CN110987921B - Portable device and method for rapidly and qualitatively determining heavy metal ions in soil - Google Patents

Portable device and method for rapidly and qualitatively determining heavy metal ions in soil Download PDF

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CN110987921B
CN110987921B CN201911368825.8A CN201911368825A CN110987921B CN 110987921 B CN110987921 B CN 110987921B CN 201911368825 A CN201911368825 A CN 201911368825A CN 110987921 B CN110987921 B CN 110987921B
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reagent
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qualitative
sample
soil
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CN110987921A (en
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石美
赵高文
王朝辉
孙莹莹
王浩琳
张欣欣
童行伟
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Northwest A&F University
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    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour

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Abstract

The invention discloses a portable device and a method for rapidly and qualitatively determining heavy metal ions in soil, wherein the device comprises a sample cylinder, a sample detection area, a soil sample area and a qualitative color development area, wherein the sample detection area, the soil sample area and the qualitative color development area are sequentially arranged from top to bottom; the upper part of the detection reagent sample area is provided with a plurality of reagent injection ports, and a bottom plate of the detection reagent sample area is in threaded connection with the soil sample area; a plurality of first reagent flow ports are formed in the bottom plate of the detection reagent sample area, and a reagent propeller for pushing a reagent is arranged in the detection reagent sample area; the lower part of the soil sample area and the qualitative color developing area are fixed into a whole; a baffle is arranged between the soil sample area and the qualitative color developing area, a plurality of second reagent circulation ports are formed in the baffle, and the bottom plate of the qualitative color developing area is in threaded connection with the side wall of the qualitative color developing area. The method has the problems of complex detection process of common pollutants in soil, professional required equipment, complex detection process, strong specialization and high popularization difficulty.

Description

Portable device and method for rapidly and qualitatively determining heavy metal ions in soil
Technical Field
The invention belongs to the technical field of environmental engineering, and particularly relates to a portable device and a method for rapidly and qualitatively determining heavy metal ions in soil. In particular to a portable device which can rapidly and effectively qualitatively detect whether certain heavy metal ions exist in soil.
Background
The current environment faces the serious pollution problem brought by the development of the fields of industry, agriculture and service industry, the soil pollution problem is more serious and prominent, the soil pollution can bring pollution elements into plants, enrich in the metabolism of crops and gradually enrich in human bodies in a food chain, so that great potential safety hazards are brought to human individuals, and partial heavy metals can influence the health of the next generation of the plants, thereby causing serious problems of malformed infants and the like. The detection of pollutants such as known pollution elements or heavy metals needs complicated procedures such as sampling, sample conveying, submission, detection and the like, the time consumption is long, the method is not suitable for soil samples needing rapid qualitative determination, not all the samples need strict quantitative pollutant analysis, and in addition, the professional determination process has high difficulty and professional performance and is difficult to widely popularize and use. In practical situations, many tests only require simple qualitative detection and then quantitative analysis.
Disclosure of Invention
The invention provides a portable device and a method for rapidly and qualitatively determining heavy metal ions in soil, and solves the problems of complicated detection process, required equipment specialty, complicated detection process, strong specialization and great popularization difficulty of common pollutants in soil.
In order to achieve the purpose, the portable soil heavy metal ion rapid qualitative determination device comprises a sample cylinder, wherein the sample cylinder comprises a detection reagent sample area, a soil sample area and a qualitative color development area which are sequentially arranged from top to bottom, and the detection reagent sample area is in threaded connection with the soil sample area;
the upper part of the detection reagent sample area is provided with a plurality of reagent injection ports, and a bottom plate of the detection reagent sample area is in threaded connection with the soil sample area; a plurality of first reagent circulation ports are formed in the bottom plate of the detection reagent sample area, and a reagent propelling device for propelling the reagent is arranged in the detection reagent sample area;
the lower part of the soil sample area and the qualitative color developing area are fixed into a whole; a baffle is arranged between the soil sample area and the qualitative color developing area, a plurality of second reagent circulation ports are formed in the baffle, and the bottom plate of the qualitative color developing area is in threaded connection with the side wall of the qualitative color developing area.
Further, the reagent pushing device comprises a hydraulic pushing plate and a hydraulic button, the hydraulic pushing plate is driven by the hydraulic device, and the hydraulic button is used for starting or retracting the hydraulic pushing plate.
