A sulfide content analyzer

By designing a sulfide content analyzer that includes a separator, an electromagnetic stirrer, and lead acetate paper, the problem of low accuracy in sulfide content measurement in existing technologies has been solved, and uniform stirring of sample solutions and rapid qualitative and quantitative detection have been achieved.

CN224518553UActive Publication Date: 2026-07-17QINGDAO CHUANGMENG INSTR CO LTD

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
QINGDAO CHUANGMENG INSTR CO LTD
Filing Date
2025-07-25
Publication Date
2026-07-17

AI Technical Summary

Technical Problem

Existing methods for measuring sulfide content have poor reproducibility, low sensitivity, complex operation, and are not suitable for low-concentration samples, resulting in low measurement accuracy.

Method used

A sulfide content analyzer is used, which includes a separator, an electromagnetic stirrer, a magnetic stirring rod, lead acetate paper, and a flow meter. The sample solution is stirred by the electromagnetic stirrer, and black lead sulfide is generated by the reaction of lead acetate paper for qualitative detection. Quantitative analysis is performed in conjunction with the flow meter.

Benefits of technology

It achieves uniform stirring of the sample solution, improves the accuracy and sensitivity of the measurement, and is suitable for rapid qualitative and quantitative detection of low-concentration sulfides.

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Abstract

This utility model relates to the field of analytical reducing agent content technology, and discloses a sulfide content analyzer, including a separator. The separator has a top cover, an adjustment component on one side, a first chamber extending through one side of the top, a second chamber extending through the middle of the top, and a third chamber extending through the other side of the top. A first orifice is extending through one end of the top, and a second orifice is extending through one end of one side of the top. A flow meter is slidably connected to the inner wall of the first orifice. In this utility model, by first installing an electromagnetic stirrer and a magnetic stirring rod at the bottom of the separator, the sample solution can be uniformly stirred, accelerating the chemical reaction between the sulfide and the reagent, thus solving the measurement error problem caused by incomplete reaction in traditional methods.
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Description

Technical Field

[0001] This utility model relates to the field of analytical reducing agent content technology, and in particular to a sulfide content analyzer. Background Technology

[0002] During oilfield development, sulfides are present to varying degrees in surface crude oil gathering and transportation systems, wastewater treatment systems, and reinjection systems. Their sources are primarily twofold: first, the injection of various drilling fluids and fracturing fluids introduces sulfur-containing compounds into the formation, which then enters the surface system along with the produced fluids; second, during crude oil extraction and transportation, in anaerobic environments such as oil gathering pipelines, storage tanks, and pressure vessels, plasma in the transport fluids is reduced to low-valence sulfur by sulfate-reducing bacteria, which then combines with certain cations in the mobile phase to form sulfides, such as ferrous sulfide. These sulfides exist in charged colloidal form, which can lead to instability in the crude oil electrostatic dehydration system, frequently causing "electric field collapse" in the dehydrator and affecting normal safe production; furthermore, it increases the difficulty of wastewater treatment and oily wastewater recovery, deteriorating the quality of treated oily wastewater and causing formation blockage during reinjection.

[0003] Currently, the existing publicly available technologies for measuring sulfide content are mainly aimed at wastewater systems. The methods include methylene blue spectrophotometry, chemical colorimetry, and atomic absorption spectrometry. These methods are characterized by poor reproducibility, low sensitivity, expensive instruments, complicated operation, and limited application.

[0004] The petroleum and environmental protection industries commonly use the standardized method of iodometric titration (HJ / T60-2000). This method uses acidification and blowing to separate hydrogen sulfide gas, which is then absorbed by ZnAc2-NaAc solution. Under acidic conditions, the generated sulfide reacts with excess iodine, and the remaining iodine is titrated with sodium thiosulfate standard solution using starch as an indicator. The separation process is time-consuming, and the manual titration and color development operations are complex and prone to errors. The accuracy of the results is not high, and it is not suitable for testing samples with low sulfide content (≤5mg / L). Utility Model Content

[0005] The purpose of this invention is to provide a sulfide content analyzer that solves the problem of low accuracy in the prior art.

[0006] To achieve the above objectives, this utility model provides the following technical solution: a sulfide content analyzer, comprising a separator, a top cover provided on the top of the separator, an adjustment component provided on one side of the separator, a first chamber extending through and opening on one side of the top of the separator, a second chamber extending through and opening in the middle of the top of the separator, a third chamber extending through and opening on the other side of the top of the separator, a first orifice seat extending through and opening at one end of the top of the separator, a second orifice seat extending through and opening at one end of one side of the top of the separator, a flow meter slidably connected to the inner wall of the first orifice seat, a dispersion tube extending through and slidably connected to one end of one side of the top cover, and a sealing cap slidably connected to the top of the dispersion tube.

