Method for detecting loading capacity of liquid-phase gas

By calculating the gas volume in a sealed reaction vessel and combining automatic sampling with correction coefficient calibration, the accuracy and anti-interference issues of liquid phase gas load detection are solved, achieving fully automated online measurement and high-precision detection.

CN120847336APending Publication Date: 2025-10-28GECARBON ZHIHE (BEIJING) TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202510975972.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-15
Publication Date
2025-10-28

AI Technical Summary

Technical Problem

Existing methods for detecting liquid phase gas loading are cumbersome to operate, cannot provide real-time feedback, and suffer from insufficient accuracy and poor anti-interference capabilities.

Method used

The liquid sample and the reaction liquid are fully reacted in a sealed reaction vessel. The gas quantity is calculated by fusing the ideal gas law and Henry's law into two models. Combined with automatic sample introduction and correction coefficient calibration, fully automatic online measurement is achieved.

Benefits of technology

It improves the accuracy and anti-interference ability of gas load detection, realizes fully automatic online measurement, and reduces human error and maintenance costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention provides a method for detecting the loading capacity of liquid-phase gas, which comprises the following steps: a reaction and data acquisition step: injecting a liquid-phase sample with a first volume V1 and a reaction liquid with a second volume V2 into a reaction container with a volume V, and fully reacting the liquid-phase sample with the reaction liquid to release gas under the condition of keeping the reaction container sealed, collecting the temperature T in the reaction container in the reaction process and the pressure P0 and P1 in the reaction container before the reaction is started and after the reaction is completed; calculating the amount of released gas: calculating the amount of substance of the released gas through double-model fusion of an ideal gas state equation and a Henry law according to the collected temperature T, pressure P0 and P1, the first volume V1, the second volume V2 and the volume V; and a gas loading capacity calculation step: calculating the gas loading capacity of the liquid phase sample according to the substance amount of the released gas, the first volume V1 and the effective component concentration of the liquid phase sample. And the accuracy and the anti-interference performance of gas loading capacity detection are improved.
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Description

Technical Field

[0001] This invention relates to the field of analytical measurement technology, and in particular to a method for detecting the gas loading in a liquid phase. Background Technology

[0002] Gas separation in chemical, medical, and environmental fields involves a large number of sample tests and analyses. These tests often involve numerous chemical reactions that generate gases. Rapid and accurate measurement of the gas load released during sample testing is crucial for technological development, real-time monitoring of industrial processes, and improvement of industrial production efficiency. Particularly in carbon capture technology, the CO2 loading of chemical absorbents is a critical indicator. The CO2 loading of liquid-phase CO2 absorbents (such as amine solutions like MEA) directly affects carbon capture efficiency.

[0003] Traditional acid-base titration methods for detecting CO2 loading require manual sampling and the addition of a strong acid (such as hydrochloric acid) to release CO2. The loading is indirectly calculated using gas volume or weight methods based on the principle of communicating vessels, which are cumbersome and lack real-time feedback. Existing online detection technologies such as conductivity and spectroscopy are susceptible to interference from absorbent degradation products and require complex calibration procedures. To address these issues, researchers have proposed a method for calculating gas loading based on pressure conversion; however, this method still requires manual sample introduction, cannot be used for online detection, and its accuracy and interference resistance remain insufficient.

[0004] Therefore, there is an urgent need to develop an automated online detection method based on classical chemical reactions that combines high accuracy with strong anti-interference capabilities. Summary of the Invention

[0005] In view of the above, the present invention proposes a method for detecting liquid phase gas loading that overcomes or at least partially solves the above problems.

[0006] One objective of this invention is to improve the accuracy and anti-interference capability of gas load detection.

[0007] Another objective of this invention is to achieve fully automated online measurement.

[0008] Specifically, the present invention provides a method for detecting liquid-phase gas loading, comprising:

[0009] Reaction and data acquisition steps: Inject the liquid sample of the first volume V1 and the reaction liquid of the second volume V2 into the reaction container of volume V. Under the condition of keeping the reaction container sealed, allow the liquid sample and the reaction liquid to react fully to release gas, and collect the temperature T in the reaction container during the reaction process, as well as the pressure P0 and P1 in the reaction container before the start of the reaction and after the reaction is completed.

[0010] Steps for calculating the amount of gas released: Based on the collected temperature T, pressure P0 and P1, and the first volume V1, second volume V2, and volume V, the amount of substance of the released gas is calculated using a dual-model fusion of the ideal gas law and Henry's law; and

[0011] Gas loading calculation steps: Calculate the gas loading of the liquid sample based on the amount of gas released, the first volume V1, and the effective component concentration of the liquid sample.

[0012] Optionally, the steps for calculating the amount of gas released specifically include:

[0013] Based on the collected temperatures T, pressures P0 and P1, and the first volume V1, the second volume V2, and the volume V, the amount of substance of the released gas is calculated according to the dual-model fusion formula (1) of the ideal gas law and Henry's law:

[0014]

[0015] Where n is the amount of substance of the gas released, in mol;

[0016] The units for V, V1, and V2 are L;

[0017] T represents temperature in degrees Celsius, expressed in °C.

[0018] The units for P0 and P1 are kPa;

[0019] H(T) is the Henry coefficient, H(T) = 0.034 × exp(2600(1 / (T+273.15)-1 / 298.15)) / 100, with units of mol / (L*kPa).

[0020] Optionally, the gas load calculation steps specifically include:

[0021] Based on the amount of gas released, the first volume V1, and the effective component concentration of the liquid sample, the gas molar loading of the liquid sample is calculated according to the following formula (2):

[0022]

[0023] And / or

[0024] Based on the amount of gas released and the first volume V1, the gas volume loading of the liquid sample is calculated according to the following formula (3):

[0025]

[0026] Where a is the gas molar loading of the liquid sample, in mol / mol of effective component; b is the gas volume loading of the liquid sample, in L / L of sample; n is the amount of gas released, in mol; c is the concentration of effective component of the liquid sample, in mol / L; Vm represents the gas molar volume under standard conditions, with a value of 22.4, in L / mol; and V1 is in L.

[0027] Optionally, before injecting the first volume V1 of liquid sample and the second volume V2 of reaction solution into the reaction vessel of volume V, the method further includes:

[0028] Calibration steps: Using at least one standard liquid sample with known effective component concentration and known gas load, follow the steps of reaction and data acquisition and gas release calculation to obtain the amount of gas released by at least one standard liquid sample. Based on the relationship between the amount of gas released by at least one standard liquid sample and its known gas load, determine a correction factor.

[0029] Following the gas loading calculation step, the method also includes:

[0030] Gas loading correction step: Correct the calculated gas loading of the liquid sample using a correction factor.

[0031] Optionally, a correction factor is determined based on the relationship between the amount of gas released by at least one standard liquid sample and its known gas loading, including:

[0032] The correction factor is calculated according to the following formula (4):

[0033]

[0034] Where, k is the correction coefficient; d represents the total number of standard liquid samples, d≥1; n1,…,nd represent the amount of gas released from the 1st to the dth standard liquid samples, in mol; L1,…,Ld represent the known gas loading of the 1st to the dth standard liquid samples, in mol / mol of effective component; c1,…,cd represent the effective component concentration of the 1st to the dth standard liquid samples, in mol / L; and V1 is in L.

