Detection device

By designing a device for detection of volatile sulfides in solid samples and using a diaphragm pump to realize gas circulation flow, the problems of expensive and cumbersome gas chromatography detection methods in the prior art are solved, and efficient and accurate sulfide detection is achieved.

CN119985366APending Publication Date: 2025-05-13CHINA UNIV OF GEOSCIENCES (BEIJING)
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Patent Information

Application Number
CN202510171064.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-02-17
Publication Date
2025-05-13

AI Technical Summary

Technical Problem

In the prior art, gas chromatography is used to detect volatile sulfides in solids with high maintenance and operation costs, and cumbersome operation process, which affects the convenience and accuracy of detection.

Method used

A detection device is designed, through the combination of the gas generating part, absorbing part, reflux part and detection part, and the diaphragm pump is used to circulate between the gas generating part and the alkali absorption bottle until all the gas is absorbed by the alkali absorption bottle, reducing the number of alkali absorption bottles and improving the detection accuracy.

Benefits of technology

By reducing the number of alkali absorbing bottles, the device improves the absorption efficiency and detection accuracy of sulfides, reduces the operation complexity and system errors, and is suitable for the rapid detection of field samples.

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Abstract

The invention discloses a detection device, and relates to the technical field of detection devices. The device is used for detecting the content of volatile sulfide in a solid sample or hydrogen sulfide in gas, and comprises a gas generation part, the output end of which is connected with an output pipe; the absorption part comprises an alkali liquor absorption bottle, the alkali liquor absorption bottle is a three-way reagent bottle, the end, away from the gas generation part, of the output pipe is connected with a gas inlet pipe of the alkali liquor absorption bottle, the alkali liquor absorption bottle is further connected with an exhaust pipe and a liquid discharge pipe, and liquid in the alkali liquor absorption bottle is discharged through the liquid discharge pipe; the backflow part comprises a diaphragm pump, the input end of the diaphragm pump is connected with the exhaust pipe through a conveying pipe, the output end of the diaphragm pump is connected with a backflow pipe, and the end, away from the diaphragm pump, of the backflow pipe is connected with the input end of the gas generation part; and the detection part comprises a spectrophotometer. The detection device provided by the invention can be used for detecting the content of volatile sulfide in a solid sample or hydrogen sulfide in gas, so that the detection accuracy is improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of detection devices, and more particularly to a detection device. Background Art

[0002] Sulfide is widely present in nature and artificial environments, such as volcanoes, hot springs, sulfur-rich soils, industrial wastewater, and artificially constructed sulfur autotrophic microbial systems or sulfate reduction systems. The reduction of elemental sulfur or sulfate will produce sulfide, which is specifically manifested as volatile sulfide in sediments, sulfur ions or hydrogen sulfide ions in water, and hydrogen sulfide in the gas phase. Sulfide in water or volatilized to form hydrogen sulfide is seriously harmful to the human body, so the detection of sulfide is of great significance.

[0003] In the currently available technology, the detection of sulfide in liquid phase can be quickly detected by methylene blue spectrophotometry, and the detection of gaseous hydrogen sulfide is mainly through gas chromatography. Similarly, the detection of volatile sulfide in solid phase such as activated sludge and soil sediment is mainly to acidify sulfide to produce hydrogen sulfide, and then the concentration of hydrogen sulfide is detected by gas chromatography to calculate the content of sulfide in solid phase. However, gas chromatography is expensive and has high maintenance and operation costs. The pretreatment and operation process of gas chromatography detection of volatile sulfide in solid are cumbersome. According to the above, absorbing gas phase or solid phase sulfide into liquid phase and then detecting it by methylene blue spectrophotometry is simple to operate and has strong applicability.