[0007] By adopting the above technical solution, the flow meter should preferably be a float type, capable of measuring carrier gas flows between 200 and 400 cubic centimeters per minute. The syringe and injection tube must be made of glass or plastic that is non-reactive to sulfides and oil slurries.

[0008] As a further description of the above technical solution: the adjustment component includes an adjuster, one side of which is connected to one side of the separator, and the other side of the adjuster is threaded with evenly distributed bolts, which are threaded with the separator, and the top of the adjuster is provided with an adjustment tube.

[0009] Precise control of gas flow and pressure can be achieved by setting up regulators, bolts, and regulating pipes. The bolts are evenly distributed and pass through the regulator and separator, and the threaded connection ensures the regulating assembly is securely installed, preventing gas leakage.

[0010] As a further description of the above technical solution: a pressure reducer is provided on one side of the regulator, and a first connecting pipe is provided on one side of the pressure reducer.

[0011] By adopting the above technical solution, by installing a pressure reducer on one side of the regulator and connecting it to the first connecting pipe, the high-pressure gas of the gas source (such as CO2) can be reduced to a low-pressure state suitable for the system, preventing the high-pressure airflow from impacting and causing liquid splashing in the separator or abnormal flow meter readings.

[0012] As a further description of the above technical solution: an electromagnetic stirrer is provided at the bottom of the separator, and a magnetic stirring rod is provided at one end of the top of the electromagnetic stirrer.

[0013] By adopting the above technical solution, the electromagnetic stirrer at the bottom of the separator, together with the magnetic stirring rod at the top, can drive the stirring rod to rotate through electromagnetic induction, so as to uniformly mix the sample solution and reagents (such as deionized water and defoamer) in the separator.

[0014] As a further description of the above technical solution: the top outer side of the top cover is threaded with evenly distributed screws, and the screws are threaded with the separator.

[0015] By adopting the above technical solution, the outer side of the top cover is connected to the separator by evenly distributed screws, forming a tight sealing structure.

[0016] As a further description of the above technical solution: a second connecting pipe is provided through the first chamber and the second chamber, and a third connecting pipe is provided between the second chamber and the first hole seat.

[0017] By adopting the above technical solution, the second connecting pipe between the first chamber and the second chamber, and the third connecting pipe between the second chamber and the first orifice, constitute a complete gas flow path.

[0018] As a further description of the above technical solution: nylon tube retainers are threaded through and connected to both sides of the top center of the top cover, and a test tube is provided on the inner wall of the nylon tube retainer.

[0019] By adopting the above technical solution, the nylon tube retainers on both sides of the top of the cover can securely hold the test tube, which usually contains a test reagent (such as a solution that absorbs hydrogen sulfide).

[0020] As a further description of the above technical solution: lead acetate paper is provided on one side of the bottom inner wall of the top cover.

[0021] By adopting the above technical solution, when the lead acetate paper on the inner wall of the bottom of the top cover comes into contact with hydrogen sulfide gas, a chemical reaction will occur to generate black lead sulfide, thus visually indicating whether there are sulfides in the system.

[0022] Compared with the prior art, the beneficial effects of this utility model are as follows:

[0023] 1. The sulfide content analyzer provided by this utility model firstly uses an electromagnetic stirrer and a magnetic stirring rod at the bottom of the separator to uniformly stir the sample solution, accelerate the chemical reaction between sulfides and reagents, and solve the measurement error problem caused by insufficient reaction in traditional methods.

[0024] 2. The sulfide content analyzer provided by this utility model achieves rapid qualitative detection of sulfides by placing lead acetate paper on the inner wall of the bottom of the top cover and utilizing the property that hydrogen sulfide reacts with lead acetate to generate black lead sulfide; at the same time, the test tube is installed by a nylon tube holder and quantitative analysis is carried out in combination with gas flow control. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of the overall structure of this utility model;

[0026] Figure 2 This is a schematic diagram of the gas separator of this utility model;

[0027] Figure 3 This is a schematic diagram of the separator of this utility model;

[0028] Figure 4 This is a schematic diagram of the top cover of this utility model;

[0029] Figure 5 This is a schematic diagram of the dispersion tube of this utility model.