[0035] Correcting the calculated gas loading of the liquid sample using correction factors includes:

[0036] The corrected gas loading is obtained by multiplying the calculated gas loading of the liquid sample by (2-k).

[0037] Optionally, prior to the reaction and data acquisition steps, the method further includes:

[0038] Cleaning steps: Inject the first preset volume of liquid sample and the second preset volume of reaction solution into the reaction vessel, allow the liquid sample to react with the reaction solution for a preset time, and then drain the solution from the reaction vessel.

[0039] Optionally, the liquid sample and reaction solution are automatically injected, and each step is automatically executed according to a set time sequence under the control of the central processing module.

[0040] Optionally, automated injection of liquid phase samples is achieved in the following ways:

[0041] The liquid sample is pumped into and fills the inner cavity of the piston injector by a liquid pump. The piston of the piston injector is controlled to move a set distance to inject a set amount of liquid sample from the piston injector into the reaction vessel.

[0042] Optionally, the reaction and data acquisition steps specifically include:

[0043] The second volume V2 of the reaction solution is injected into a reaction vessel with a volume of V;

[0044] Seal the reaction vessel and collect the pressure P0 inside the reaction vessel before the reaction begins;

[0045] A liquid sample of volume V1 is injected into the reaction vessel to allow the liquid sample to react fully with the reaction liquid to release gas.

[0046] The temperature T inside the reaction vessel during the reaction process and the pressure P1 inside the reaction vessel after the reaction is completed are collected.

[0047] Optionally, the gas is CO2, the liquid sample is an absorption solution containing a CO2 absorbent as an effective component, and the reaction solution is an acid solution that reacts with the CO2 absorbent.

[0048] The method for detecting liquid-phase gas loading provided by this invention allows the liquid sample to fully react with the reaction liquid while maintaining a sealed reaction vessel to release gas. This closed reaction avoids interference from ambient gases, and degradation products (such as thermally stable salts) do not participate in the gas release reaction, thus not affecting the detection results, thereby improving the anti-interference capability of gas loading detection. Furthermore, after collecting the temperature T inside the reaction vessel during the reaction process, and the pressures P0 and P1 inside the reaction vessel before and after the reaction, the amount of gas released is calculated using a dual-model fusion of the ideal gas law and Henry's law. This method greatly reduces the influence of gas dissolution in water and gas compression in a closed space on the gas quantity detection results, improving the accuracy of the detected amount of gas released in the reaction, thereby improving the precision of liquid-phase gas loading detection.

[0049] Furthermore, in the method for detecting the gas loading of a liquid phase provided by the present invention, before starting the measurement of the gas loading of the liquid phase sample, a standard liquid phase sample with a known gas loading is used for calibration. A correction coefficient is determined by the relationship between the amount of gas released by the standard liquid phase sample and the known gas loading. The calculated gas loading of the liquid phase sample is then corrected using the correction coefficient, thereby further improving the accuracy of the detection of the gas loading of the liquid phase.

[0050] Furthermore, in the method for detecting liquid-phase gas loading provided by this invention, the liquid sample and reaction solution are automatically introduced, and each step is automatically executed according to a set timing sequence under the control of the central processing module. This achieves fully automated online measurement, completely eliminating human error, and providing high stability and low maintenance.

[0051] Furthermore, in the method for detecting liquid phase gas loading provided by this invention, a liquid sample is first pumped into and fills the inner cavity of a piston-type sampler using a liquid pump. Then, the piston of the piston-type sampler is controlled to move a set distance to inject a set amount of liquid sample from the piston-type sampler into the reaction vessel, thereby achieving automatic injection of the liquid sample. This method overcomes the problems of unstable injection volume and large errors in general pumping methods (e.g., peristaltic pumps) when performing small-volume quantitative injections. It can accurately and stably inject small volumes, further improving the accuracy of liquid phase gas loading detection, and has a lower overall cost.

[0052] The above description is merely an overview of the technical solution of the present invention. In order to better understand the technical means of the present invention and to implement it in accordance with the contents of the specification, and in order to make the above and other objects, features and advantages of the present invention more apparent and understandable, specific embodiments of the present invention are described below.

[0053] The above and other objects, advantages and features of the present invention will become more apparent to those skilled in the art from the following detailed description of specific embodiments of the invention in conjunction with the accompanying drawings. Attached Figure Description

[0054] Various other advantages and benefits will become apparent to those skilled in the art upon reading the following detailed description of preferred embodiments. The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. The same reference numerals in the drawings denote the same or similar parts or components. Those skilled in the art should understand that these drawings are not necessarily drawn to scale. In the drawings:

[0055] Figure 1 This is a schematic flowchart of a method for detecting liquid phase gas loading according to an embodiment of the present invention;

[0056] Figure 2This is a schematic flowchart of a method for detecting liquid phase gas loading according to another embodiment of the present invention;

[0057] Figure 3 This is a schematic structural block diagram of a device for detecting liquid phase gas loading according to an embodiment of the present invention;

[0058] Figure 4 This is a schematic diagram of the external shape of a device for detecting liquid phase gas load according to an embodiment of the present invention;

[0059] Figure 5 This is a schematic diagram of a device for detecting liquid phase gas loading according to an embodiment of the present invention;

[0060] Figure 6a This is a front structural schematic diagram of the piston sampler of a device for detecting liquid phase gas loading according to an embodiment of the present invention.

[0061] Figure 6b yes Figure 6a A top view schematic diagram of the piston-type sampler shown;

[0062] Figure 6c yes Figure 6a The diagram shows a left-side view of the piston-type sampler. Detailed Implementation

[0063] Exemplary embodiments of the present disclosure will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.

[0064] To address the aforementioned problems, this invention proposes a method for detecting liquid-phase gas loading.

[0065] Figure 1 This is a schematic flowchart of a method for detecting liquid-phase gas loading according to an embodiment of the present invention. See also... Figure 1 As shown, the method for detecting liquid phase gas loading includes at least the following steps S102 to S106.

[0066] Step S102, reaction and data acquisition steps: Inject the liquid sample of the first volume V1 and the reaction liquid of the second volume V2 into the reaction container of volume V. Under the condition of keeping the reaction container sealed, allow the liquid sample and the reaction liquid to react fully to release gas, and collect the temperature T in the reaction container during the reaction process, as well as the pressure P0 and P1 in the reaction container before the start of the reaction and after the reaction is completed.

[0067] Step S104, calculation of the amount of gas released: Based on the collected temperature T, pressure P0 and P1, and the first volume V1, the second volume V2 and the volume V, the amount of substance of the gas released is calculated by fusing the ideal gas law and Henry's law into a dual model.

[0068] Step S106, Gas Load Calculation Step: Calculate the gas load of the liquid sample based on the amount of gas released, the first volume V1, and the effective component concentration of the liquid sample.

