Online preconcentration sampling injection device

Abstract

The utility model provides a kind of online pre-concentration sampling injection device, it includes: a double-layer structure absorption bottle is with foaming device and sampling tube in inside;A multi-way flow control valve has multiple interfaces, for controlling the flow direction between multiple pipelines;A sampling valve is arranged at detector end;A liquid transfer pump is used to extract liquid in absorption bottle;And a gas suction pump is connected to the absorption bottle and the multi-way flow control valve.The online pre-concentration sampling injection device adopts rear introduction design, can reduce the dead angle and residual possibility of sampling process, improve analysis repeatability, and can be integrated with multiple detectors, realize the online analysis of compound in multiple types of gas.

Description

Technical Field

[0001] This invention relates to an online pre-concentration sampling and injection device, particularly a device that can be used for the collection and analysis of gas and liquid samples. Background Technology

[0002] In the existing technology, most similar collection devices adopt a push-type design, that is, a pressurized or pushing gas extraction pump is installed on the sampling pipeline to push the sample into the system by mechanical force.

[0003] This design has the following specific problems:

[0004] 1. The mechanical pushing force on the sample may change the physical state of the sample and affect the accuracy of the analysis results.

[0005] 2. The internal structure of the gas extraction pump is prone to creating dead zones, leading to sample residue and affecting the accuracy and reliability of continuous analysis.

[0006] 3. The push-type design requires more valves to control the pressurized and pushed sample, which not only increases the complexity of the system, but also increases the difficulty of maintenance.

[0007] 4. Due to the complex system structure and difficulty in cleaning, the risk of cross-contamination increases.

[0008] Furthermore, existing online sampling devices typically focus on analyzing a single type of sample, with few devices capable of handling multiple components and detectors. Existing devices often use absorption bottles made of a single material, such as PTFE, while different analytes require different absorption bottle materials, thus limiting the device's application range. Utility Model Content

[0009] In view of the above, the purpose of this utility model is to provide an online pre-concentration sampling and injection device, which adopts a back-draw design, can reduce dead zones and the possibility of residues in the sampling process, improve the repeatability of analysis, and can be integrated with multiple detectors to realize online analysis of compounds in various types of gases.

[0010] According to this disclosure, an online pre-concentration sampling and injection device is provided, comprising: an absorption bottle,

[0011] It features a double-layer structure for capturing and concentrating analytes in samples; a multi-flow control valve with multiple interfaces for controlling the flow direction between multiple pipelines; an injection valve located at a detector end and connected to the multi-flow control valve and an extractant pipeline; a liquid transfer pump connected to the multi-flow control valve for drawing liquid from the absorption bottle; and a gas extraction pump connected to the absorption bottle and the multi-flow control valve for generating negative pressure to introduce gaseous samples into the absorption bottle. The multi-flow control valve has ten interfaces, one connected to the absorption bottle and another to the injection valve. The absorption bottle is connected to the gas extraction pump via a first pipeline and to the liquid transfer pump via a second pipeline. The injection valve is connected to the extractant pipeline.

[0012] In one embodiment, the device further includes: a temperature-controlled absorbent metering loop, which is a pipeline with a fixed volume connected to the multi-way flow control valve for quantitatively controlling the amount of absorbent used; and an injection metering loop, which is a pipeline with a fixed volume connected to the injection valve for quantitatively controlling the volume of the liquid to be tested entering the detector.

[0013] In one embodiment, the gas extraction pump includes a metering valve for controlling the flow rate to ensure a fixed sampling volume.

[0014] In one embodiment, the absorption bottle is provided with a foaming device and a sample inlet tube. The foaming device is used to increase the contact area between the gas sample and the absorption liquid to improve the capture efficiency, and the sample inlet tube is used to introduce the captured components into the detector at the back end.