[0030] Legend:

[0031] 1. Electromagnetic stirrer; 2. Magnetic stirring rod; 3. Separator; 4. Top cover; 5. Screw; 6. Pressure reducer; 7. Nylon tube holder; 8. Test tube; 9. Regulator; 10. Regulating tube; 11. Bolt; 12. First chamber; 13. Second chamber; 14. Third chamber; 15. First orifice seat; 16. Second orifice seat; 17. Dispersion tube; 18. Sealing cap; 19. Lead acetate paper; 20. Flow meter; 21. First connecting tube; 22. Second connecting tube; 23. Third connecting tube. Detailed Implementation

[0032] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0033] To further understand the content of this utility model, a detailed description of this utility model will be provided in conjunction with the accompanying drawings.

[0034] Combination Figure 1 and Figure 4 The present invention provides a sulfide content analyzer, comprising a separator 3, a top cover 4 on the top of the separator 3, an adjustment component on one side of the separator 3, an electromagnetic stirrer 1 at the bottom of the separator 3, a magnetic stirring rod 2 at one top end of the electromagnetic stirrer 1, nylon tube retainers 7 threadedly connected to both sides of the top middle of the top cover 4, a test tube 8 on the inner wall of the nylon tube retainer 7, and lead acetate paper 19 on one side of the bottom inner wall of the top cover 4.

[0035] Place the magnetic stirring rod into the first chamber 12. Assemble the gas separator for routine sulfur gas testing. Place the gas separator on the electromagnetic stirrer 1. Open both ends of the test tube and insert it into the port next to the third chamber 14, pointing downwards as indicated by the arrow. Ensure the arrow on the tube points downwards and the test tube is sealed. Insert the sample injection tube through the rubber stopper at the top of the first chamber 12, ensuring a seal. Add 20 ml of a mixture of 2M citric acid demulsifier and isopropanol into the first chamber 12. Add 10 drops of octanol defoamer to the first chamber 12. Operate the magnetic stirrer 1 at a medium speed. Carefully place the dispersion tube 17 into the circulating liquid until it is just above the magnetic stirring rod 2. Slowly inject the correct volume of sample using a syringe, allowing it to mix into the vortex of the stirring rod. Stir for at least 2 minutes. Immediately start the CO2 gas source and adjust the flow rate so that the bulb in the flow meter 20 remains between the two lines. (A CO2 gas cartridge at this rate can provide a flow rate of approximately 15 to 20 minutes.) Observe the changes in the appearance of the test tube. Record the maximum length of the brown (black) color before the "feather-like" or "spot-like" appearance. Continue injecting gas for 15 minutes. Although color diffusion or feather-like hues may appear at the front, in the case of a high-range test tube, orange-yellow spots caused by SO2 (from sulfates in the mud) may appear before the brown (black) color appears. If sulfides are present in the sample, the orange-yellow SO2 area should be ignored when recording the brown (black) length. To achieve the highest accuracy of the test tube, the brown (black) length should be greater than half the total length of the test tube, so the filtrate sample volume must be carefully selected.

[0036] Combination Figure 1 and Figure 2 The adjustment assembly includes an adjuster 9, one side of which is connected to one side of the separator 3. The other side of the adjuster 9 is threaded with evenly distributed bolts 11, which are threaded through and connected to the separator 3. An adjustment tube 10 is provided through and installed on the top of the adjuster 9. A pressure reducer 6 is provided on one side of the adjuster 9. A first connecting tube 21 is provided on one side of the pressure reducer 6. A screw 5 is threaded through and connected to the outer side of the top of the top cover 4, which is threaded through and connected to the separator 3.

[0037] The regulator 9 is fixedly connected to the side of the separator 3 by bolts 11, and a regulating pipe 10 is installed through the top to control the gas input flow rate and pressure. The bolts 11 are evenly distributed and pass through the regulator 9 and the separator 3, and the threaded connection achieves a stable installation, ensuring that the components will not loosen during gas regulation.

[0038] Combination Figures 3-5A first chamber 12 is provided through one side of the top of the separator 3, a second chamber 13 is provided through the middle of the top of the separator 3, a third chamber 14 is provided through the other side of the top of the separator 3, a first orifice 15 is provided through one end of the top of the separator 3, a second orifice 16 is provided through one end of one side of the top of the separator 3, a flow meter 20 is slidably connected to the inner wall of the first orifice 15, a dispersion tube 17 is provided through one end of one side of the top of the top cover 4, and a sealing cover 18 is slidably connected to the top of the dispersion tube 17.