[0069] The method for detecting gas loading in liquid phase provided by the present invention allows the liquid sample to fully react with the reaction liquid to release gas while keeping the reaction container sealed. This avoids interference from ambient gas through a closed reaction, and the degradation products (such as thermally stable salts) do not participate in the reaction of the released gas and do not affect the detection results, thereby improving the anti-interference capability of gas loading detection.

[0070] Furthermore, the inventors of this application have innovatively recognized that existing methods for calculating gas load based on pressure conversion do not consider the influence of gas solubility in water and gas compression in a confined space on the detection results, resulting in insufficient accuracy. Therefore, the technical solution of this invention, after collecting the temperature T inside the reaction vessel during the reaction process, and the pressures P0 and P1 inside the reaction vessel before and after the reaction, calculates the amount of gas released by fusing a dual model of the ideal gas law and Henry's law. This method greatly reduces the influence of gas solubility in water and gas compression in a confined space on the gas quantity detection results, improves the accuracy of detecting the amount of gas released in the reaction, and thus improves the accuracy of liquid-phase gas load detection.

[0071] The active ingredient in a liquid sample refers to the component in the liquid sample that can react with CO2 to load the liquid sample with CO2. For example, in a CO2 absorbent, the active ingredient refers to the CO2 absorbent (such as an organic amine) in the absorbent solution.

[0072] The values ​​of V1 and V2 should be chosen to ensure that the liquid sample reacts fully with the reaction solution to completely release the gas. In some embodiments, V2 can be 3 to 25 times V1 to ensure complete gas release.

[0073] The volume V of the reaction vessel can be provided by the manufacturer, determined based on the geometric dimensions of the reaction vessel, or calibrated by injecting a known volume of air into the sealed reaction vessel. The method of calibrating the volume of the reaction vessel by injecting a known volume of air into the sealed reaction vessel has been described in detail in the prior art and will not be repeated here.

[0074] In some embodiments, the liquid sample is an absorption solution containing a CO2 absorbent as an active ingredient. The CO2 absorbent may be an organic amine, such as monoethanolamine (MEA). The released gas is CO2.

[0075] The reaction solution is an acid that can react with the CO2 absorbent, such as hydrochloric acid, sulfuric acid, nitric acid, etc., with sulfuric acid being preferred.

[0076] In practical applications, the concentration of the acid solution can be selected in the range of 0.5–6 mol / L, for example, 1, 2, 3, 4, 5, and 6 mol / L. Typically, a concentration of 2 mol / L is chosen.

[0077] In one specific embodiment, the reaction and data acquisition steps may include the following operations: First, a second volume V2 of reaction liquid is injected into a reaction vessel of volume V. Then, the reaction vessel is sealed, and the pressure P0 inside the reaction vessel before the reaction begins is collected. Next, a first volume V1 of liquid phase sample is injected into the reaction vessel to allow the liquid phase sample to fully react with the reaction liquid to release gas. After the reaction begins, the temperature T inside the reaction vessel during the reaction and the pressure P1 inside the reaction vessel after the reaction is completed are collected.

[0078] In some embodiments, temperature T and pressures P0 and P1 can be obtained by real-time monitoring of temperature and gas pressure changes inside the reaction vessel using temperature sensing elements and pressure sensing elements.

[0079] To ensure a complete reaction between the liquid sample and the reaction solution, the solution in the reaction vessel can be stirred during the reaction process. In one specific embodiment, stirring can begin after the reaction solution has been injected into the reaction vessel.

[0080] In some embodiments, the step of calculating the amount of gas released may specifically include:

[0081] Based on the collected temperatures T, pressures P0 and P1, and the first volume V1, the second volume V2, and the volume V, the amount of substance of the released gas is calculated according to the dual-model fusion formula (1) of the ideal gas law and Henry's law:

[0082]

[0083] Where n is the amount of substance of the gas released, in mol;

[0084] The units for V, V1, and V2 are L;

[0085] T represents temperature in degrees Celsius, expressed in °C.

[0086] The units for P0 and P1 are kPa;

[0087] H(T) is the Henry coefficient, H(T) = 0.034 × exp(2600(1 / (T+273.15)-1 / 298.15)) / 100, with units of mol / (L*kPa).

[0088] In formula (1) used in this embodiment, based on the calculation of the molar amount of gas using the ideal gas law in the first term, a second term is added to correct the error caused by the entry of a liquid sample of volume V1 into the reaction vessel. A third term is also added to correct the error caused by the Henry's law coefficient for the gas dissolved in water. This improves the accuracy of the detected amount of gas released from the reaction.

[0089] In some embodiments, the calculated gas molar loading of the liquid sample is obtained. Accordingly, the gas loading calculation step may specifically include:

[0090] Based on the amount of gas released, the first volume V1, and the effective component concentration of the liquid sample, the gas molar loading of the liquid sample is calculated according to the following formula (2):

[0091]

[0092] Where a is the gas molar loading of the liquid sample, in mol / mol of effective component; n is the amount of gas released, in mol; c is the concentration of the effective component of the liquid sample, in mol / L; and V1 is in L.

[0093] In other embodiments, the calculated gas volume loading of the liquid sample is the gas volume loading. Accordingly, the gas loading calculation step may specifically include:

[0094] Based on the amount of gas released and the first volume V1, the gas volume loading of the liquid sample is calculated according to the following formula (3):

[0095]

[0096] Where b is the gas volume loading of the liquid sample, in L / L sample; n is the amount of gas released, in mol; Vm represents the gas molar volume under standard conditions, with a value of 22.4, in L / mol; and V1 is in L.

[0097] In some other embodiments, the gas molar loading and gas volumetric loading of the liquid sample can also be calculated simultaneously.

[0098] In some embodiments, after calculating the gas molar loading and / or gas volumetric loading of the liquid sample, the obtained gas molar loading and / or gas volumetric loading of the liquid sample can also be displayed.

[0099] In some embodiments, the collected temperature T and pressures P0 and P1 can also be displayed so that users can better understand the detection process and situation.

[0100] Figure 2 This is a schematic flowchart of a method for detecting liquid phase gas loading according to another embodiment of the present invention, wherein steps S206, S208 and S210 are the same as steps S102, S104 and S106, respectively, and will not be repeated here.

[0101] See Figure 2 As shown, in some embodiments, the method for detecting the liquid phase gas load may further include a calibration step S202 before injecting the liquid phase sample of the first volume V1 and the reaction liquid of the second volume V2 into a reaction vessel of volume V.

[0102] The calibration steps may include: using at least one standard liquid sample with a known effective component concentration and a known gas load, following the steps of reaction and data acquisition and the step of calculating the amount of gas released, obtaining the amount of gas released by the at least one standard liquid sample, and determining a correction factor based on the relationship between the amount of gas released by the at least one standard liquid sample and its known gas load.

[0103] Specifically, a correction factor is obtained by taking a weighted average of the amount of gas released by the at least one standard liquid sample relative to the known effective component concentration and the known gas load of the at least one standard liquid sample.

[0104] Accordingly, after the gas loading calculation step, the method for detecting the gas loading of the liquid phase may also include a gas loading correction step S212: correcting the calculated gas loading of the liquid phase sample using a correction coefficient.

