CN211611721U

CN211611721U - Device of heavy metal in desorption reagent

Info

Publication number: CN211611721U
Application number: CN201922277906.9U
Authority: CN
Inventors: 曾嵘斌
Original assignee: Nanjing Yunyou Biotechnology Co ltd
Current assignee: Nanjing Yunyou Biotechnology Co ltd
Priority date: 2019-12-18
Filing date: 2019-12-18
Publication date: 2020-10-02
Anticipated expiration: 2029-12-18

Abstract

The utility model provides a device of heavy metal in desorption reagent, including constant potential device, power module, power adapter and electrolysis container, power adapter with power module connects, power module with constant potential device connects, the inside grafting of electrolysis container has counter electrode, working electrode and reference electrode, counter electrode, working electrode and reference electrode are connected respectively to constant potential device's C, W, R ports. The utility model discloses a heavy metal among the electrochemical reduction heavy metal technique desorption reagent, its simple structure easily realizes, does not destroy other compositions of reagent in the desorption heavy metal, can greatly reduce reagent solution's heavy metal background, can provide pure reagent for more accurate heavy metal analysis detects.

Description

Device of heavy metal in desorption reagent

Technical Field

The utility model relates to a heavy metal analysis technical field particularly, relates to a device of heavy metal in desorption reagent.

Background

Heavy metals as products of heavy nuclear fission are widely existed in nature in the earth evolution process, particularly lead elements, most of the heavy metals such as lead, cadmium, mercury and the like are not necessary for life activities, thus threatening the survival of organisms and the health of human beings, and the analysis and detection of the heavy metals can lead people to early warn in advance to reduce the damage of the heavy metals. With the rapid development of analysis and test technologies, more and more methods can be applied to the analysis of the content of heavy metals in different samples, the sensitivity and accuracy of detection are greatly improved, and trace heavy metals can be detected, so that a technical guarantee is provided for people pursuing safer and healthier life. However, when the heavy metal lead is a trace sample, the background brought by the used reagent is equivalent to or slightly greater than the lead content in the sample, and the background brought by the reagent influences the test result. The corresponding method comprises the following steps: 1. selecting a very pure reagent (such as a reagent with a high grade purity or a reagent with a higher grade purity); 2. in the analysis, a blank sample is tested, and a blank background is deducted after the test of the actual sample is combined; 3. the background of heavy metals, particularly lead, in the reagent is removed.

Because heavy metals, particularly lead, generally exist, the reagent still can cause heavy metal residues in the environment in the preparation process, and the reagent with more or less heavy metal lead residues no matter how high the grade of the reagent is; blank background subtraction is adopted, when the amount of the blank background is equal to or slightly larger than that of the sample, the blank background presents larger error to low concentration, and the result of the actual sample is seriously interfered; the background of heavy metal lead in the reagent is removed, so that the background can be ignored in the detection, and the analysis is convenient.

Removing heavy metal by medicament method, adsorption method, ultrafiltration method, electrolysis method, etc., such as patent CN200910192427.5, adjusting pH to 9-10 with medicament sodium carbonate, and maintaining temperature to remove heavy metal impurities; the use of added agents introduces impurities to the reagents.

The adsorption method is simple to operate, for example, patent CN201410375446.2 discloses a bifunctional mesoporous silica for adsorbing heavy metal ions in water, the working process is performed at room temperature, no other chemical reagent is required to be added, and the problems of complex preparation of the adsorbent, high price, regeneration of the adsorbent and the like mainly exist.

Ultrafiltration is commonly used for preparing pure water, for example, CN201711410355.8 provides a green preparation method of integrated circuit boards, where the treated waste water of cleaning liquid is sequentially micro-filtered and ultra-filtered, and then enters a reuse water treatment system, but when used for removing heavy metals from reagents, the content of reagents affecting analysis is often reduced.

For example, patent CN201510907181.0 discloses an electrochemical method for removing heavy metal impurities in potassium salt reagent, which is to use an electrolysis method to reduce the concentration of heavy metal impurities in potassium salt, and the electrolysis device is complex and complicated to operate.