[0015] In one embodiment, the multi-way flow control valve has multiple ports for introducing pure water into the absorption bottle through the multi-way flow control valve, and for connecting a nitrogen line, a pure water line, and the injection tube; the pure water line is used to introduce pure water into the absorption bottle through the multi-way flow control valve, the nitrogen line is used to introduce nitrogen into the absorption bottle through the multi-way flow control valve, and one end of the injection tube is disposed inside the absorption bottle, and the other end is connected to the multi-way flow control valve.

[0016] In one embodiment, the constant temperature absorption liquid metering loop and the sample injection metering loop are used for sample injection of a fixed volume. These metering loops are actually fixed volume pipelines. By switching the valve, the liquid remaining in the fixed volume pipeline is introduced into the required pipeline during the switching process, thereby achieving sample injection of a fixed volume of liquid.

[0017] This utility model also provides a sample injection method for an online pre-concentration sampling injection device, which includes:

[0018] Next steps:

[0019] A negative pressure is generated in the absorption bottle by a gas extraction pump, and the gas sample is introduced into the absorption bottle.

[0020] The gas sample is brought into full contact with the absorbent liquid through the foaming device inside the absorption bottle to capture the sample.

[0021] The target substance;

[0022] The absorbent containing the sample is drawn using a liquid transfer pump;

[0023] By switching the multi-flow control valve, the absorbent is introduced into the constant temperature absorbent metering loop;

[0024] The volume of sample entering the detector is controlled by a quantitative injection loop;

[0025] The quantified sample is introduced into the detector via the injection valve for analysis.

[0026] In one embodiment, a preparatory step is included before the gas sample is introduced into the absorption bottle:

[0027] A fixed amount of pure water is introduced into the absorption bottle as the absorption liquid through the multi-way flow control valve;

[0028] A measured amount of pure water is propelled into the absorption bottle using nitrogen gas.

[0029] This allows the analyte in the gas sample to be captured by the absorbent liquid.

[0030] In one embodiment, after sample analysis is completed, a cleaning step is included:

[0031] The absorption bottle and pipeline are cleaned by introducing pure water through the multi-way flow control valve.

[0032] Nitrogen gas is introduced into the pipeline through the multi-way flow control valve to remove residual substances in preparation for the next sampling.

[0033] In one embodiment, the absorbent can be selected according to the characteristics of the analyte:

[0034] When the substance to be tested is a metal, nitric acid is used as the absorption liquid;

[0035] When the substance to be tested is in an ionic state or a polar substance, pure water is used as the absorption liquid. Attached Figure Description

[0036] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0037] Figure 1 This is an exploded view of the device components of this utility model.

[0038] Figure 2 This is a schematic diagram of the sample injection method operation steps of this utility model.

[0039] Figure 3 This is a schematic diagram of the preparatory steps performed before the sample introduction step.

[0040] Figure 4 This diagram illustrates the steps required after the sample analysis is completed. Detailed Implementation

[0041] The following description contains specific information relating to exemplary embodiments of the present invention. The accompanying drawings and detailed description are merely exemplary embodiments. However, the present invention is not limited to these exemplary embodiments. Other variations and embodiments of the present invention will occur to those skilled in the art. Unless otherwise stated, the same or corresponding components in the drawings may be indicated by the same or corresponding reference numerals. Furthermore, the drawings and illustrations in the present invention are generally not drawn to scale and are not intended to correspond to actual relative dimensions.

[0042] For the purposes of consistency and ease of understanding, the same features are indicated by reference numerals in the exemplary drawings (although this is not the case in some examples). However, features in different embodiments may differ in other respects, and therefore should not be narrowly limited to the features shown in the drawings.

[0043] The terms "at least one embodiment," "one embodiment," "multiple embodiments," "different embodiments," "some embodiments," and "this embodiment" indicate that the described embodiments of the present invention may include specific features, structures, or characteristics, but not every possible embodiment of the present invention must include such specific features, structures, or characteristics. Furthermore, the repeated use of the phrases "in one embodiment" and "in this embodiment" does not necessarily refer to the same embodiment, although they may be identical. Moreover, the use of phrases such as "embodiment" in connection with "the present invention" does not mean that all embodiments of the present invention must include specific features, structures, or characteristics, and should be understood as "at least some embodiments of the present invention."

