first clearance hole, and the second push-pull rod passes through the second clearance hole. The first push-pull rod is provided with a first adjustment groove, and the second push-pull rod is provided with a second adjustment groove. The frame is provided with a first fixing hole and a second fixing hole. The sample processing mechanism also includes a first fixing nail and a second fixing nail. The first fixing nail passes through the first adjustment groove and is threadedly connected to the first fixing hole, and the second fixing nail passes through the first adjustment groove and is threadedly connected to the second fixing hole.

3. The speciation analysis device for mercury in mercury-contaminated soil according to claim 1, characterized in that, The heating chamber is hinged to the frame, and the heating chamber is connected to the frame by a tension spring.

4. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 1, characterized in that, The mercury speciation extraction module includes an acid-exchange mercury extraction group, an iron-manganese oxide mercury extraction group, an organic-sulfide mercury extraction group, and a residual mercury extraction group.

5. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 4, characterized in that, The acid-exchangeable mercury extraction kit includes a first centrifuge tube and a hydrochloric acid solution addition device. The first centrifuge tube is used to hold the conditioned soil sample, and the hydrochloric acid solution addition device is used to add hydrochloric acid solution to the first centrifuge tube to extract acid-exchangeable mercury.

6. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 4, characterized in that, The iron-manganese-oxidized mercury extraction kit includes a second centrifuge tube and a hydroxylamine hydrochloride solution addition device. The second centrifuge tube is used to hold the conditioned soil sample, and the hydroxylamine hydrochloride solution addition device is used to add hydrochloric acid solution to the second centrifuge tube to extract iron-manganese-oxidized mercury.

7. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 4, characterized in that, The organic-sulfide mercury extraction kit includes a third centrifuge tube and an acetic acid solution addition device. The third centrifuge tube is used to hold the conditioned soil sample, and the acetic acid solution addition device is used to add acetic acid solution to the third centrifuge tube to extract organic-sulfide mercury.

8. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to any one of claims 5-7, characterized in that, The mercury speciation extraction module also includes a pH testing device and an oscillation device.

9. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 4, characterized in that, The residual mercury extraction unit includes a crucible, a concentrated nitric acid addition device, a hydrofluoric acid addition device, a perchloric acid addition device, a heating device, a cleaning device, and a volume-fixing device.

10. The apparatus for analyzing the speciation of mercury in mercury-contaminated soil according to claim 9, characterized in that, The volume-fixing device includes a liquid injection mechanism, a shaking mechanism, and a vision sensor. The liquid injection mechanism is used to inject water, the shaking mechanism is used to shake the volume-fixing reagent, and the vision sensor is used to determine the height of the volume-fixing liquid level through acquired image data.

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