SUMMERY OF THE UTILITY MODEL

An object of the utility model is to provide a device of heavy metal in desorption reagent, it is complicated to have solved the device structure among the prior art, complex operation, problem that the cost is with high costs.

In order to solve the technical problem, the utility model discloses a technical scheme is: the device for removing heavy metals in the reagent comprises a constant potential device, a power supply module, a power supply adapter and an electrolytic container, wherein the power supply adapter is connected with the power supply module, the power supply module is connected with the constant potential device, a counter electrode, a working electrode and a reference electrode are inserted into the electrolytic container, and the C, W, R port of the constant potential device is respectively connected with the counter electrode, the working electrode and the reference electrode.

As a preferred scheme, the device also comprises a blending device, wherein the blending device comprises a series container and a pump, the series container is communicated with the electrolysis container through two guide pipes, and the guide pipes are provided with the pump for providing power for circulation.

Preferably, the catheter is a transparent PVC plastic pipe, the pump is a direct-current peristaltic pump, the input voltage of the direct-current peristaltic pump is 5V, and the output flow rate of the direct-current peristaltic pump is 0.5 ml/min to 100 ml/min.

Preferably, the electrolytic cell further comprises a blending device, wherein the blending device comprises a magnetic stirrer and a stirrer, and the stirrer is positioned inside the electrolytic vessel.

Preferably, the counter electrode is a platinum sheet electrode, the working electrode is a bismuth carbon electrode, and the reference electrode is a silver-silver chloride electrode.

Preferably, the power supply further comprises a rechargeable battery, and the rechargeable battery is electrically connected with the power supply module and serves as a standby power supply.

Compared with the prior art, the beneficial effects of the utility model include: the electrochemical reduction heavy metal technology is adopted, heavy metal ions in the reagent are reduced to be elementary substances which are enriched on the working electrode, the content of heavy metal in the reagent is removed, the heavy metal background of the reagent is reduced, a device for removing the heavy metal in the reagent is built according to the principle, the structure is simple, the realization is easy, other components in the reagent are not damaged when the heavy metal is removed, the heavy metal background of the reagent solution can be greatly reduced, and the pure reagent can be provided for more precise analysis and detection of the heavy metal.

Drawings

The disclosure of the present invention is explained with reference to the drawings. It is to be understood that the drawings are designed solely for the purposes of illustration and not as a definition of the limits of the invention. In the drawings, like reference numerals are used to refer to like parts. Wherein:

fig. 1 schematically shows a structural diagram of an apparatus for removing heavy metals from a reagent according to an embodiment of the present invention;

fig. 2 schematically shows a schematic circuit diagram of a potentiostat according to an embodiment of the invention;

fig. 3 schematically shows a structural diagram of an apparatus for removing heavy metals from a reagent according to another embodiment of the present invention.

Reference numbers in the figures: 1-a constant potential device, 2-a power supply module, 3-a power supply adapter, 4-a rechargeable battery, 5-a counter electrode, 6-a working electrode, 7-a reference electrode, 8-an electrolytic container, 9-a series container, 10-a conduit, 11-a pump, 12-a magnetic stirrer and 13-a stirrer.

Detailed Description

It is easily understood that, according to the technical solution of the present invention, a plurality of alternative structural modes and implementation modes can be proposed by those skilled in the art without changing the spirit of the present invention. Therefore, the following detailed description and the accompanying drawings are merely illustrative of the technical solutions of the present invention, and should not be considered as limiting or restricting the technical solutions of the present invention in their entirety or in any other way.

An embodiment according to the present invention is shown in conjunction with fig. 1. The utility model provides a device of heavy metal in desorption reagent, including constant potential device 1, power module 2, power adapter 3 and electrolytic container 8, power adapter 3 is connected with power module 2, power module 2 is connected with constant potential device 1, electrolytic container 8 is the polypropylene wide-mouthed reagent bottle, and reagent bottle bottleneck threaded connection has the bottle lid, it has counter electrode 5 to peg graft on the bottle lid, working electrode 6 and reference electrode 7, counter electrode 5 is connected respectively to constant potential device 1's C, W, R port, working electrode 6 and reference electrode 7.