[0044] This includes the specific features, structures, or properties described. The term "coupled" is defined as a connection, whether direct or indirect through intermediate components, and is not necessarily limited to physical connections. When the term "comprising" is used, it means "including but not limited to," explicitly indicating an open inclusion or relationship of the described combinations, groups, series, and equivalences.

[0045] Furthermore, for illustrative and non-restrictive purposes, specific details such as functional entities, technologies, protocols, and standards are elaborated to provide an understanding of the described technologies. In other examples, detailed descriptions of well-known methods, technologies, systems, architectures, etc., are omitted to avoid obscuring the explanatory narrative with unnecessary details.

[0046] The terms "first," "second," and "third" in the specification and accompanying drawings of this utility model.

[0047] The terms "comprising" and any variations thereof are used to distinguish different objects, not to describe a specific order. Furthermore, the term "comprising" and any variations thereof are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or modules is not limited to the steps or modules listed, but may optionally include steps or modules not listed, or may optionally include other steps or modules inherent to those processes, methods, products, or devices.

[0048] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0049] Please refer to Figure 1 The figure shows a schematic diagram of the detection system of this utility model. The detection system includes an online pre-concentration sampling and injection device 10 and a detector 11. The online pre-concentration sampling and injection device 10 functions to collect gas or liquid samples, capture and concentrate the analyte in the samples, and quantitatively introduce the concentrated analyte into the detector 11, thereby achieving accurate detection and analysis of the analyte in the sample. It is understood that the online pre-concentration sampling and injection device 10 can be integrated with various detectors 11 to achieve diverse detection and analysis functions. For example, ion chromatography (IC) for analyzing acid and alkali components and amines; liquid chromatography (LC) for analyzing industrial oxidants, fluorescent agents, and solvents; and inductively coupled plasma mass spectrometry (ICP-MS) for analyzing metal components—as long as the detector 11 has an injection valve, the analyte absorbent can be introduced into the detector 11 for detection and analysis through the pipeline connection method of this utility model. Furthermore, existing detectors can be used for the detector 11, and will not be described in detail here.

[0050] Please refer to the following: Figure 1 The online pre-concentration sampling and injection device 10 provided in this application includes an absorption bottle 101, a foaming device 102, an injection tube 103, a multi-way flow control valve 104, an injection valve 105, a liquid transfer pump 106, a gas extraction pump 107, a quantitative loop for absorption liquid at a certain temperature 108, and an injection quantitative loop 109.

[0051] The absorption bottle 101 has a double-layer structure, which is used to capture and concentrate the analyte in the sample.

[0052] Specifically, the absorption bottle 101 contains an absorbent suitable for the specific analyte (such as pure water or nitric acid). When the gas sample enters the absorption bottle through the foaming device 102, the foaming device 102 forms tiny bubbles in the gas sample, increasing the contact area between the gas and the absorbent. This allows the analyte in the gas (such as ionic substances, polar substances, or metallic substances) to dissolve or be absorbed into the absorbent, thus achieving the capture process. As the sampling time increases, more and more analytes accumulate in the limited volume of absorbent, causing the concentration of the analyte in the absorbent to gradually increase, thereby achieving a concentration effect and facilitating subsequent detection and analysis. The double-layer structure consists of inner and outer glass walls. The inner glass wall forms an inner cavity for containing the sample and absorbent, while an isolation space is formed between the outer and inner glass walls. This double-layer structure provides insulation, reduces heat loss, and allows for water-cooled low-temperature circulation to be added in the isolation space for temperature control when low-temperature absorption is required. This increases the stability of the operating environment and improves the repeatability of online concentration performance. Furthermore, the absorption bottle 101 of this invention can be made of different materials depending on the analyte. For example, when the analyte is a metal, PFA (perfluoroalkoxyalkanes) material with good chemical stability is used; when the analyte is a strong acid, glass is used; when the analyte is a strong alkali or amine, PTFE (polytetrafluoroethylene) material is used; and when the analyte is a weak acid or weak alkali, glass is used. The selection of different materials mainly considers properties such as corrosion resistance and leaching resistance to ensure the accuracy of the analysis.