Furthermore, the soil sample area and the qualitative color developing area are both provided with a backflow-preventing and blocking-preventing vertical pipe, a backflow-preventing and blocking-preventing cap is sleeved on the top of the backflow-preventing and blocking-preventing vertical pipe, the backflow-preventing and blocking-preventing cap is a shell, the upper portion of the backflow-preventing and blocking-preventing cap is waterproof, and the lower portion of the backflow-preventing and blocking-preventing cap is permeable.
Furthermore, the side walls of the soil sample area and the qualitative color developing area are both provided with an electric heating spiral pipe and a temperature sensor.
Furthermore, a reagent recovery port is formed in a bottom plate of the qualitative color developing area, a waste liquid area is in threaded connection with the lower portion of the qualitative color developing area, the waste liquid area is divided into a hydraulic bin and a liquid storage bin by a partition plate, waste liquid holes are formed in the partition plate, a sponge and a hydraulic rod are arranged in the liquid storage bin, and a hydraulic pushing plate is fixed at the upper end of the hydraulic rod; the bottom of the liquid storage bin is connected with a waste liquid pipeline, and a valve is arranged on the waste liquid pipeline.
Further, a sealing plug is arranged in the reagent injection port.
Further, when the measurement is carried out, the sample cylinder is fixed on a fixing frame through a device fixing clamp, and the fixing frame is fixed on the base.
Furthermore, the detection reagent sample area is divided into a plurality of sample chambers which are independent from each other by a separation plate.
A soil heavy metal ion rapid qualitative determination method based on the device comprises the following steps:
step 1, separating a soil sample area from a detection reagent sample area; separating the bottom plate of the qualitative color developing area from the side wall of the qualitative color developing area, putting a solid or liquid reagent required for color development into the qualitative color developing area, and then reinstalling the bottom plate of the qualitative color developing area to the qualitative color developing area;
step 2, loading a soil sample into a soil sample area;
step 3, adding the leaching reagent solution into the separated detection reagent sample area through a reagent injection port;
step 4, mounting the detection reagent sample area and the soil sample area together;
and 5, enabling the detection reagent to flow into the soil sample area and react with the heavy metal salt in the soil body in the soil sample area, enabling the heavy metal to flow into the qualitative color developing area along with the detection reagent, observing the change of the color developing agent in the qualitative color developing area, and comparing the related colors to give a qualitative conclusion whether the pollutants containing the heavy metal are contained.
Further, in step 5, the sample cylinder is fixed on a fixing frame, the waste liquid recovery cup is placed below a reagent recovery port formed in a bottom plate of the qualitative color developing area, and waste liquid is collected.
Compared with the prior art, the invention has at least the following beneficial technical effects:
the portable soil heavy metal ion rapid qualitative determination device provided by the invention integrates the functions of sample, reagent and color development, avoids complicated operation steps, does not need to carry various glass containers and reagents for detection, and can perform a soil heavy metal detection test at any time. After the heavy metals in the soil sample containing the heavy metals are leached out, different colors can be displayed in the color development solid or liquid reagent in the color development area after a certain reagent is added, so that whether the heavy metals and the heavy metal content are contained can be judged according to the color and the shade degree of the color development area reagent or the solid, the defects of a complicated detection quantitative determination process can be overcome, the composition is complete, and through a simpler operation process, the qualitative detection of pollutants can be simultaneously carried out on multiple soil samples, so that the pollutant monitoring efficiency is improved, and the invention is beneficial to popularization.
Furthermore, the soil sample area and the qualitative color developing area are both provided with a backflow-preventing and blocking-preventing vertical pipe, a backflow-preventing and blocking-preventing cap is sleeved on the top of the backflow-preventing and blocking-preventing vertical pipe, the backflow-preventing and blocking-preventing cap is a shell, the upper portion of the backflow-preventing and blocking-preventing cap is waterproof, and the lower portion of the backflow-preventing and blocking-preventing cap is permeable. On one hand, soil sample particles are prevented from entering the next flow, on the other hand, the reagent is ensured to be fully contacted with the soil sample, heavy metals and other pollutants in the soil sample can be fully leached or dissolved, and the smooth operation of the color development flow is facilitated; in order to ensure the effect of the backflow-preventing and blocking-preventing vertical pipe, the backflow-preventing and blocking-preventing cap is sleeved at the top end of the backflow-preventing and blocking-preventing vertical pipe, the upper part of the backflow-preventing and blocking-preventing cap is waterproof, the lower part of the backflow-preventing and blocking-preventing cap is made of soft plastics full of pores, and equivalently, liquid enters a solution channel from the lower part and then enters the next step flow, so the effect is better.
