An inductively coupled plasma mass spectrometer

Abstract

The utility model relates to mass spectrometer technical field discloses an inductance coupling plasma mass spectrometer, including control module, control module both -way electric connection has on -line calibration module, detection and signal processing module, cooling module, vacuum module, control module one -way electric connection has gas control module and mass analysis module, detection and signal processing module one -way electric connection has data storage and management module, cooling module one -way electric connection vacuum module. In the utility model, through the coordinated operation of each module, can realize sample ionization, transmission, separation's whole process stable high -efficient, improve inductance coupling plasma mass spectrometer's plasma stability, reduce signal drift, reduce matrix effect interference to improve detection accuracy and sensitivity.

Description

Technical Field

[0001] This utility model relates to the field of mass spectrometry technology, and in particular to an inductively coupled plasma mass spectrometer. Background Technology

[0002] Inductively coupled plasma mass spectrometry (ICP-MS) plays a crucial role in rapid multi-element analysis and is widely used in various fields such as environment, biology, food, and materials. With the development of ICP-MS technology, it is of great significance to improve detection accuracy and sensitivity, and shorten analysis time. Therefore, there is a need to develop an inductively coupled plasma mass spectrometer.

[0003] A search revealed Chinese Patent Publication No. CN212459511U, which discloses a novel inductively coupled plasma mass spectrometer (ICP-MS). The mass spectrometer includes a main body with a matching base. Multiple support rods are evenly arranged vertically along the lower part of the base, each passing through a buffer plate located below the base. A shock-absorbing washer is fitted onto the portion of each support rod between the base and the buffer plate. Each support rod has an external thread on its lower half, and a nut is threaded onto the portion of each support rod below the buffer plate. The lower end of each support rod connects to a base, and each base has a connection hole that fits with the support rod with a clearance fit. A buffer spring is installed between the lower end of the support rod and the bottom of the connection hole. This invention effectively reduces vibration in the mass spectrometer, minimizing noise generated during operation and preventing loosening of components due to vibration, thus extending the instrument's lifespan.

[0004] The aforementioned utility model reduces noise generated by vibration during the operation of the mass spectrometer and avoids the loss of instrument life due to loosening of components caused by vibration. However, in actual use, some ICP-MS devices have problems such as poor plasma stability, signal drift, matrix effect interference, and high detection limit, which limits their application in the field of high-precision analysis. Utility Model Content

[0005] To overcome the above shortcomings, this invention provides an inductively coupled plasma mass spectrometer, which aims to improve the problems of poor plasma stability, signal drift, matrix effect interference, and high detection limits of some existing ICP-MS devices, thus limiting their application in the field of high-precision analysis.

[0006] To achieve the above objectives, the present invention adopts the following technical solution: an inductively coupled plasma mass spectrometer, comprising a control module, wherein the control module is bidirectionally electrically connected to an online calibration module, a detection and signal processing module, a cooling module, and a vacuum module; the control module is unidirectionally electrically connected to a gas control module and a mass analysis module; the detection and signal processing module is unidirectionally electrically connected to a data storage and management module; and the cooling module is unidirectionally electrically connected to the vacuum module.

[0007] The above technical solution achieves fully automated collaborative operation through the electrical connection between the control module and each functional module, and reduces environmental interference through multi-module collaborative temperature and vacuum control.

[0008] As a further description of the above technical solution: The online calibration module is electrically connected to the sample introduction module, and the gas control module is electrically connected to the sample introduction module. The sample introduction module includes a dual-layer atomization system. The atomizer used in the dual-layer atomization system is used to ensure the atomization efficiency of the sample and to actively cool and coordinate with the vertical optical path.

[0009] Through the above technical solution: the connection between the online calibration module and the sample introduction module realizes the automated process of "calibration signal generation - sample introduction execution - data correction", while the connection between the gas control module and the sample introduction module ensures the stability of gas conditions during the atomization process. Then, the dual-layer atomization system can be responsible for converting liquid samples into aerosols and transporting them to plasma.

[0010] As a further description of the above technical solution: The sample introduction module is electrically connected to an ion source module, and the ion source module is electrically connected to a gas control module.

[0011] The above technical solution can trigger the synchronous timing of aerosol injection and plasma generation, ensuring improved sample ionization efficiency, avoiding signal delay or pulse fluctuations, and dynamically adjusting the plasma argon flow rate.

[0012] As a further description of the above technical solution: The plasma outlet of the ion source module is connected to the input of the ion extraction interface module via a sampling cone.

[0013] The above technical solution optimizes the ion transmission path by controlling the sampling cone voltage, compresses the ion beam diameter, improves ion transmission efficiency, and reduces neutral particle interference.