[0053] Furthermore, the foaming device 102 is installed inside the absorption bottle 101. Its function is to make the introduced gas sample form bubbles in the water, thereby increasing the contact probability and area between the gas sample and the absorption liquid, thus improving the absorption probability and capture efficiency of water-soluble or polar molecules.

[0054] One end of the injection tube 103 is located inside the absorption bottle 101, and the other end is connected to a multi-way flow control valve 104, which is used to introduce the absorption liquid that has captured the air sample components into the pipeline of the detector 11.

[0055] This invention can be integrated with different detectors 11: for example, ion chromatographs (IC) for analyzing acid and base components and amines; liquid chromatographs (LC) for analyzing industrial oxidants, fluorescent agents and solvents; and inductively coupled plasma mass spectrometers (ICP-MS) for analyzing metal components. As long as the detector 11 has an injection valve, the absorbent to be analyzed can be introduced into the detector 11 for analysis through the pipeline connection method of this invention.

[0056] Furthermore, the multi-way flow control valve 104 has multiple ports for controlling the flow direction between multiple pipelines and changing the connection relationship between these ports by switching positions. One port is connected to the absorption bottle 101, and another port is connected to a sample injection valve 105. The ports of the multi-way flow control valve 104 are also used to connect a nitrogen line and a pure water line. The pure water line is used to introduce pure water into the absorption bottle 101 as the absorbent through the multi-way flow control valve 104, and the nitrogen line is used to introduce nitrogen into the absorption bottle 101 through the multi-way flow control valve 104 to assist in pushing a quantitative amount of pure water into the absorption bottle 101 and to flush the pipeline to remove residual substances. The multi-way flow control valve 104 is a 10-hole two-way valve with two switching positions. In the first position, the nitrogen line is connected to the absorption bottle 101, and the pure water line is closed; when switched to the second position, the pure water line is connected to the absorption bottle 101, and the nitrogen line is closed. This switching method allows for flexible control over the timing of introducing different fluids.

[0057] The online pre-concentration sampling and injection device 10 also includes a liquid transfer pump 106 and a gas extraction pump 107. The liquid transfer pump 106 is connected to a multi-way flow control valve 104 and is specifically used for extracting liquid and draining water from the absorption bottle 101. Specifically, when analysis is required after sample capture, the liquid transfer pump 106 is used to extract the absorption liquid containing the analyte and introduce it into the isothermal absorption liquid metering loop 108 for subsequent analysis. However, during the cleaning stage after analysis or before changing to a different type of analysis, the liquid transfer pump 106 is used to extract and drain waste liquid or cleaning solution from the absorption bottle for the next sample collection.

[0058] A gas extraction pump 107 is connected to a multi-way flow control valve 104. In one embodiment, the gas extraction pump 107 includes a metering valve 1071, which controls the flow rate of the gas sample to ensure a fixed sampling volume and accurate sampling. By precisely controlling the flow rate and time of the gas sample through the absorption bottle, a fixed volume of gas sample can be used for each analysis, thereby improving the repeatability and accuracy of the analysis results. The gas extraction pump 107 is used to generate a negative pressure in the absorption bottle 101, allowing the gas sample to be introduced into the absorption bottle 101. Specifically, the gas extraction pump 107 is connected to the multi-way flow control valve 104 through a first pipeline, and the multi-way flow control valve 104 is in turn connected to the absorption bottle 101 through a pipeline. When the gas extraction pump 107 is started, it draws gas from the outlet side of the absorption bottle 101, creating a negative pressure environment inside the absorption bottle 101 that is lower than the external atmospheric pressure. Due to the pressure difference, external gas samples are automatically drawn into the inlet side of the absorption bottle 101 and then come into contact with the absorption liquid through the foaming device 102. This post-draw design avoids the gas sample passing through the internal structure of the pump, reducing dead zones and sample residue problems, while ensuring that the sample contacts the absorption liquid in a natural state without being mechanically squeezed, thus improving capture efficiency and analytical accuracy.