The constant potential device 1 is of a YB-P-M-I type produced by Nanjing Yunyu biological technology limited, and the power supply module 2 is of a YB-PMM-A type produced by Nanjing Yunyu biological technology limited.

In this embodiment, the working electrode 6 is an inert electrode, in order to enhance the electrochemical reduction enrichment effect, a mercury, bismuth or antimony membrane material is modified on the surface of the inert electrode, preferably a bismuth carbon working electrode, in order to improve the electrochemical reduction efficiency, the surface area of the working electrode 6 is larger than that of the counter electrode 5 and the reference electrode 7, and the area of the working electrode 6 is 6 × 10 cm; the counter electrode 5 is an inert electrode, preferably a platinum sheet electrode; the reference electrode 7 is commonly a calomel electrode, a silver-silver chloride electrode, preferably a silver-silver chloride electrode.

Fig. 2 is a schematic circuit diagram of the potentiostat 1. The constant potential device 1 outputs the electric potential regulated by the electrode to control the electrochemical reaction process, the high-impedance-1V input voltage is output as the low-impedance-1V output voltage through the voltage follower U5-B, the standard-1V voltage (which is not changed by the resistance change of the electrolytic cell) provided to the W end of the working electrode is taken as the reference voltage, when the constant potential device works, the D/A input of the control module is converted by the D/A of the U5-A chip, through negative feedback, the constant voltage output with high impedance is provided for the R end of the reference electrode and the output with low impedance current is provided for the C end of the counter electrode to maintain the constant potential between the W end and the R end, the constant potential between the W end and the R end is controlled by changing the D/A input of the control module, and different electrochemical actions with different requirements are realized by different constant potentials between the W end and the R end.

The counter electrode 5, the working electrode 6 and the reference electrode 7 are respectively connected with an C, W, R port of the constant potential device 1, the effective areas of the three electrodes are immersed in a reagent solution to be treated, a reduction potential is applied to the working electrode 6, the range is-1.4V-0.8V, preferably-1.0V, and electrochemical reduction is started to enrich heavy metal on the working electrode 6.

In the embodiment, the device further comprises a blending device, the blending device comprises a serial container 9 and a pump 11, the serial container 9 is communicated with the electrolytic container 8 through an upper guide pipe 10 and a lower guide pipe 10, the guide pipes 10 are made of transparent PVC plastic pipes with the diameter of 5 mm, the pump 11 is arranged on the guide pipe 10 located below the guide pipes and used for providing power for circulation of reagent solution, a direct-current peristaltic pump is selected, the input voltage is 5V, and the output flow rate is 0.5 ml/min-100 ml/min, preferably 10 ml/min. The power module 2 is electrically connected with the direct-current peristaltic pump and provides electric energy for the direct-current peristaltic pump. After the device is started, the direct-current peristaltic pump conveys the reagent solution in the electrolytic container 8 to the series container 9 through the lower conduit 10, and then conveys the reagent solution in the series container 9 to the electrolytic container 8 through the upper conduit 10, so that the reagent solution is circularly and uniformly mixed.

Further, the power supply device also comprises a rechargeable battery 4, wherein the rechargeable battery 4 is electrically connected with the power supply module 2, 5V voltage is input from the power supply adapter 3 to the power supply module 2, the power supply module 2 respectively outputs the voltage to the constant potential device 1 and the rechargeable battery 4, a comparison circuit is attached to the power supply module 2, and when no 5V voltage is output from the power supply adapter 3 due to power failure and the like, the power supply device is immediately switched to the rechargeable battery 4 for supplying power.

When the device works, a proper amount of reagent solution of ammonium citrate and hydrochloric acid is added into an electrolytic container 8 and a series container 9, the electrolytic container 8 is communicated with the series container 9 through a guide pipe 10, a working electrode 6, a reference electrode 7 and a counter electrode 5 are fixed on a bottle cap, the bottle cap is screwed on the electrolytic container 8, and the positions of the electrodes are adjusted to ensure that the effective areas of the three electrodes are fully immersed in the reagent solution; the three electrodes are connected with a constant potential device through signal lines, the constant potential device 1 is powered by a power module 2, a direct current peristaltic pump is started, the reagent solution stably and circularly flows in the series container 9, the constant potential device 1 is started, and the heavy metal in the reagent solution is enriched on the working electrode 6. In the working process, only the heavy metal content of the reagent solution in the series container 9 needs to be detected, when the heavy metal background of the reagent solution is lower than the specified requirement, the series container 9 can be replaced, and the treated reagent solution for removing the heavy metal is extracted; it is also possible to first take the electrodes out, then turn off the potentiostat 1 and finally turn off the power supply and then extract the treated reagent solution.