[0004] The Chinese utility model patent with application number "201721166608.7" discloses a sulfide detection device in mud samples, including a blowing device, a detection frame, an acidification device and an absorption device. The acidification device includes a three-necked flask, and a temperature sensor and a hydrogen sulfide outlet pipe are arranged in the right inlet of the three-necked flask. The absorption device includes a first overflow pipe, the first overflow pipe is connected to the hydrogen sulfide outlet pipe through a second connecting hose, the first overflow pipe is connected to a first absorption bottle, the first absorption bottle is connected to the second overflow pipe, the second overflow pipe is connected to the third overflow pipe through a third connecting hose, and the third overflow pipe is connected to the second absorption bottle. The utility model has a compact structure and is easy to use. The nitrogen blowing flow rate can be accurately controlled by a needle valve flowmeter, the water bath temperature can be accurately controlled by a temperature sensor, and the two groups of absorption bottles can effectively improve the hydrogen sulfide recovery rate and improve the accuracy of the detection results. However, there are the following disadvantages: 1. The absorption efficiency of hydrogen sulfide is improved by adding alkali solution absorption bottles. The ability of two groups of absorption bottles to improve the absorption efficiency of hydrogen sulfide is limited. Too many absorption bottles will affect the workload of subsequent detection, and the operation is cumbersome and increases the system error; 2. Inert gas nitrogen is required for stripping, and a flow meter is required to strictly control the gas flow, and a water bath device is required for heating, which is not conducive to the collection and pretreatment of field samples; 3. No anti-backflow device is set, and the pressure difference at the end of nitrogen stripping may cause alkali solution reflux and contaminate the sample. Summary of the invention

[0005] In view of this, the present invention provides a detection device for detecting the content of volatile sulfide in solid samples or hydrogen sulfide in gas, which enhances the absorption effect and improves the detection accuracy. In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0006] The present invention provides a detection device, comprising:

[0007] A gas generating unit, wherein an output end of the gas generating unit is connected to an output pipe, and an anti-back-inhalation airbag is connected to the output pipe;

[0008] The absorption part comprises an alkali solution absorption bottle, wherein the alkali solution absorption bottle is a three-way reagent bottle, wherein one end of the output pipe away from the gas generating part is connected to the air inlet pipe of the alkali solution absorption bottle, and the alkali solution absorption bottle is also connected to an exhaust pipe and a drain pipe, through which the liquid in the alkali solution absorption bottle is discharged;

[0009] A reflux unit, comprising a diaphragm pump, wherein the input end of the diaphragm pump is connected to the exhaust pipe via a delivery pipe, the output end of the diaphragm pump is connected to a reflux pipe, and one end of the reflux pipe away from the diaphragm pump is connected to the input end of the gas generating unit;

[0010] The detection part includes a spectrophotometer, which detects the sulfide ion concentration of the liquid in the alkali solution absorption bottle by using the spectrophotometer.

[0011] According to some embodiments provided by the present invention, when used to detect the content of volatile sulfides in a solid sample, the gas generating part includes an acidifying reagent bottle, which is a three-way reagent bottle, and is connected to a liquid inlet pipe, an air outlet pipe and an air guide pipe, the end of the air outlet pipe away from the acidifying reagent bottle is connected to the output pipe, the end of the air guide pipe away from the acidifying reagent bottle is connected to the reflux pipe, and a hydrochloric acid solution is introduced into the acidifying reagent bottle through the liquid inlet pipe.

[0012] According to other embodiments provided by the present invention, when used to detect the content of hydrogen sulfide in gas, the gas generating part includes a gas collecting bag, and the gas collecting bag is provided with a gas inlet and a gas outlet, the gas inlet is connected to the reflux pipe, and the gas outlet is connected to the output pipe.

[0013] Furthermore, the air inlet pipe extends into the bottom end of the alkali solution absorption bottle, and one end of the air inlet pipe away from the output pipe is connected to a porous aeration head.

[0014] Furthermore, an acidification syringe is connected to one end of the liquid inlet tube away from the acidification reagent bottle.

[0015] Furthermore, the liquid inlet pipe and the liquid discharge pipe are respectively provided with an injection valve and a sampling valve.

[0016] Furthermore, the diaphragm pump is connected with a USB wire.

[0017] Furthermore, the output pipe is connected to an anti-backflow airbag.