[0059] In one embodiment, both the isothermal absorption liquid metering loop 108 and the sample injection metering loop 109 are pipelines with fixed volumes. The isothermal absorption liquid metering loop 108 is connected to the multi-way flow control valve 104 to quantitatively control the amount of absorption liquid used, ensuring that a fixed volume of absorption liquid is used each time. The sample injection metering loop 109 is connected to the injection valve 105 to quantitatively control the volume of the analyte entering the detector 11, ensuring that the same volume of sample is used for each analysis. Furthermore, the injection valve 105 can be further disposed at the detector 11 end and connected to an eluent pipeline 1051. The eluent pipeline 1051 is used to propel the analyte in the sample injection metering loop 109 and push it into the detector 11 for analysis. By switching the valves, the isothermal absorption liquid metering loop 108 and the sample injection metering loop 109 can, during switching, introduce the liquid remaining in the fixed-volume pipeline into the required pipeline, achieving the injection of a fixed volume of liquid.

[0060] As described above, this invention employs a rear-entry gas pipeline design, placing the gas extraction pump at the rear end of the sample inlet path. The sample is introduced into the absorption bottle via this rear-entry gas extraction pump. This design reduces the amount of residue and dead zones in the sampling pipeline caused by the gas extraction pump, and reduces the number of valves and pipeline components, thus improving the repeatability of online sampling and analysis. Furthermore, the absorption bottle of this invention uses a double-layered glass design, which provides insulation to reduce heat loss and allows for water-cooled low-temperature circulation for temperature control when low-temperature absorption is required, increasing the stability of the operating environment.

[0061] Please see Figure 2 The following are the operational steps of the injection method of this utility model. The online pre-concentration sampling injection method of this utility model mainly includes the following steps:

[0062] Sample introduction step 201: A negative pressure is generated in the absorption bottle 101 to introduce the gas sample into the absorption bottle 101. In one embodiment, a negative pressure is generated in the absorption bottle 101 by a gas extraction pump 107 to introduce the gas sample into the absorption bottle 101. This back-inlet design reduces the problems of dead corners and residues.

[0063] Sample capture step 202: The gas sample is brought into full contact with the absorbent liquid in the absorption bottle 101. In one embodiment, a foaming device 102 is used to ensure full contact between the gas sample and the absorbent liquid in the absorption bottle 101. It is understood that increasing the contact area through this foaming method can more effectively improve the capture efficiency of the analyte.

[0064] Step 203: The absorbent containing the analyte is extracted by the liquid transfer pump 106, and the liquid is discharged from the absorption bottle 101 and sent to the multi-way flow control valve 104 to prepare for subsequent quantification and analysis.

[0065] A certain amount control step 204: By switching the multi-way flow control valve 104, the absorbent is introduced into the constant temperature absorbent quantitative loop 108, and the sample volume entering the detector 11 is controlled by the sample injection quantitative loop 109 to ensure that the analysis uses a fixed volume of sample.

[0066] Sample analysis step 205: After quantification, the sample is introduced through the injection valve 105 and further analyzed in the detector 11.

[0067] Please see Figure 3 In one embodiment, the following preparatory steps are required before the sample introduction step 201:

[0068] Step 301: A quantitative amount of pure water is introduced into the absorption bottle 101 through the multi-way flow control valve 104 to serve as the absorption liquid for capturing the analyte.

[0069] Auxiliary pushing step 302: Use nitrogen to push a quantitative amount of pure water to ensure that pure water enters the absorption bottle 101 so that the analyte in the gas sample can be captured by the absorption liquid.

[0070] Please see Figure 4 In one embodiment, after sample analysis step 205 is completed, the following steps need to be performed:

[0071] Pure water cleaning step 2051: Pure water is introduced through the multi-way flow control valve 104 to clean the absorption bottle 101 and the pipeline system.