[0105] In this embodiment of the invention, before measuring the gas load of the liquid sample, a standard liquid sample with a known gas load is used for calibration. A correction coefficient is determined by the relationship between the amount of gas released by the standard liquid sample and the known gas load. The calculated gas load of the liquid sample is then corrected using the correction coefficient, thereby further improving the accuracy of the liquid gas load detection.

[0106] In some specific embodiments, determining a correction factor based on the relationship between the amount of gas released by the at least one standard liquid sample and its known gas loading includes:

[0107] The correction factor is calculated according to the following formula (4):

[0108]

[0109] Where, k is the correction coefficient; d represents the total number of standard liquid samples, d≥1; n1,…,nd represent the amount of gas released from the 1st to the dth standard liquid samples, in mol; L1,…,Ld represent the known gas loading of the 1st to the dth standard liquid samples, in mol / mol of effective component; c1,…,cd represent the effective component concentration of the 1st to the dth standard liquid samples, in mol / L; and V1 is in L.

[0110] In one specific embodiment, the number of standard liquid phase samples is 3, and the known loading of each standard liquid phase sample is 1 mol / mol of active ingredient. In this case, the formula for calculating the correction factor can be simplified to:

[0111]

[0112] Where k is the correction coefficient; n1, n2, and n3 represent the amount of gas released by the three standard liquid phase samples, in mol; c1, c2, and c3 represent the effective component concentrations of the three standard liquid phase samples, in mol / L; and V1 is in L.

[0113] The composition of the standard liquid sample can be the same as or different from that of the liquid sample to be measured.

[0114] For example, in some embodiments, a potassium carbonate solution with a known gas loading (such as CO2 loading) and a known potassium carbonate concentration can be used as a standard liquid phase sample.

[0115] In some embodiments, correcting the calculated gas load of the liquid sample using a correction factor includes multiplying the calculated gas load of the liquid sample by (2-k) to obtain the corrected gas load.

[0116] When the value of k is greater than 1, it indicates that the measured gas release is greater than the actual amount of gas that should be released; that is, the measured gas load will be greater than the actual gas load. By multiplying the calculated gas load of the liquid sample by (2-k) (which is less than 1), the measured value of the gas load can be regressed to be closer to the true value.

[0117] Similarly, when the value of k is less than 1, it indicates that the measured amount of gas released is less than the actual amount of gas that should be released; that is, the measured gas load will be less than the actual gas load. By multiplying the calculated gas load of the liquid sample by (2-k) (which has a value greater than 1), the measured value of the gas load can be made closer to the true value.

[0118] Continue to see Figure 2 In some embodiments, prior to the reaction and data acquisition steps, the method for detecting the liquid phase gas load may further include a cleaning step S204: injecting a first preset volume of liquid phase sample and a second preset volume of reaction liquid into a reaction container, allowing the liquid phase sample to react with the reaction liquid for a preset time, and then draining the solution from the reaction container.

[0119] To promote the reaction between the liquid sample and the reaction solution, stirring can be performed during the reaction.

[0120] The values ​​of the first preset volume and the second preset volume are preferably such that the injected liquid sample reacts completely with the reaction solution. In some embodiments, the second preset volume may be equal to the second volume V2 to simplify the control of the reaction solution injection operation.

[0121] The cleaning process helps to remove residual liquids and gases from the reaction vessel and the pipes connected to it, thereby improving the accuracy of the detection.

[0122] In particular, performing a cleaning step after the calibration step and before the reaction and data acquisition steps can remove as much of the residual standard liquid sample as possible from the reaction vessel and the pipes connected to the reaction vessel.

[0123] In some embodiments, in the method for detecting liquid phase gas loading of the present invention, the liquid phase sample and the reaction solution are automatically injected.

[0124] Furthermore, each step is executed automatically according to a set timing sequence under the control of the central processing module 110.

[0125] This enables fully automated online measurement, completely eliminating human error and providing high stability and low maintenance.

[0126] In some further embodiments, automated injection of liquid phase samples can be achieved by combining a liquid pump and a piston-type precision sampler 7.

[0127] Specifically, the liquid sample is first pumped into and fills the inner cavity of the piston injector 7 by a liquid pump. Then, the piston of the piston injector 7 is controlled to move a set distance to inject a set amount of liquid sample from the piston injector 7 into the reaction vessel.

[0128] The liquid pump can be any commonly used liquid pump, such as a peristaltic pump.

[0129] Traditional peristaltic pump injection methods, due to the presence of pulses, suffer from unstable injection volumes and significant errors when performing small quantitative doses (e.g., 0.1–1 mL). In contrast, the combination of a liquid pump and a piston-type precision injector 7 in this embodiment eliminates pulses, enabling accurate and stable quantitative injection of small volumes, further improving the accuracy of liquid-phase gas loading detection. Moreover, it offers lower overall cost compared to high-precision plunger pumps.

[0130] In some embodiments, the liquid sample (including the liquid sample to be tested and the standard liquid sample) may be filtered to remove particulate matter before being injected into the reaction vessel (specifically, before being pumped into the piston injector 7 by a liquid pump). Filtration may be achieved through a single-stage or multi-stage filtration unit. The filtration accuracy may be greater than 5 μm.

[0131] In some embodiments, the solution (mainly composed of reaction liquid) after the reaction in the cleaning step and the reaction and data acquisition step can be discharged into the reaction liquid unit 140 for collection and recycling. When the cumulative test amount of released gas (i.e., the cumulative amount of released gas detected) reaches the replacement condition, fresh reaction liquid is replaced for detection.

[0132] Specifically, when detecting the CO2 loading in a liquid sample, if the cumulative molar amount of released CO2 exceeds 1 / 10 to 1 / 2 of the total molar amount of hydrogen ions in the acid solution, the acid solution should be replaced with fresh acid solution.

[0133] In some embodiments, the solution after the reaction in the calibration step can also be discharged into the reaction solution unit 140 and eventually drained away.

[0134] In some embodiments, excess sample during the injection of the liquid phase sample to be measured can be recycled through the sample recycling module 191.

[0135] During the reaction, the temperature of the reaction vessel can be controlled to ensure suitable reaction and detection conditions.

[0136] Based on the same technical concept, the present invention also proposes a device 100 for detecting liquid-phase gas loading. This device 100 can be used to implement the method for detecting liquid-phase gas loading described in any of the foregoing embodiments or combinations thereof.

[0137] Figure 3 This is a schematic structural block diagram of a device 100 for detecting liquid phase gas load according to an embodiment of the present invention, wherein solid arrows indicate material flow and dashed arrows indicate signal flow. Figure 4 This is a schematic diagram of the external appearance of a device 100 for detecting liquid phase gas loading according to an embodiment of the present invention; Figure 5 This is a schematic diagram of the structure of a device 100 for detecting liquid-phase gas loading according to an embodiment of the present invention. The following is in conjunction with... Figures 3 to 5 The structure of the apparatus 100 for detecting liquid phase gas loading according to the present invention will be explained.