Another embodiment according to the present invention is shown in connection with fig. 3. In the present embodiment, the difference from the above embodiments is that the blending device includes a magnetic stirrer 12 and a stirrer 13, the stirrer 13 is located inside the electrolytic vessel 8, and the magnetic stirrer 12 is located below the electrolytic vessel 8 and is used for supporting the electrolytic vessel 8. After the magnetic stirrer 12 is started, the stirrer 13 is driven to rotate under the action of magnetic force, and the reagent solution to be treated in the electrolytic container 8 is uniformly mixed.

When the device works, a proper amount of ammonium oxalate and hydrochloric acid reagent solution is added into an electrolytic container 8, then a working electrode 6, a reference electrode 7 and a counter electrode 5 are fixed on a bottle cap, the bottle cap is screwed on the electrolytic container 8, and the position of the electrode is adjusted, so that the effective area of the electrode is fully immersed in the reagent solution; the three electrodes are connected with a constant potential device 1 through a signal wire, the constant potential device 1 is powered by a power module 2, a magnetic stirrer 12 is started, a stirrer 13 drives a reagent solution to stably rotate and mix uniformly at the bottom of an electrolytic container 8, the constant potential device 1 is started, heavy metal in the reagent solution is enriched on a working electrode, the heavy metal content of the reagent solution is detected in the working process, when the heavy metal background of the reagent solution is lower than the specified requirement, the electrode is taken out firstly, then the constant potential device 1 and the magnetic stirrer 12 are closed, finally, a power supply is cut off, and the treated reagent solution is provided for heavy metal detection.

The technical scope of the present invention is not limited to the content in the above description, and those skilled in the art can make various modifications and alterations to the above embodiments without departing from the technical spirit of the present invention, and these modifications and alterations should fall within the protection scope of the present invention.

Claims

1. The device for removing the heavy metal in the reagent is characterized by comprising a constant potential device (1), a power supply module (2), a power supply adapter (3) and an electrolytic container (8), wherein the power supply adapter (3) is connected with the power supply module (2), the power supply module (2) is connected with the constant potential device (1), a counter electrode (5), a working electrode (6) and a reference electrode (7) are inserted into the electrolytic container (8), and C, W, R ports of the constant potential device (1) are respectively connected with the counter electrode (5), the working electrode (6) and the reference electrode (7).

2. The device for removing heavy metals in reagent according to claim 1, further comprising a blending device, wherein the blending device comprises a series container (9) and a pump (11), the series container (9) is communicated with the electrolytic container (8) through two guide pipes (10), and the guide pipes (10) are provided with the pump to provide power for circulation.

3. The device for removing heavy metals in reagent according to claim 2, wherein the conduit (10) is a transparent PVC plastic pipe, the pump (11) is a direct-current peristaltic pump, the input voltage of the direct-current peristaltic pump is 5V, and the output flow rate of the direct-current peristaltic pump is 0.5 ml/min to 100 ml/min.

4. The device for removing heavy metals in reagent according to claim 1, further comprising a blending device, wherein the blending device comprises a magnetic stirrer (12) and a stirrer (13), and the stirrer (13) is located inside the electrolytic vessel (8).

5. The device for removing the heavy metals in the reagent according to claim 1, wherein the counter electrode (5) is a platinum sheet electrode, the working electrode (6) is a bismuth carbon electrode, and the reference electrode (7) is a silver-silver chloride electrode.

6. The device for removing heavy metals in reagent according to any one of claims 1 to 4, further comprising a rechargeable battery (4), wherein the rechargeable battery (4) is electrically connected with the power supply module (2) and is used as a backup power supply.