Furthermore, the soil sample area and the qualitative color development area side wall are provided with an electric heating spiral pipe and a temperature sensor, a rechargeable electric heating sleeve can be turned on or turned off according to the real-time temperature collected by the temperature sensor, and the temperature of the soil area and the color development area is controlled, so that the whole process is effectively carried out.
Furthermore, a reagent recovery port is formed in a bottom plate of the qualitative color developing area, a waste liquid area is in threaded connection with the lower portion of the qualitative color developing area, the waste liquid area is divided into a hydraulic bin and a liquid storage bin by a partition plate, waste liquid holes are formed in the partition plate, a sponge and a hydraulic rod are arranged in the liquid storage bin, and a hydraulic pushing plate is fixed at the upper end of the hydraulic rod; the bottom of the liquid storage bin is connected with a waste liquid pipeline, and a valve is arranged on the waste liquid pipeline. The valve is adapted to be manually opened after the hydraulic button is actuated to allow waste fluid to flow through the waste pipe, and the switch prevents waste fluid from flowing when the waste reservoir is removed. Waste liquid district is arranged in the waste liquid absorbing sponge at first inhales the waste liquid that flows down on the upper portion in the sponge, prevents that equipment from getting into the color development district again and producing adverse effect to the experimental result at removal in-process waste liquid.
Furthermore, a reagent recovery port is formed in the bottom plate, a waste liquid recovery cup is placed below the reagent recovery port, waste liquid is collected, and the waste liquid can be treated in a centralized mode after being collected, so that environmental pollution is prevented.
Furthermore, a sealing plug is arranged in the reagent injection port to prevent the detection reagent from overflowing.
Further, when the test is carried out, the sample cylinder is fixed on the fixing frame through the equipment fixing clamp, the fixing frame is fixed on the base, special personnel are not needed to take the sample cylinder, the operation is convenient, and in addition, an installation space is reserved for the waste liquid recovery cup.
Furthermore, the detection reagent sample area is divided into a plurality of mutually independent sample chambers by the partition plate, the detection of the soil samples can be simultaneously carried out, the number of the sample area can be adjusted according to actual needs, and the plurality of soil sample chambers are arranged to be parallel to simultaneously carry out heavy metal detection on the plurality of soil samples, so that the detection speed and efficiency are improved, the discrete error caused by a single soil body is avoided, and the reliability and the accuracy of the obtained data can be improved.
The rapid qualitative determination method for the heavy metal ions in the soil based on the device can fully overcome the defects of a fussy quantitative determination process, and can perform pollutant qualitative detection on multiple soil samples simultaneously through a simpler operation process, so that the pollutant monitoring efficiency is improved, and the rapid qualitative determination method is favorable for popularization.
Drawings
FIG. 1 is an overall schematic view of embodiment 1;
FIG. 2 is a schematic view of a detection reagent sample zone;
FIG. 3 is a schematic view of a reagent pusher;
FIG. 4 is an overall schematic view of embodiment 2;
FIG. 5 is a partial schematic view of embodiment 2;
fig. 6 is a schematic view of the backflow prevention and anti-blocking cap of embodiment 2.
In the drawings: 1. a base, 2, a fixing frame, 3, a connecting piece, 4, an equipment fixing clamp, 5, a sample cylinder, 6, a waste liquid recovery cup, 7, a reagent propeller, 51, a detection reagent sample area, 52, a soil sample area, 53, a qualitative color development area, 54, a reagent injection port, 56, a first reagent one-way flow port, 57, a second reagent one-way flow port, 59, a reagent recovery port, 510, a separation plate, 511, a sealing plug, 512, a baffle plate, 5101 and a sample chamber; 531. a bottom plate of the qualitative color developing area, 8, a hydraulic pushing plate, 9 and a hydraulic button; 10. the device comprises an electric heating spiral pipe, 11, a first electric heating sleeve, 12, a first temperature sensor, 121, a liquid crystal temperature display screen, 13, a second temperature sensor, 14, a second electric heating sleeve, 15, a hydraulic button, 16, a backflow-preventing and blocking-preventing vertical pipe, 161, a backflow-preventing and blocking-preventing cap, 17, a hydraulic propelling plate, 18, sponge, 19, a hydraulic rod, 20, a waste liquid pipeline, 21, a waste liquid area, 22 and a partition board.