[0039] The gas is evenly dispersed into the first chamber 12 through the dispersion tube 17, reacts with the sample solution to generate hydrogen sulfide, flows through the second connecting tube 22 and the third connecting tube 23 through the flow meter 20, and is finally discharged from the third chamber 14. The flow meter 20 monitors the flow rate in real time, and the lead acetate paper 19 detects the gas composition simultaneously to ensure the accuracy of the measurement data.

[0040] Working Principle: Before use, ensure the gas separator 3 is dry and clean to prevent moisture inside the separator 3 from causing the flow meter 20 to float irregularly, affecting the accuracy of the test tube 8 reading. Place the separator 3 on a horizontal surface, remove the top cover 4, add 20ml of deionized water to the first chamber 12 as the reaction medium, and add octyl defoamer to eliminate foam interference. Then insert the flow meter 20 into the socket between the second chamber 13 and the third chamber 14, and seal evenly with an O-ring to prevent gas leakage. Next, place the dispersion tube 17 into the first chamber 12, insert the O-ring into the hole in the cover of the first chamber 12, and use the nylon tube retainer 7 to screw into the cover to secure the O-ring. Carefully close the cover and clamp the nylon tube retainer 7. Adjust the perforated plate to approximately 5mm above the bottom of the chamber to ensure even gas dispersion. Afterwards, tighten all the screws 5 on the sealing rings evenly by hand to form a sealed system. Then loosen the T-type screw of the pressure reducer 6 and connect it to the gas source (CO2 for sulfide analysis, N2O for carbonate analysis) 4. Connect the regulator 9 to the dispersion tube 17 with a rubber hose, and connect the other rubber hoses to the nylon device of the third chamber 14. Then tighten the T-type screw of the pressure reducer 6 and let the gas flow slowly through the system for 30 seconds to purge the remaining air and check for leaks. After shutting off the airflow, stir the liquid with the electromagnetic stirrer 1 at the bottom of the separator 3 and the magnetic stirring rod 2 at the top to accelerate the sulfide reaction. The lead acetate paper 19 on the bottom inner wall of the top cover 4 reacts with the generated hydrogen sulfide to produce a color. The flow meter 20 monitors the gas flow rate. The test tube 8 is connected to the test tube 8 in the nylon tube holder 7 to take a reading, thereby realizing the determination of sulfide content.

[0041] Finally, it should be noted that the above description is only a preferred embodiment of the present utility model and is not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. A sulphur content meter comprising a separator (3), characterised in that: The separator (3) is provided with a top cover (4) on its top, and an adjustment component is provided on one side of the separator (3). A first chamber (12) is provided through one side of the top of the separator (3). A second chamber (13) is provided through the middle of the top of the separator (3). A third chamber (14) is provided through the other side of the top of the separator (3). A first hole seat (15) is provided through one end of the top of the separator (3). A second hole seat (16) is provided through one end of one side of the top of the separator (3). A flow meter (20) is slidably connected to the inner wall of the first hole seat (15). A dispersion tube (17) is slidably connected through one end of one side of the top of the top cover (4). A sealing cover (18) is slidably connected to the top of the dispersion tube (17).

2. The sulfide content analyzer according to claim 1, characterized in that: The adjustment assembly includes an adjuster (9), one side of which is connected to one side of the separator (3), and the other side of the adjuster (9) is threaded with evenly distributed bolts (11), which are threaded with the separator (3). The top of the adjuster (9) is provided with an adjustment tube (10).

3. A sulphur content meter as claimed in claim 2, wherein: A pressure reducer (6) is provided on one side of the regulator (9), and a first connecting pipe (21) is provided on one side of the pressure reducer (6).

4. A sulphur content meter as claimed in claim 1, wherein: The separator (3) is equipped with an electromagnetic stirrer (1) at the bottom, and a magnetic stirring rod (2) is provided at one end of the top of the electromagnetic stirrer (1).

5. A sulphur content meter as claimed in claim 1, wherein: The top outer side of the top cover (4) is threaded with evenly distributed screws (5), and the screws (5) are threaded with the separator (3).

6. A sulphur content meter as claimed in claim 1, wherein: A second connecting pipe (22) is provided between the first chamber (12) and the second chamber (13), and a third connecting pipe (23) is provided between the second chamber (13) and the first hole seat (15).

7. A sulphur content meter as claimed in claim 1, wherein: The top cover (4) has nylon tube retainers (7) threaded through and connected to both sides of the top middle. The inner wall of the nylon tube retainer (7) is provided with a test tube (8).

8. A sulphur content meter as claimed in claim 1, wherein: Lead acetate paper (19) is provided on one side of the bottom inner wall of the top cover (4).