[0138] See Figure 3 As shown, in one embodiment, the apparatus 100 for detecting the liquid phase gas load generally includes a central processing module 110, a gas detection module 120, a precision sampling module 130, and a reaction liquid unit 140.

[0139] The gas detection module 120 includes a reaction vessel 12, and a temperature detection element 29 and a pressure detection element 30 for measuring the temperature and pressure values ​​inside the reaction vessel 12, respectively.

[0140] The precision sampling module 130 is used to inject a first volume V1 of liquid sample into the reaction vessel 12. The reaction liquid unit 140 is used to inject a second volume V2 of reaction liquid into the reaction vessel 12. The precision sampling module 130, the reaction liquid unit 140, and the gas detection module 120 work together to perform the reaction and data acquisition steps.

[0141] The central processing module 110 obtains the collected temperature T, pressure P0 and P1 from the gas detection module 120, and performs the gas release calculation step and the gas load calculation step accordingly.

[0142] In some embodiments, the apparatus 100 for detecting liquid-phase gas load may further include a temperature control unit 150 for temperature control of the entire apparatus 100, particularly the gas detection module 120. The temperature control unit 150 may be, for example, an electric heater (heating) and / or an air conditioner (cooling and heating).

[0143] In some embodiments, the apparatus 100 for detecting the liquid phase gas loading may further include a calibration unit 160. The calibration unit 160 can be used to provide a standard liquid phase sample to the precision sampling module 130, thereby implementing a calibration step. In the calibration step, a correction factor is determined by the central processing module 110. Accordingly, the central processing module 110 can implement a gas loading correction step.

[0144] In some embodiments, the precision sampling module 130, the reaction liquid unit 140, and the gas detection module 120 can also work together to implement the cleaning step.

[0145] In some embodiments, the solution (mainly composed of reaction liquid) after reaction in the gas detection module 120 can be discharged into the reaction liquid unit 140 for collection and recycling. When the cumulative test amount of released gas (i.e., the cumulative amount of released gas detected) reaches the replacement condition, the reaction liquid in the reaction liquid unit 140 is discharged as waste liquid and replaced with fresh reaction liquid for detection.

[0146] In some embodiments, the apparatus 100 for detecting the liquid phase gas load may further include a sample circulation module 191. Excess liquid phase sample in the precision sampling module 130 can be discharged to the sample circulation module 191 for recycling.

[0147] In some embodiments, the solution after the reaction in the calibration step can also be discharged into the reaction liquid unit 140 as calibration waste liquid and eventually disposed of.

[0148] In some embodiments, the apparatus 100 for detecting liquid phase gas loading may further include a filtration unit 27 for filtering the liquid phase sample (including the liquid phase sample to be tested and the standard liquid phase sample) to remove particulate matter before injecting the liquid phase sample (including the liquid phase sample to be tested and the standard liquid phase sample) into the reaction vessel 12.

[0149] In some embodiments, the apparatus 100 for detecting liquid phase gas load may further include a power supply unit 180 for supplying power to the electrical components in the apparatus 100.

[0150] In some embodiments, the apparatus 100 for detecting liquid-phase gas load may further include a central control system 190. After calculating the gas load, the central processing module 110 can transmit the calculated gas load and / or acquired data (such as temperature T, pressure P0 and P1) to the central control system 190 for display via analog / communication signals. The central control system 190 can also be used to input commands from external sources, such as detection commands.

[0151] The gas detection module 120, precision sampling module 130, temperature control unit 150, sample circulation module 191, reaction liquid unit 140, power supply unit 180 and central control system 190 can all be connected to the central processing module 110 for control and automatic operation according to the set timing and logic.

[0152] The following is for reference. Figure 5 The specific structure of the device 100 for detecting liquid phase gas load will be further explained.

[0153] In some embodiments, the reaction container 12 in the gas detection module 120 may be a closed reaction container 12. The closed reaction container 12 may be an internally controlled closed shell with a closed internal cavity and a sample inlet 16.

[0154] Temperature sensing element 29 and pressure sensing element 30 are arranged such that their sensing parts are connected to the internal cavity of the sealed reaction vessel 12, and are used to measure the temperature and pressure values ​​inside the sealed reaction vessel 12, respectively.

[0155] In some embodiments, the temperature sensing element 29 may be a temperature sensor.

[0156] In one specific embodiment, a first interface 17 can be opened on the top or side wall of the sealed reaction vessel 12, and the temperature sensor can be sealed and installed at the first interface 17.

[0157] In some embodiments, the pressure sensing element 30 may be a pressure sensor.

[0158] In one specific embodiment, a second interface 18 may be provided on the top or side wall of the sealed reaction vessel 12, and the second interface 18 is connected to a pressure sensor via a pipe.

[0159] The central processing module 110 includes a central processing unit 25. The central processing unit 25 is communicatively connected to the temperature sensing element 29 and the pressure sensing element 30, respectively, and is configured to acquire the temperature and pressure values ​​measured by the temperature sensing element 29 and the pressure sensing element 30, and calculate the gas load of the liquid sample based on the temperature and pressure values.

[0160] In some embodiments, the precision sampling module 130 includes a piston injector 7. The piston injector 7 has a sampling interface 73 and an injection interface 71 communicating with an injection port 16. The piston injector 7 is configured to acquire an input liquid sample through the sampling interface 73 and, through its piston, move a predetermined distance under controlled drive to inject a first predetermined amount (e.g., volume V1) of the liquid sample into the reaction vessel 12 via the injection interface 71 and the injection port 16. The injection interface 71 and the injection port 16 may be connected by a conduit.

[0161] In some embodiments, the precision sampling module 130 has a sampling port 1 and also includes a sample injection pump 9. The inlet of the sample injection pump 9 is connected to the sampling port 1, for example, via a pipe, and the outlet of the sample injection pump 9 is connected to the sampling interface 73 of the piston injector 7, for example, via a pipe. The sample injection pump 9 is configured to draw a liquid sample through the sampling port 1 and pump the liquid sample through the sampling interface 73 to fill the piston injector 7.

[0162] In some embodiments, the injection pump 9 may be a peristaltic pump.

[0163] Figure 6a This is a front structural schematic diagram of the piston-type sampler 7 of the apparatus 100 for detecting the gas loading in a liquid phase according to an embodiment of the present invention. Figure 6b yes Figure 6a The diagram shows a top view of the piston-type sampler 7. Figure 6c yes Figure 6a The diagram shows the left-side view of the piston-type sampler 7.

[0164] like Figures 6a to 6cAs shown, the piston-type injector 7 may include a hollow cylindrical injection housing 70 and a piston 8. A sampling port 73 and an injection port 71 are respectively located on the side and one end of the injection housing 70. The injection housing 70 also has a piston inlet 74 located at the other end opposite to the injection port 71. The piston 8 includes a piston disc and a piston rod fixedly connected to the piston disc. The piston disc is inserted into the inner cavity of the injection housing 70 through the piston inlet 74 and moved within the inner cavity of the injection housing 70 by the piston rod. Those skilled in the art will understand that the periphery of the piston disc is fluid-tightly fitted with the inner peripheral wall of the injection housing 70, thereby preventing liquid leakage.