Detailed Description
In order to make the objects and technical solutions of the present invention clearer and easier to understand. The present invention will be described in further detail with reference to the following drawings and examples, wherein the specific examples are provided for illustrative purposes only and are not intended to limit the present invention.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientations and positional relationships indicated in the drawings, which are based on the orientations and positional relationships indicated in the drawings, and are used for convenience in describing the present invention and for simplicity in description, but do not indicate or imply that the device or element so referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified. In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; 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 meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
Referring to fig. 1, a portable soil heavy metal ion rapid qualitative determination device comprises a base 1, an equipment fixing clamp 4, a sample cylinder 5, a reagent propeller 7 and a waste liquid recovery cup 6.
The upper end fixedly connected with equipment fixing clamp of base 1 is fixed with connecting piece 3 on the equipment fixing clamp, is fixed with a plurality of equipment fixing clamps through the fastener on the connecting piece 3, and the centre gripping has sample cylinder 5 in the equipment fixing clamp, and reagent propeller 7 is installed on 5 upper portions of sample cylinder, and 5 below of sample cylinder are provided with waste liquid recovery cup 6, and waste liquid recovery cup 6 places on base 1.
The sample cylinder 5 comprises a detection reagent sample area 51, a soil sample area 52 and a qualitative color developing area 53 which are sequentially connected from top to bottom, wherein the detection reagent sample area 51 is in threaded connection with the soil sample area 52.
The detection reagent sample area 51 is used for containing liquid reagents for leaching heavy metals or other pollutants in the soil sample, a plurality of reagent injection ports are formed in the upper portion of the detection reagent sample area 51 and used for injecting detection reagents into the detection reagent sample area, the detection reagents can be blocked by the sealing plug 511 after injection, the reagents are prevented from being leaked, and the sealing plug 511 is a rubber plug. The detection reagent sample area 51 is provided with a reagent pusher 7 that can be pushed. The bottom plate of the detection reagent sample area is provided with external threads for being fixedly connected with the soil sample area. The type and form of the reagent are determined according to the detection requirement of the reagent.
The soil sample area 52 is used for containing soil samples obtained in the environment, the upper end of the inner wall of the soil sample area 52 is provided with threads for being fixedly connected with the detection reagent sample area, and the lower part of the inner wall of the soil sample area 52 is fixedly integrated with the qualitative color developing area 53.
The qualitative color developing area 53 is used for containing a color developing solid or liquid reagent, and the type and the form of the reagent are determined according to the detection requirement of the reagent.
A plurality of first reagent circulation ports 56 are uniformly formed in the bottom plate 515 of the detection reagent sample area 51, and one-way valves are installed in the first reagent circulation ports 56; the soil sample area 52 is fixedly connected with the qualitative color developing area 53, a baffle 512 is arranged between the soil sample area 52 and the qualitative color developing area 53, a plurality of second reagent flow ports 57 are formed in the baffle 512, and one-way valves are installed in the second reagent flow ports 57; qualitative color development district's bottom plate 531 and its lateral wall threaded connection have seted up reagent recovery mouth 59 on qualitative color development district's the bottom plate 531, and waste liquid recovery cup 6 has been placed to reagent recovery mouth below, and waste liquid recovery cup 6 is used for collecting the waste liquid that flows from color development district's reagent recovery mouth 59.
The reagent propeller 7 is positioned in the detection reagent sample area 51, and carries out waterproof treatment on the bottom of the bottom plate 531 of the qualitative color development area, so as to prevent the reagent of the color development area and the liquid leached by the soil sample chamber on the upper part from leaking out of the detection reagent, and the specific waterproof treatment is to wind a waterproof adhesive tape at the threaded connection part of the bottom plate 531 and the qualitative color development area 53 of the qualitative color development area. Reagent propeller main action lies in utilizing the promotion process, pushes away measuring reagent in the soil sample through first one-way circulation port 61 to reach and leach the effect of soil with the pollutant.
Referring to fig. 2, the sample area of the detection reagent is divided into four independent sample chambers 5101 by cross-shaped partition plates, which can simultaneously detect 4 groups of soil samples, and the number of the sample areas can be adjusted according to actual needs.
Referring to fig. 3, the reagent pusher 7 includes a connecting rod 71, a pressing plate 72 is fixed to one end of the connecting rod 71, a handle 73 is fixed to the other end of the connecting rod 71, the pressing plate 72 extends into the detection reagent sample region 51, the handle 73 and the pressing plate 72 are disc-shaped, and the pressing plate 72 is in clearance fit with the inner wall of the detection reagent sample region 51.