[0072] Nitrogen flushing step 2052: Nitrogen gas is introduced through the multi-way flow control valve 104 to flush and remove residual substances in the pipeline in preparation for the next sampling.

[0073] In one embodiment, different absorbents can be selected according to the characteristics of the analyte. For example, if metal composition analysis is performed, nitric acid is used as the absorbent, which is suitable for capturing metal substances in the gas; if ionic or polar substances are analyzed, pure water is used as the absorbent, which is suitable for capturing water-soluble or highly polar substances.

[0074] In summary, the key feature of this method is its post-guided design, which guides the sample using negative pressure, effectively reducing dead zones and residue issues, and improving the accuracy and repeatability of the analysis. Simultaneously, the quantitative loop design ensures precise control of the sample volume, and combined with the selection of different absorbents, it is applicable to the analysis of various types of analytes.

[0075] The embodiments of this utility model have been described in detail above with reference to the accompanying drawings. However, the specific configuration is not limited to these embodiments and includes design changes that do not depart from the spirit and scope of this utility model. Furthermore, this utility model can be modified in various ways within the scope of the claims. Embodiments obtained by appropriately combining the technical means disclosed in different embodiments are also included within the technical scope of this utility model. Additionally, it also includes configurations obtained by interchanging elements that are elements described in the above embodiments and achieve the same effect.

Claims

1. An online pre-concentration sampling and injection device, characterized in that, include: An absorption bottle with a double-layer structure is used to capture and concentrate the analyte in a sample; A multi-way flow control valve with multiple ports for controlling the flow direction between multiple pipelines; An injection valve is located at a detector end and connected to the multi-way flow control valve and an extraction liquid pipeline; A liquid transfer pump, connected to the multi-way flow control valve, is used to draw liquid from the absorption bottle; A gas extraction pump, connected to the multi-way flow control valve, is used to generate negative pressure to introduce the gas sample into the absorption bottle; The multi-way flow control valve has ten ports, one of which is connected to the absorption bottle and another port is connected to the injection valve. The absorption bottle is connected to the gas extraction pump through a first pipeline and to the liquid transfer pump through a second pipeline. The injection valve is connected to the flushing liquid pipeline.

2. The online pre-concentration sampling and injection device as described in claim 1, characterized in that, The device also includes: A metering loop for absorbent liquid at a constant temperature, which is a pipeline with a fixed volume, is connected to the multi-way flow control valve for metering control of the amount of absorbent liquid used; and A sample injection loop, which is a pipeline with a fixed volume, is connected to the injection valve to quantitatively control the volume of the liquid to be tested entering the detector.

3. The online pre-concentration sampling and injection device as described in claim 1, characterized in that, The gas extraction pump includes a metering valve, which is used to control the flow rate to ensure a constant sampling volume.

4. The online pre-concentration sampling and injection device as described in claim 1, characterized in that, The absorption bottle is equipped with a foaming device and a sample inlet tube. The foaming device is used to increase the contact area between the gas sample and the absorption liquid to improve the capture efficiency. The sample inlet tube is used to introduce the captured components into a detector at the rear end.

5. The online pre-concentration sampling and injection device as described in claim 4, characterized in that, The multi-way flow control valve has multiple ports for introducing pure water into the absorption bottle through the multi-way flow control valve. It is used to connect a nitrogen line, a pure water line and the injection tube. The pure water line is used to introduce pure water into the absorption bottle through the multi-way flow control valve. The nitrogen line is used to introduce nitrogen into the absorption bottle through the multi-way flow control valve. One end of the injection tube is located inside the absorption bottle and the other end is connected to the multi-way flow control valve.

6. The online pre-concentration sampling and injection device as described in claim 2, characterized in that, The constant-temperature absorption liquid metering loop and the injection metering loop are used for injecting a fixed volume of sample. These metering loops are actually fixed-volume pipelines. By switching the valve, the liquid remaining in the fixed-volume pipeline is introduced into the required pipeline during the switching process, thereby achieving the injection of a fixed volume of liquid.

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