[0165] In some further embodiments, the precision sampling module 130 may also include a slide 5 and a limiter 6. The slide 5 is connected to the piston rod. The limiter 6 is located in the direction of movement of the piston rod and is used to limit the termination position of the piston rod when it moves away from the injection housing 70.

[0166] The central processing module 110 may also include a first control unit 4. The first control unit 4 is communicatively connected to the slide 5 and is configured to drive the slide 5 to move the piston rod in response to a detection command, thereby causing the piston rod to move the piston disc within the cavity of the injection housing 70.

[0167] In some embodiments, the precision sampling module 130 further includes a discharge port 2 and may also include a discharge pump 10. The injection housing 70 also has a discharge interface 72 disposed on its side. The inlet of the discharge pump 10 is connected to the discharge interface 72, for example, via a pipe, and the outlet is connected to the discharge port 2, for example, via a pipe. The discharge pump 10 is used to draw liquid phase samples from the inner cavity of the injection housing 70 and discharge them through the discharge port 2.

[0168] In some embodiments, the sampling interface 73 and the discharge interface 72 are arranged sequentially from one end where the sample inlet interface 71 is located to the other end where the piston inlet 74 is located.

[0169] In practical applications, the injection housing 70 can be vertically positioned with the injection port 71 facing downwards. This allows the piston disc and piston rod to move vertically.

[0170] In some embodiments, the central processing module 110 may further include a second control unit 11, which is communicatively connected to the injection pump 9 and the discharge pump 10, respectively, and configured to control the operation of the injection pump 9 and the discharge pump 10. The second control unit 11 may be triggered based on a received instruction or may be triggered in other ways.

[0171] In one specific embodiment, the second control unit 11 can be triggered by the piston rod being moved by the slide table 5 to the limit switch 6 and stopped.

[0172] In some embodiments, each of the injection port 71, the sampling port 73, and the discharge port 72 has a neck formed between it and the inner cavity of the injection housing 70.

[0173] By forming a constriction between each interface and the inner cavity of the injection housing 70, the accuracy of liquid (especially micro-liquid) delivery can be improved, and liquid residue and waste can be reduced.

[0174] In some embodiments, the apparatus 100 may further include a filtration unit 27. The filtration unit 27 is disposed between the sampling port 1 and the injection pump 9 for filtering the extracted liquid phase sample.

[0175] The filter unit 27 can be a single-stage or multi-stage filter unit, and the filtration accuracy can be above 5μm.

[0176] In some embodiments, the reaction liquid output port of the reaction liquid unit 140 is connected to the internal cavity of the sealed reaction container 12, and is used to inject a second set amount (e.g., volume V2) of reaction liquid into the internal cavity of the sealed reaction container 12 so that the liquid sample reacts with the reaction liquid to release gas.

[0177] Specifically, a fourth interface 20 can be provided on the top or side wall of the sealed reaction vessel 12. The reaction liquid output port of the reaction liquid unit 140 can be connected to a pipe. By extending the pipe through the fourth interface 20 into the internal cavity of the sealed reaction vessel 12, the reaction liquid output port of the reaction liquid unit 140 can be connected to the internal cavity of the sealed reaction vessel 12. In a specific embodiment, the fourth interface 20 is provided on the top wall of the sealed reaction vessel 12.

[0178] In some embodiments, the reaction liquid unit 140 may include a reaction liquid container 24, an inlet pump 22, and an outlet pump 23.

[0179] The inlet and outlet of the feed pump 22 are connected to the interior of the reaction liquid container 24 and the interior cavity of the sealed reaction container 12, respectively. The feed pump 22 is used to pump a second set amount of reaction liquid from the reaction liquid container 24 into the interior cavity of the sealed reaction container 12. At this time, the outlet of the feed pump 22 serves as the reaction liquid output port of the reaction liquid unit 140.

[0180] Specifically, the inlet connection pipe of the liquid inlet pump 22 extends into the reaction liquid container 24 and is immersed in the reaction liquid.

[0181] The inlet and outlet of the discharge pump 23 are connected to the internal cavity of the sealed reaction vessel 12 and the interior of the reaction liquid container 24, respectively. The discharge pump 23 is used to discharge the solution in the internal cavity of the sealed reaction vessel 12 into the reaction liquid container 24.

[0182] In some embodiments, a drain port 15 may be provided at the bottom of the sealed reaction vessel 12, and the inlet of the drain pump 23 is connected to the drain port 15 via a pipe. The outlet of the drain pump 23 is connected to a pipe, and the outlet of the drain pump 23 is connected to the interior of the reaction vessel 24 by extending the end of the pipe connected to the outlet into the reaction liquid container 24.

[0183] In one specific embodiment, the bottom of the sealed reaction vessel 12 can be formed in the shape of a funnel, and the drain port 15 is located at the lowest point in the center of the bottom of the funnel shape, so as to ensure that the solution in the sealed reaction vessel 12 can be completely drained.

[0184] In some specific embodiments, the inlet pump 22 and / or the outlet pump 23 may be peristaltic pumps.

[0185] In some embodiments, both the inlet pump 22 and the outlet pump 23 are communicatively connected to the second control unit 11 to operate under the control of the second control unit 11.

[0186] In some embodiments, the apparatus 100 for detecting the liquid phase gas load may further include a sealing valve 21. The sealing valve 21 is in communication with the internal cavity of the sealed reaction vessel 12 and is connected to the second control unit 11, and is used to operate under the control of the second control unit 11 to seal or deseal the sealed reaction vessel 12.

[0187] In one specific embodiment, a third interface 19 may be opened on the top wall or side wall of the sealed reaction vessel 12, and the sealing valve 21 is connected to the third interface 19 through a pipe to communicate with the internal cavity of the sealed reaction vessel 12.

[0188] In some specific embodiments, the sealing valve 21 may be a solenoid valve.

[0189] Furthermore, the sealing valve 21 can be either a normally open or normally closed solenoid valve. When a normally open solenoid valve is used, it seals the reaction vessel 12 when controlled to open and unseals it when controlled to close. When a normally closed solenoid valve is used, it unseals the reaction vessel 12 when controlled to open and seals it when controlled to close.

[0190] In some embodiments, the apparatus 100 for detecting the liquid phase gas load may further include a stirring element 13. The stirring element 13 is disposed at the sealed reaction vessel 12 and is communicatively connected to the second control unit 11, and is used to operate under the control of the second control unit 11 to stir and mix the solution in the sealed reaction vessel 12.

[0191] The stirring element 13 can be a magnetic stirrer, a mechanical stirrer, or an oscillating stirrer (such as an ultrasonic transducer).

[0192] In some specific embodiments, the stirring element 13 is a magnetic stirrer, including a magnetic stirrer body 131 disposed at the bottom of the sealed reaction container 12 and a magnetic element 132 placed inside the sealed reaction container 12.

[0193] In some embodiments, the gas detection module 120, the reaction liquid unit 140, and the sealing valve 21 constitute a reaction system 200.