The method for carrying out the rapid qualitative determination of the metal ions by using the device comprises the following steps:
step 1, firstly, rotating a detection reagent sample area 51 to separate the soil sample area from the detection reagent sample area; separating the bottom plate of the qualitative color developing area from the side wall of the qualitative color developing area, inverting the qualitative color developing area 53, putting a color developing reagent into the qualitative color developing area 53, putting a solid or liquid reagent required for color development into the qualitative color developing area, leaving a space for the entry of leachate if the liquid reagent cannot be filled, screwing the bottom plate 531 of the qualitative color developing area, and then reloading the bottom plate of the qualitative color developing area back to the qualitative color developing area 53.
And 2, filling the soil sample into the soil sample area 52, wherein the soil sample can be filled or partially filled according to the reagent condition, and the soil sample cannot be compacted to ensure that the leaching process is smoothly carried out.
And 3, pulling the reagent pusher 7 to the highest position, wherein the highest position of the reagent pusher 7 is above the position of the reagent injection port, adding the leaching reagent solution into the separated detection reagent sample area through the reagent injection port 54, and plugging the reagent injection port 54 by using a sealing plug 511 after the injection is finished.
Step 4, connecting the detection reagent sample area 51 with the soil sample area through threads, and finishing the basic sample loading process; before screwing, a waterproof adhesive tape is wound on the lower inner thread of the detection reagent sample area 51.
And 5, clamping the connected device on the fixed frame 2 by using two equipment fixing clamps 4, wherein the reliability and stability of clamping are required to be paid attention to in the clamping process.
And 6, placing the waste liquid recovery cup under the reagent recovery port for collecting waste liquid in the detection process.
And 7, pushing down the reagent propeller 7 according to actual measurement requirements for testing, wherein after the reagent propeller 7 pushes down the reagent, the reagent can enter the soil sample area 52, fully reacts with heavy metal salt in the soil body, releases heavy metal in the soil body, and enters the color development area along with the reagent, and at the moment, because the reagent carries heavy metal ions, the reagent can perform color development reaction with the reagent in the color development area to present different colors, and the change of the color development agent is observed in the qualitative color development area 53, so that a qualitative conclusion whether the color card contains pollutants including the heavy metal is given by comparing the color card.
For example, when heavy metals Cr (VI) are detected, the corresponding color developing agents are: weighing diphenyl carbonyl dihydrazide, dissolving in a small amount of acetone, adding water for dilution, and then adding sulfuric acid for acidification to serve as a color development reagent. The color development results are: purple red. The color varies depending on the Cr (VI) concentration. Cr (VI) can be directly filtered out by pure water, and the color developing agent is prepared by the following steps: weighing diphenyl carbodihydrazide, dissolving in a small amount of acetone, adding water for dilution, and then adding sulfuric acid for acidification to complete the preparation of the color developing agent. Therefore, in this example, pure water is used as the leaching agent, and by pushing water into the soil sample chamber, cr (vi) is washed out and enters the color development region, in which the color development agent configured as described above is placed, and when cr (vi) enters the color development region along with pure water, a purple color appears.
Example 2
Referring to fig. 4 to 5, the portable soil heavy metal ion rapid qualitative determination device comprises a base 1, an equipment fixing clamp 4, a sample cylinder 5, a reagent propulsion device and a waste liquid recovery cup 6.
The upper end fixedly connected with equipment fixing clamp of base 1 is fixed with connecting piece 3 on the equipment fixing clamp, is fixed with a plurality of equipment fixing clamps through the fastener on the connecting piece 3, and the centre gripping has sample cylinder 5 in the equipment fixing clamp, and reagent pusher is installed on 5 upper portions of sample cylinder, and 5 below of sample cylinder are provided with waste liquid recovery cup 6, and waste liquid recovery cup 6 places on base 1.
The sample cylinder 5 comprises a detection reagent sample area 51, a soil sample area 52 and a qualitative color developing area 53 which are sequentially connected from top to bottom, wherein the detection reagent sample area 51 is in threaded connection with the soil sample area 52.
The detection reagent sample area 51 is used for containing liquid reagents for leaching heavy metals or other pollutants in the soil sample, a plurality of reagent injection ports are formed in the upper portion of the detection reagent sample area 51 and used for injecting detection reagents into the detection reagent sample area, the detection reagents can be blocked by the sealing plug 511 after injection, the reagents are prevented from being leaked, and the sealing plug 511 is a rubber plug. The detection reagent sample area 51 is provided with a reagent propulsion device which can be pushed. The bottom plate of the detection reagent sample area is provided with external threads for being fixedly connected with the soil sample area. The type and form of the reagent are determined according to the detection requirement of the reagent.