[0018] It can be seen from the above technical scheme that, compared with the prior art, the present invention discloses a detection device, which uses a diaphragm pump to allow the gas in the gas generating part to enter the alkali solution absorption bottle through the output pipe to react, and then the unreacted gas in the alkali solution collecting bottle is re-introduced into the gas generating part, so that the gas circulates between the gas generating part and the alkali solution absorption bottle until the gas is completely absorbed by the alkali solution absorption bottle. The gas can be completely absorbed using one alkali solution absorption bottle, thereby reducing the number of alkali solution absorption bottles and improving the detection accuracy. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.

[0020] Figure 1 A schematic diagram of the structure of the detection device provided by the present invention;

[0021] Figure 2 A schematic diagram of the structure of an air collecting bag is provided for the present invention;

[0022] Figure 3 A graph showing the results of alkaline solution absorption testing after acidification using a solid sulfide ion standard sample provided by the present invention;

[0023] Figure 4 This is a graph of the alkaline solution absorption test results after acidification of a gaseous sulfide ion standard sample provided by the present invention.

[0024] In the figure: 1. Gas generating part; 101. Acidification syringe; 102. Injection valve; 103. Acidification reagent bottle; 104. Connecting hose; 105. Gas collecting bag; 106. Gas inlet, 107. Gas outlet; 2. Reflux part; 201. Reflux pipe; 202. Diaphragm pump; 203. USB wire; 205. Delivery pipe; 3. Absorption part; 301. Anti-backflow air bag; 302. Drain pipe; 303. Alkali solution absorption bottle; 304. Porous aeration head; 305. Sampling valve. DETAILED DESCRIPTION

[0025] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0026] See also Figure 1-4 The embodiment of the present invention discloses a detection device for detecting the content of volatile sulfide in a solid sample or hydrogen sulfide in a gas, comprising:

[0027] A gas generating unit 1, wherein an output end of the gas generating unit 1 is connected to an output pipe;

[0028] The absorption part 3 includes an alkali solution absorption bottle 303, which is a three-way reagent bottle. The end of the output pipe away from the gas generating part 1 is connected to the air inlet pipe of the alkali solution absorption bottle 303. The alkali solution absorption bottle 303 is also connected to an exhaust pipe and a drain pipe 302, and the liquid in the alkali solution absorption bottle 303 is discharged through the drain pipe 302;

[0029] The reflux part 2 includes a diaphragm pump 202, the input end of the diaphragm pump 202 is connected to the exhaust pipe through a delivery pipe 205, the output end of the diaphragm pump 202 is connected to a reflux pipe 201, and one end of the reflux pipe 201 away from the diaphragm pump 202 is connected to the input end of the gas generating part 1;

[0030] The detection unit includes a spectrophotometer, which detects the sulfide ion concentration of the liquid in the alkali solution absorption bottle 303 using a spectrophotometer.

[0031] The alkali solution absorption bottle 303 contains sodium hydroxide solution. The hydrogen sulfide in the gas generating part 1 enters the alkali solution absorption bottle 303 through the output pipe and the air inlet pipe under the action of the diaphragm pump 202. Part of the hydrogen sulfide gas reacts with the sodium hydroxide solution, and part of the gas that fails to react with the sodium hydroxide returns to the gas generating part 1 along the exhaust pipe, the delivery pipe 205 and the reflux pipe 201 under the action of the diaphragm pump 202 and enters the alkali solution absorption bottle 303 again to react with the sodium hydroxide. This process is repeated until the hydrogen sulfide gas is completely absorbed by the sodium hydroxide solution. The reacted material in the alkali solution absorption bottle 303 is taken out through the drain pipe 302, and the sulfide ion concentration in the material is detected by a spectrophotometer using methylene blue spectrophotometry.

[0032] In some embodiments, the gas flow rate of the diaphragm pump 202 is 200-2000 mL / min, and the gas circulation time is 10-300 min.

[0033] In some embodiments, the alkali solution collection bottle contains 0.5-2M NaOH solution with a volume of 50-150 mL.