[0194] In some embodiments, the sealed reaction vessel 12 may include a reaction vessel body 121 and a protrusion 122 that protrudes upward from the top surface of the reaction vessel body 121 to form a cylindrical space inside the sealed reaction vessel 12. A pressure sensing element 30 is provided such that its sensing portion communicates with the cylindrical space inside the sealed reaction vessel 12. That is, a second interface 18 is provided on the protrusion 122.

[0195] The protrusion 122 can be located at any position on the top of the sealed reaction vessel 12. Preferably, the protrusion 122 is located at the center of the top of the sealed reaction vessel 12.

[0196] In this embodiment, the top region of the sealed reaction vessel 12 is extended by providing a protrusion 122 at the top, and the pressure detection element 30 is disposed on the protrusion 122. This prevents liquid from splashing onto the pressure detection element 30 during the reaction process (especially the stirring process), thereby improving detection accuracy. In particular, compared with the method of providing a baffle (partition) in the reaction vessel 12 to prevent liquid splashing, since the baffle essentially divides the reaction vessel 12 into upper and lower regions, the liquid is stirred and generated pressure in the sealed cavity during the stirring process. The presence of the baffle will aggravate this phenomenon and cause a large error. However, the solution of the present invention prevents liquid splashing by extending the top region of the sealed reaction vessel 12, thus avoiding increased error.

[0197] In some embodiments, the horizontal cross-section of the protrusion 122 and the horizontal cross-section of the reaction vessel body 121 are both circular. The diameter of the horizontal cross-section of the protrusion 122 is greater than or equal to 3 mm and less than or equal to 1 / 3 of the diameter of the horizontal cross-section of the reaction vessel body 121. By optimizing the ratio of the horizontal cross-sectional area of ​​the protrusion 122 to the horizontal cross-sectional area of ​​the reaction vessel body 121, it is possible to effectively prevent liquid splashing while ensuring uniform gas pressure balance within the reaction vessel 12.

[0198] In some embodiments, the ratio of the height of the protrusion 122 to the height of the reaction vessel body 121 is 0.1 to 1, for example, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, or 1.0. By optimizing the ratio of the height of the protrusion 122 to the height of the reaction vessel body 121, the overall height of the reaction vessel 12 can be reduced as much as possible while ensuring the effect of preventing liquid splashing, thereby reducing the size of the entire device 100.

[0199] In some embodiments, the apparatus 100 for detecting liquid phase gas load may further include a communication and display module 26, which is communicatively connected to the central processing module 110 and is used to display the data (such as temperature and pressure values) and / or calculation results (i.e., gas load) acquired by the central processing module 110.

[0200] Specifically, the communication and display module 26 is communicatively connected to the central processing unit 25. The central processing unit 25 sends the acquired data and / or calculation results to the communication and display module 26 for display.

[0201] The communication and display module 26 may be at least a part of the central control system 190.

[0202] In some embodiments, the apparatus 100 for detecting the liquid phase gas load may further include a switch signal transmitting module 3, which is communicatively connected to the central processing module 110. The switch signal transmitting module 3 may include, for example, a switch button.

[0203] Specifically, the switch signal transmitting module 3 can be communicatively connected to the first control unit 4.

[0204] The switch signal sending module 3 can also be part of the central control system 190.

[0205] In actual operation, the communication and display module 26 or the switch signal sending module 3 can send a detection command to the central processing module 110 (specifically the first control unit 4 and the central processing unit 25) to trigger the central processing module 110.

[0206] The communication connection mentioned in this article can be a wired connection (such as a connection via a wire) or a wireless connection.

[0207] The above describes various implementation methods of the method for detecting liquid phase gas load of the present invention and the structure of the apparatus 100 for detecting liquid phase gas load. The method and apparatus 100 for detecting liquid phase gas load of the present invention will be further described below through a specific embodiment.

[0208] Example 1

[0209] This embodiment is based on, as follows Figures 3 to 5The apparatus 100 shown implements a method for detecting liquid phase gas load.

[0210] In this embodiment, all hardware units in the device 100 are controlled by the central processing module 110. When a detection command is received, the central processing module 110 issues instructions, and all hardware operates according to logic. At the same time, it collects data signals during the test process, performs calculations and processing, obtains the gas load, and transmits it to the central control system 190.

[0211] In this embodiment, the liquid sample is a CO2 absorption solution containing organic amines as the active ingredient, and the reaction solution is an acid solution.

[0212] Specifically, the method for detecting liquid-phase gas loading includes the following steps:

[0213] (1) Before starting the measurement, the device 100 is calibrated using the calibration unit 160, precision sampling module 130, reaction liquid unit 140, gas detection module 120, and central processing module 110 to determine a calibration coefficient. The calibration waste liquid enters the reaction liquid unit 140 and is eventually discharged. The calibration method is as described above, wherein the central processing unit 25 calculates the calibration coefficient.

[0214] (2) Before liquid phase sample measurement, it passes through a single-stage / multi-stage filtration unit 27 to remove particulate matter, with a filtration accuracy of more than 5μm.

[0215] (3) The injection pump 9 draws the liquid sample into the piston injector 7. After the injection pump 9 operates continuously for a period of time, the piston injector 7 is filled with fresh liquid sample to be tested, and the excess sample is returned to its original position through the sample circulation module 191. Then, the piston injector 7 injects a first preset volume (which may not be equal to V1) of liquid sample into the reaction container 12 of volume V in the gas detection module 120. At the same time, the injection pump 22 draws a second preset volume (which may be equal to V2) of reaction liquid and injects it into the reaction container 12. After stirring, the solution in the reaction container 12 is discharged into the reaction liquid container 24 of the reaction liquid unit 140.

[0216] (4) The inlet pump 22 draws the reaction liquid with a volume of V2 into the reaction container 12 and seals the reaction container 12. Then the piston injector 7 injects the liquid sample with a volume of V1 into the reaction container 12 for reaction. The high-precision pressure sensor monitors the gas pressure change in the reaction container 12 in real time to obtain P0 before the reaction and P1 after the reaction. The high-precision temperature sensor detects the temperature T in the reaction container 12.

[0217] (5) The pressure values ​​P0, P1 and temperature value T in step (4) are collected by the central processing unit 25, and the amount of gas moles n released is calculated by the fusion of the ideal gas law and Henry's law.

[0218] The specific calculation method is as described above and will not be repeated here.

[0219] (6) The central processing unit 25 calculates the gas molar load a and volume load b of the sample based on the molar amount n of the released gas, the sample volume V1, and the effective component concentration c of the sample.

[0220] The calculation methods for gas molar loading a and volumetric loading b are as described above.

[0221] (7) The calculated gas molar load a and volume load b of the sample are transmitted to the central control system 190 via analog / communication signals.

[0222] (8) After the test is completed, the post-reaction solution in the gas detection module 120 is returned to the reaction liquid container 24 in the reaction liquid unit 140 via the drain pump 23 and can be recycled. When the cumulative molar amount of CO2 exceeds 1 / 10-1 / 2 of the molar amount of hydrogen ions in the acid solution, fresh acid solution should be replaced.