The soil sample area 52 is used for containing soil samples obtained in the environment, the upper end of the inner wall of the soil sample area 52 is provided with threads for being fixedly connected with the detection reagent sample area, and the lower part of the inner wall of the soil sample area 52 is fixedly integrated with the qualitative color developing area 53. The qualitative color developing area 53 is used for containing a color developing solid or liquid reagent, and the type and the form of the reagent are determined according to the detection requirement of the reagent.
A plurality of first reagent circulation ports 56 are uniformly formed in the bottom plate 515 of the detection reagent sample area 51, and one-way valves are installed in the first reagent circulation ports 56; the soil sample area 52 is fixedly connected with the qualitative color developing area 53, a baffle 512 is arranged between the soil sample area 52 and the qualitative color developing area 53, a plurality of second reagent flow ports 57 are formed in the baffle 512, and one-way valves are installed in the second reagent flow ports 57; qualitative color development district's bottom plate 531 and its lateral wall threaded connection have seted up reagent recovery mouth 59 on qualitative color development district's the bottom plate 531, and waste liquid recovery cup 6 has been placed to reagent recovery mouth below, and waste liquid recovery cup 6 is used for collecting the waste liquid that flows from color development district's reagent recovery mouth 59. All install the check valve in first reagent circulation mouth and the second reagent circulation mouth, ensure the flow direction of reagent, guarantee the accuracy of testing result.
The reagent propeller 7 is positioned in the detection reagent sample area 51, and carries out waterproof treatment on the bottom of the bottom plate 531 of the qualitative color development area, so as to prevent the reagent of the color development area and the liquid leached by the soil sample chamber on the upper part from leaking out of the detection reagent, and the specific waterproof treatment is to wind a waterproof adhesive tape at the threaded connection part of the bottom plate 531 and the qualitative color development area 53 of the qualitative color development area. Reagent propeller main effect lies in utilizing the promotion process, pushes away detection reagent to soil sample through first one-way circulation mouth 61 in to reach and drench the effect of filtering out soil with the pollutant.
Referring to fig. 2, the sample area of the detection reagent is divided into four independent sample chambers 5101 by cross-shaped partition plates, which can simultaneously detect 4 groups of soil samples, and the number of the sample areas can be adjusted according to actual needs.
Referring to fig. 4, the reagent advancing device comprises a hydraulic advancing plate 8 and a hydraulic button 9 for activating or retracting the hydraulic advancing plate 8. The hydraulic pushing plate 8 is disc-shaped, and the hydraulic pushing plate 8 is in clearance fit with the inner wall of the detection reagent sample area 51. The reagent pushing device is used for starting the hydraulic device after the reagent is placed in the reagent area, and the hydraulic plate pushes the reagent downwards.
The backflow-preventing and anti-blocking vertical pipe 16 is arranged in each independent subarea of the soil sample area 52 and the qualitative color developing area 53, so that on one hand, soil sample particles are prevented from entering the next flow, on the other hand, the reagent is ensured to be fully contacted with a soil sample, heavy metals and other pollutants in the soil sample can be fully leached or dissolved, and the smooth proceeding of the color developing flow is facilitated;
referring to fig. 6, in order to ensure the function of the backflow-preventing and blocking-preventing vertical pipe 16, a backflow-preventing and blocking-preventing cap 161 is installed on the backflow-preventing and blocking-preventing vertical pipe 16, the backflow-preventing and blocking-preventing cap 161 is a shell, the upper part of the backflow-preventing and blocking-preventing cap 161 is cylindrical, the top surface and the circumference of the cylindrical shell are impermeable, the lower part of the cylindrical shell is a conical shell, the conical shell is made of soft plastic full of pores, and can be sleeved on the top of the backflow-preventing and blocking-preventing vertical pipe, which is equivalent to that liquid enters a solution channel from the lower part and then enters the next process, so that the effect is better.
The soil sample area 52 is provided with a first temperature sensor 12, the qualitative color area 53 is provided with a second temperature sensor 13, and the liquid crystal temperature display screens 121 of the first temperature sensor 12 and the second temperature sensor 13 are arranged on the outer wall of the sample cylinder 5 to display the temperature conditions collected by the two sensors in real time.
Soil sample district 52 lateral wall all is provided with first electric heat sleeve 11, qualitative color development district 53 lateral wall all is provided with second electric heat sleeve 14, all be provided with electric heat spiral pipe 10 in first electric heat sleeve 11 and the second electric heat sleeve 14, because some color development reactions or drench the reaction that filters out with heavy metal and pollutant and need go on under specific high temperature, can open or close rechargeable electric heat sleeve according to the real-time temperature that temperature sensor gathered, the temperature in control soil district and color development district, thereby guarantee that whole process is effectual goes on.