[0034] In some embodiments, the hydrochloric acid solution is 0.1-2M, and the amount of hydrochloric acid added is 10-100 mL according to the type and content of the test sample.

[0035] In some embodiments, when used to detect the content of volatile sulfides in a solid sample, the gas generating part 1 includes an acidifying reagent bottle 103, which is a three-way reagent bottle. The acidifying reagent bottle 103 is connected with a liquid inlet pipe, an air outlet pipe and an air guide pipe. The end of the air outlet pipe away from the acidifying reagent bottle 103 is connected to the output pipe, and the end of the air guide pipe away from the acidifying reagent bottle 103 is connected to the reflux pipe 201, and a hydrochloric acid solution is introduced into the acidifying reagent bottle 103 through the liquid inlet pipe.

[0036] When the content of volatile sulfide in the solid sample is detected, the outlet pipe and the output pipe, the reflux pipe 201 and the air guide pipe are connected to form a circulation loop among the acidifying reagent bottle 103, the output pipe, the alkali solution absorption bottle 303, the exhaust pipe, the diaphragm pump 202 and the reflux pipe 201. The solid sample containing volatile sulfide to be detected is placed in the acidifying reagent bottle 103, 50 mL of 2M hydrochloric acid solution is introduced into the acidifying reagent bottle 103 through the liquid inlet pipe, and 20 mL of 2M hydrochloric acid solution is introduced into the alkali solution absorption bottle 303. 3 is filled with 150 mL of 1M sodium hydroxide solution, and the diaphragm pump 202 is turned on. The hydrochloric acid solution reacts with the sulfide to generate hydrogen sulfide. Under the action of the diaphragm pump 202, the hydrogen sulfide generated in the acidifying reagent bottle 103 circulates in the alkali solution absorption bottle 303 and the acidifying reagent bottle 103. After 30 minutes, the material in the alkali solution absorption bottle 303 is taken out, and the sulfur ion concentration in the material is detected by a spectrophotometer, and the content of volatile sulfide in the solid sample is converted.

[0037] In some embodiments, an end of the liquid inlet tube away from the acidification reagent bottle 103 is connected to an acidification syringe 101 .

[0038] In some embodiments, the liquid inlet pipe and the liquid outlet pipe 302 are respectively provided with an injection valve 102 and a sampling valve 305 .

[0039] In other embodiments, when used to detect the content of hydrogen sulfide in the gas, the gas generating unit 1 includes a gas collecting bag 105, which is provided with a gas inlet 106 and a gas outlet 107, the gas inlet 106 is connected to the reflux pipe 201, and the gas outlet 107 is connected to the output pipe.

[0040] When used to detect the content of hydrogen sulfide in the gas, the gas inlet 106 is connected to the reflux pipe 201, the gas outlet 107 and the output pipe, so that the gas collecting bag 105, the output pipe, the alkali solution absorption bottle 303, the exhaust pipe, the diaphragm pump 202 and the reflux pipe 201 form a circulation loop, the gas collecting bag 105 is filled with 200mL of hydrogen sulfide-containing gas, 150mL of 1M sodium hydroxide solution is added to the alkali solution absorption bottle 303, and then the diaphragm pump 202 is turned on, and the material in the alkali solution absorption bottle 303 is taken out after 30 minutes, and the sulfur ion concentration in the material is detected by a spectrophotometer, and the concentration of hydrogen sulfide in the gas is converted.

[0041] In some embodiments, the air inlet pipe extends into the bottom end of the alkali solution absorption bottle 303 , and one end of the air inlet pipe away from the output pipe is connected to a porous aeration head 304 .

[0042] The porous aeration head 304 accelerates the absorption rate of hydrogen sulfide by sodium hydroxide, thereby speeding up the detection speed.

[0043] The volume of the hydrochloric acid solution injected into the acidification reagent bottle 103 is controlled by the cooperation of the acidification syringe 101 and the injection valve 102, and the sealing of the sodium hydroxide solution and the hydrogen sulfide gas during the reaction is ensured by the sampling valve 305 to ensure the accuracy of the detection result.