[0223] Table 1 lists the results of multiple measurements of the same sample in this embodiment.

[0224] Table 1

[0225]

[0226] In the table above, P0 and P1 are both gauge pressures.

[0227] The method and apparatus 100 for detecting liquid-phase gas loading proposed in this invention increases the accuracy of the amount of gas obtained from the reaction by integrating the ideal gas law and Henry's law dual models. Simultaneously, by combining automation technology and program algorithms, it achieves fully automated measurement, completely eliminating human error. This invention achieves high-precision, low-maintenance gas loading monitoring, solving the problems of traditional titration methods, such as inability to operate online, low accuracy, and poor repeatability.

[0228] The beneficial effects of the method and apparatus 100 for detecting liquid phase gas loading proposed in this invention are as follows:

[0229] (1) High precision: absolute error <1.5%.

[0230] (2) Anti-interference: The closed reaction avoids interference from environmental gases, and the degradation products (such as heat-stable salts) do not participate in acid-base reactions and do not affect the detection results.

[0231] (3) High stability: repeatability error is less than 0.5%.

[0232] (4) Low maintenance: It can run continuously without human intervention, except for input commands.

[0233] In the description provided herein, numerous specific details are described. However, it is understood that embodiments of the present invention may be practiced without these specific details. In some instances, well-known methods, structures, and techniques are not shown in detail so as not to obscure the understanding of this description.

[0234] Therefore, those skilled in the art should recognize that although numerous exemplary embodiments of the present invention have been shown and described in detail herein, many other variations or modifications conforming to the principles of the present invention can be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the invention. Thus, the scope of the present invention should be understood and construed as covering all such other variations or modifications.

Claims

1. A method for detecting liquid-phase gas loading, comprising: Reaction and data acquisition steps: Inject the first volume V1 of liquid sample and the second volume V2 of reaction solution into a reaction container with a volume of V. Under the condition of keeping the reaction container sealed, allow the liquid sample and the reaction solution to react fully to release gas, and collect the temperature T inside the reaction container during the reaction process, as well as the pressure P0 and P1 inside the reaction container before the start of the reaction and after the reaction is completed. Steps for calculating the amount of gas released: Based on the collected temperature T, pressure P0 and P1, as well as the first volume V1, the second volume V2 and the volume V, the amount of substance of the gas released is calculated by fusing the ideal gas law and Henry's law into a dual model. as well as Gas loading calculation steps: Calculate the gas loading of the liquid sample based on the amount of gas released, the first volume V1, and the effective component concentration of the liquid sample.

2. The method for detecting liquid-phase gas loading according to claim 1, wherein, The specific steps for calculating the amount of gas released include: Based on the collected temperatures T, pressures P0 and P1, and the first volume V1, the second volume V2, and the volume V, the amount of substance of the released gas is calculated according to the dual-model fusion formula (1) of the ideal gas law and Henry's law: Where n is the amount of substance of the gas released, in mol; The units for V, V1, and V2 are L; T represents temperature in degrees Celsius, expressed in °C. The units for P0 and P1 are kPa; H(T) is the Henry coefficient, H(T) = 0.034 × exp(2600(1 / (T+273.15)-1 / 298.15)) / 100, with units of mol / (L*kPa).

3. The method for detecting liquid-phase gas loading according to claim 1, wherein, The gas load calculation steps specifically include: Based on the amount of gas released, the first volume V1, and the effective component concentration of the liquid sample, the gas molar loading of the liquid sample is calculated according to the following formula (2): And / or Based on the amount of gas released and the first volume V1, the gas volume loading of the liquid sample is calculated according to the following formula (3): Wherein, a is the gas molar loading of the liquid sample, in mol / mol of effective component; b is the gas volumetric loading of the liquid sample, in L / L of sample; n is the amount of substance of the released gas, in mol; c is the concentration of the effective component of the liquid sample, in mol / L; Vm represents the gas molar volume under standard conditions, with a value of 22.4, in L / mol; and V1 is in L.

4. The method for detecting liquid-phase gas loading according to claim 1, wherein, Before injecting the first volume V1 of liquid sample and the second volume V2 of reaction solution into a reaction vessel of volume V, the method further includes: Calibration steps: Using at least one standard liquid sample with known effective component concentration and known gas loading, follow the steps of reaction and data acquisition and the step of calculating the amount of gas released to obtain the amount of gas released by the at least one standard liquid sample. Based on the relationship between the amount of gas released by the at least one standard liquid sample and its known gas loading, determine a correction coefficient. Following the gas load calculation step, the method further includes: Gas loading correction step: The calculated gas loading of the liquid sample is corrected using the correction coefficient.

5. The method for detecting liquid-phase gas loading according to claim 4, wherein, Determining a correction factor based on the relationship between the amount of gas released from the at least one standard liquid sample and its known gas load includes: The correction factor is calculated according to the following formula (4): Where, k is the correction coefficient; d represents the total number of standard liquid samples, d≥1; n1,…,nd represent the amount of gas released from the 1st to the dth standard liquid samples, in mol; L1,…,Ld represent the known gas loading of the 1st to the dth standard liquid samples, in mol / mol of effective component; c1,…,cd represent the effective component concentration of the 1st to the dth standard liquid samples, in mol / L; and V1 is in L. The step of correcting the calculated gas loading of the liquid sample using the correction factor includes: The corrected gas load is obtained by multiplying the calculated gas load of the liquid sample by (2-k).

6. The method for detecting liquid-phase gas loading according to claim 1, wherein, Prior to the reaction and data acquisition steps, the method further includes: Cleaning steps: Inject a first preset volume of the liquid sample and a second preset volume of the reaction solution into the reaction container, allow the liquid sample to react with the reaction solution for a preset time, and then drain the solution from the reaction container.

7. The method for detecting liquid-phase gas loading according to any one of claims 1-6, wherein, The liquid sample and the reaction solution are automatically injected, and each step is automatically executed according to a set time sequence under the control of the central processing module.

8. The method for detecting liquid-phase gas loading according to claim 7, wherein, The automatic injection of the liquid phase sample is achieved through the following methods: The liquid sample is pumped into and fills the inner cavity of the piston injector by a liquid pump, and the piston of the piston injector is controlled to move a set distance to inject a set amount of liquid sample from the piston injector into the reaction vessel.

9. The method for detecting liquid-phase gas loading according to claim 1, wherein, The reaction and data acquisition steps specifically include: The second volume V2 of the reaction solution is injected into a reaction vessel with a volume of V; Seal the reaction vessel and collect the pressure P0 inside the reaction vessel before the reaction begins; A liquid sample of a first volume V1 is injected into the reaction vessel to allow the liquid sample to fully react with the reaction liquid and release gas. The temperature T inside the reaction vessel during the reaction process and the pressure P1 inside the reaction vessel after the reaction is completed are collected.

10. The method for detecting liquid-phase gas loading according to claim 1, wherein, The gas is CO2, the liquid sample is an absorption solution containing a CO2 absorbent as an effective component, and the reaction solution is an acidic solution that reacts with the CO2 absorbent.