The lower part of the qualitative color display area 53 is in threaded connection with a waste liquid area 21, the waste liquid area 21 is divided into a hydraulic bin and a liquid storage bin by a partition plate 22, a waste liquid hole is formed in the partition plate 22, a sponge 18 and a hydraulic rod 19 are arranged in the liquid storage bin, a hydraulic pushing plate 17 is fixed at the upper end of the hydraulic rod, the hydraulic pushing plate 17 is a porous thin plate, and a waste liquid area hydraulic button 15 is arranged on the outer wall of the waste liquid area 21 and used for starting or withdrawing the hydraulic rod 19; waste liquid district 21 bottom is provided with waste liquid pipeline 20 at waste liquid district hydraulic button 15's offside, installs the valve on the waste liquid pipeline, after opening hydraulic button 15, manually opens this valve to allow the waste liquid to flow through waste liquid pipeline, this switch can prevent that the waste liquid from flowing when removing the waste liquid pond in addition. The waste liquid area is provided with a sponge 18 for absorbing waste liquid, and waste liquid flowing down from the upper part is firstly absorbed into the sponge 18, so that the waste liquid is prevented from entering the color development area again in the moving process of the equipment to generate adverse effect on the experimental result.
A one-key hydraulic extrusion device is additionally arranged in the waste liquid area 21 and consists of a hydraulic propulsion plate 17 and a hydraulic rod 19, the hydraulic propulsion plate 17 is a porous thin plate and is connected with the hydraulic rod 19, the sponge 18 is pressed under the hydraulic propulsion plate, waste liquid can enter the sponge through holes in the hydraulic propulsion plate 17, and after more waste liquid is absorbed in the sponge 18, the hydraulic device is started to extrude the waste liquid into a waste liquid bin and discharge the waste liquid.
The hydraulic button 9 is a control button of the hydraulic propelling plate 8 corresponding to a hydraulic system, and the inside of the device is integrally communicated without applying a large load, so that the force required in the liquid propelling process and the sponge compressing process is very small, the required hydraulic device is small, and large burden can not be caused to carrying.
Another alternative method is to replace the lifting of the motor, and replace the hydraulic plate 8 and the hydraulic device corresponding to the waste recovery with the driving of a small motor, because the force for driving the two plates is small, the control of the small motor can be realized.
The method for carrying out the rapid qualitative determination of the metal ions by using the device comprises the following steps:
step 1, firstly, rotating a detection reagent sample area 51 to separate the soil sample area from the detection reagent sample area; separating the bottom plate of the qualitative color developing area from the side wall of the qualitative color developing area, inverting the qualitative color developing area 53, putting a color developing reagent into the qualitative color developing area 53, putting a solid or liquid reagent required for color development into the qualitative color developing area, leaving a space for the entry of leachate if the liquid reagent cannot be filled, screwing the bottom plate 531 of the qualitative color developing area, and then reloading the bottom plate of the qualitative color developing area back to the qualitative color developing area 53.
Step 2, the soil sample is filled into the soil sample area 52, and the soil sample can be filled or partially filled according to the reagent condition, so that the leaching process can be carried out smoothly, and the soil sample cannot be compacted excessively.
And 3, adding the leaching reagent solution into the separated detection reagent sample area through the reagent injection port 54, and after the injection is finished, plugging the reagent injection port 54 by using a sealing plug 511.
Step 4, connecting the detection reagent sample area 51 with the soil sample area through threads, and finishing the basic sample loading process; before screwing, a waterproof adhesive tape is wound on the lower inner thread of the detection reagent sample area 51.
And 5, clamping the connected device on the fixed frame 2 by using two equipment fixing clamps 4, wherein the reliability and stability of clamping are required to be paid attention to in the clamping process.
And 6, placing the waste liquid recovery cup under the reagent recovery port for collecting waste liquid in the detection process.
And 7, pushing down the reagent pushing device according to actual metering requirements for testing, wherein after the reagent pushing device pushes down the reagent, the reagent enters the soil sample area 52, at the moment, the reagent can fully react with heavy metal salt in the soil body due to the existence of the backflow prevention anti-blocking vertical pipe, the heavy metal in the soil body is released and enters the color development area along with the reagent, at the moment, the reagent can generate color development reaction with the reagent in the color development area due to the fact that the reagent carries heavy metal ions, different colors are presented, the change of the color development agent is observed in the qualitative color development area 53, and a qualitative conclusion that whether the color card contains pollutants including the heavy metal is given by comparing.