[0044] In some embodiments, a USB wire 203 is connected to the diaphragm pump 202 .

[0045] The USB wire 203 is used to improve the portability of the gas generating part 1, the reflux part 2 and the absorption part 3. After sampling the sample in the field, it can be immediately placed in the gas generating part 1. The gas in the gas generating part 1 enters the absorption part 3 under the action of the diaphragm pump 202, so that the absorption part 3 absorbs the hydrogen sulfide gas, thereby ensuring the accuracy of the test results.

[0046] In some embodiments, an anti-back-inhalation airbag 301 is connected to the output tube.

[0047] The anti-backflow airbag 301 prevents the material in the alkali solution absorption bottle 303 from flowing back due to the pressure difference, thereby avoiding contamination of the sample.

[0048] In some embodiments, the air outlet pipe and the output pipe, the air guide pipe and the return pipe 201 , the diaphragm pump 202 and the return pipe 201 , the diaphragm pump 202 and the delivery pipe 205 , the delivery pipe 205 and the exhaust pipe, and the air inlet pipe and the output pipe are all connected by a connecting hose 104 .

[0049] The sealing of the detection device is ensured by connecting the hose 104, so that the hydrogen sulfide gas will not leak during the circulation process.

[0050] In this specification, each embodiment is described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the embodiments can be referred to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant parts can be referred to the method part.

[0051] The above description of the disclosed embodiments enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A detection device for detecting the content of volatile sulfide in a solid sample or hydrogen sulfide in a gas, characterized in that: include: A gas generating part, wherein an output end of the gas generating part is connected to an output pipe; The absorption part comprises an alkali solution absorption bottle, wherein the alkali solution absorption bottle is a three-way reagent bottle, wherein one end of the output pipe away from the gas generating part is connected to the air inlet pipe of the alkali solution absorption bottle, and the alkali solution absorption bottle is also connected to an exhaust pipe and a drain pipe, through which the liquid in the alkali solution absorption bottle is discharged; A reflux unit, comprising a diaphragm pump, wherein the input end of the diaphragm pump is connected to the exhaust pipe via a delivery pipe, the output end of the diaphragm pump is connected to a reflux pipe, and one end of the reflux pipe away from the diaphragm pump is connected to the input end of the gas generating unit; The detection part includes a spectrophotometer, which detects the sulfide ion concentration of the liquid in the alkali solution absorption bottle by using the spectrophotometer.

2. The detection device according to claim 1, characterized in that: When used to detect the content of volatile sulfides in a solid sample, the gas generating part includes an acidifying reagent bottle, which is a three-way reagent bottle. The acidifying reagent bottle is connected with a liquid inlet pipe, an air outlet pipe and an air guide pipe. The end of the air outlet pipe away from the acidifying reagent bottle is connected to the output pipe, and the end of the air guide pipe away from the acidifying reagent bottle is connected to the reflux pipe. Hydrochloric acid solution is introduced into the acidifying reagent bottle through the liquid inlet pipe.

3. The detection device according to claim 1, characterized in that: When used to detect the content of hydrogen sulfide in gas, the gas generating part includes a gas collecting bag, and the gas collecting bag is provided with a gas inlet and a gas outlet. The gas inlet is connected to the reflux pipe, and the gas outlet is connected to the output pipe.

4. The detection device according to claim 1, characterized in that: The air inlet pipe extends into the bottom end of the alkali solution absorption bottle, and one end of the air inlet pipe away from the output pipe is connected to a porous aeration head.

5. The detection device according to claim 2, characterized in that: One end of the liquid inlet tube away from the acidifying reagent bottle is connected with an acidifying syringe.

6. The detection device according to claim 2, characterized in that: The liquid inlet pipe and the liquid discharge pipe are respectively provided with an injection valve and a sampling valve.

7. The detection device according to claim 1, characterized in that: The diaphragm pump is connected with a USB wire.

8. The detection device according to claim 1, characterized in that: The output pipe is connected with an anti-backflow air bag.

Citation Information

Patent Citations

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