For example, when heavy metals Cr (VI) are detected, the corresponding color developing agents are: weighing diphenyl carbonyl dihydrazide, dissolving in a small amount of acetone, adding water for dilution, and then adding sulfuric acid for acidification to serve as a color development reagent. The color development results are: purple red. The color varies depending on the Cr (VI) concentration. Cr (VI) can be directly filtered out by pure water, and the color developing agent is prepared by the following steps: weighing diphenyl carbodihydrazide, dissolving in a small amount of acetone, adding water for dilution, and then adding sulfuric acid for acidification to complete the preparation of the color developing agent. Therefore, in this example, pure water is used as the leaching agent, and by pushing water into the soil sample chamber, cr (vi) is washed out and enters the color development region, in which the color development agent configured as described above is placed, and when cr (vi) enters the color development region along with pure water, a purple color appears.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.

Claims (7)

1. The portable soil heavy metal ion rapid qualitative determination device is characterized by comprising a sample cylinder (5), wherein the sample cylinder (5) comprises a detection reagent sample area (51), a soil sample area (52) and a qualitative color development area (53) which are sequentially arranged from top to bottom, and the detection reagent sample area (51) is in threaded connection with the soil sample area (52);
a plurality of reagent injection ports (54) are formed in the upper part of the detection reagent sample area (51), and the bottom plate of the detection reagent sample area (51) is in threaded connection with the soil sample area (52); a plurality of first reagent circulation ports (56) are formed in the bottom plate of the detection reagent sample area (51), and a reagent pushing device for pushing a reagent is arranged in the detection reagent sample area (51);
the lower part of the soil sample area (52) is fixed with the qualitative color developing area (53) into a whole; a baffle plate (512) is arranged between the soil sample area (52) and the qualitative color developing area (53), a plurality of second reagent flow ports (57) are formed in the baffle plate (512), and the bottom plate of the qualitative color developing area (53) is in threaded connection with the side wall of the qualitative color developing area;
soil sample district (52) and qualitative color rendering district (53) all are provided with prevents that the refluence prevents stifled riser (16), prevent that the cover of stifled riser of refluence (16) top has prevents stifled cap of refluence (161), prevent that the cap of refluence prevents stifled (161) is the casing, prevent that the cap of refluence prevents stifled (161) upper portion is waterproof, and the lower part permeates water.
2. The portable soil heavy metal ion rapid qualitative and quantitative determination device according to claim 1, characterized in that, the reagent propulsion device comprises a hydraulic propulsion plate and a hydraulic button (9), the hydraulic propulsion plate is driven by a hydraulic device, and the hydraulic button (9) is used for starting or retracting the hydraulic propulsion plate.
3. The portable soil heavy metal ion rapid qualitative determination apparatus according to claim 1, characterized in that the soil sample region (52) and the qualitative color development region (53) are provided with an electrothermal spiral tube (10) and a temperature sensor on their side walls.
4. The portable soil heavy metal ion rapid qualitative and quantitative determination device according to claim 1, wherein a reagent recovery port (59) is formed in a bottom plate of the qualitative color development region (53), a waste liquid region (21) is in threaded connection with the lower portion of the qualitative color development region (53), the waste liquid region (21) is divided into a hydraulic chamber and a liquid storage chamber by a partition plate (22), a waste liquid hole is formed in the partition plate (22), a sponge (18) and a hydraulic rod (19) are arranged in the liquid storage chamber, and a hydraulic propulsion plate is fixed at the upper end of the hydraulic rod; the bottom of the liquid storage bin is connected with a waste liquid pipeline, and a valve is arranged on the waste liquid pipeline.
5. The portable soil heavy metal ion rapid qualitative and quantitative determination device as claimed in claim 1, wherein the reagent injection port (54) is provided with a sealing plug (511).
6. The portable soil heavy metal ion rapid qualitative and qualitative determination apparatus according to claim 1, characterized in that, when performing the determination, the sample cylinder (5) is fixed on the fixing frame (2) through the device fixing clamp (4), and the fixing frame (2) is fixed on the base (1).
7. The portable soil heavy metal ion rapid qualitative determination device of claim 1, wherein the detection reagent sample area (51) is divided into a plurality of independent sample chambers (5101) by partition plates (510).
CN201911368825.8A 2019-12-26 2019-12-26 Portable device and method for rapidly and qualitatively determining heavy metal ions in soil Active CN110987921B (en)

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