[0014] As a further description of the above technical solution: The ion extraction interface module is connected to the vacuum module via a vacuum pipeline, and the ion extraction interface module is connected to the quality analysis module via an ion transmission channel.

[0015] The above technical solution allows for real-time monitoring of the vacuum level in the ion extraction area, reducing ion scattering and loss during transmission, and effectively improving ion transmission efficiency.

[0016] As a further description of the above technical solution: The quality analysis module is bidirectionally electrically connected to the vacuum module, and the quality analysis module is electrically connected to the detection and signal processing module.

[0017] Through the above technical solution: the vacuum gauge in the mass analysis module monitors the high vacuum environment in areas such as the quadrupole in real time and feeds the data back to the vacuum module. At the same time, the vacuum module can receive control commands from the mass analysis module and adjust the pumping strategy according to the analysis requirements to ensure that ions complete mass-to-charge ratio screening under collision-free and stable vacuum conditions, thereby improving mass spectrometry resolution and detection accuracy. By adopting a noise filtering algorithm based on machine learning, the signal-to-noise ratio of the signal is significantly improved, and the data purity is enhanced.

[0018] As a further description of the above technical solution: The mass analysis module includes a quadrupole mass filter, which filters ions with a specific mass-to-charge ratio (m / z) using RF / DC voltage.

[0019] The above technical solution enables the four-stage mass filter to achieve efficient screening and quantitative detection of target elements by precisely adjusting the RF / DC voltage parameters.

[0020] As a further description of the above technical solution: The ion source module includes a radio frequency generator and a quartz torch. The vacuum module includes a mechanical pump, a turbomolecular pump, and a vacuum gauge. The radio frequency generator is connected to the cooling module via a stainless steel water-cooling pipeline. The induction coil of the radio frequency generator coaxially surrounds the quartz torch. The quartz torch ionizes argon gas through the electromagnetic field of the radio frequency generator to generate plasma. The mechanical pump is connected to the ion extraction interface module via a metal vacuum pipeline. The turbomolecular pump is connected to the cooling module via a metal heat sink. The turbomolecular pump is connected to the mass analysis module via an independent vacuum pipeline. The vacuum gauge is connected to the mechanical pump and the turbomolecular pump via signal connections.

[0021] The above technical solution involves connecting the radio frequency generator to the cooling module via stainless steel water-cooled pipes, ensuring a stable output of a high-frequency electromagnetic field. This field then drives a quartz torch to ionize argon gas, forming high-temperature plasma for efficient sample ionization. The turbomolecular pump automatically adjusts its speed based on the vacuum level in the quadrupole region. When the vacuum level drops to a certain value, it quickly recovers to the target value, ensuring collision-free ion transport. The stainless steel pipes can withstand 10 bar of pressure to cool the radio frequency generator, removing its heat and controlling temperature fluctuations, preventing radio frequency drift, and extending the lifespan of the quartz torch. Furthermore, a vacuum gauge monitors the vacuum level in the ion extraction area in real time, feeding the data back to the mechanical pump and turbomolecular pump control system of the vacuum module, thereby dynamically adjusting the pump speed and power.

[0022] This utility model has the following beneficial effects: 1. In this utility model, through the coordinated operation of each module, the entire process of sample ionization, transmission and separation can be made stable and efficient, improving the plasma stability of the inductively coupled plasma mass spectrometer, reducing signal drift, reducing matrix effect interference, and thus improving detection accuracy and sensitivity.

[0023] 2. In this invention, by employing a dual-layer atomization system and an optimized radio frequency generator, the stability of the plasma is significantly enhanced and the signal drift is significantly reduced. The mechanical pump and turbomolecular pump are connected to the ion extraction interface module and the mass analysis module respectively through vacuum pipelines. With the real-time monitoring and feedback of the vacuum gauge, a gradient environment from low vacuum to high vacuum is constructed to ensure stable ion transmission. Attached Figure Description

[0024] Figure 1 This is a schematic diagram of the module connection of an inductively coupled plasma mass spectrometer proposed in this utility model; Figure 2 This is a schematic diagram of the ion source module composition of an inductively coupled plasma mass spectrometer proposed in this utility model; Figure 3 This is a schematic diagram of the vacuum module composition of an inductively coupled plasma mass spectrometer proposed in this utility model; Figure 4 This is a schematic diagram of the vacuum module connection of an inductively coupled plasma mass spectrometer proposed in this utility model. Detailed Implementation

[0025] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0026] Reference Figure 1 The present invention provides an embodiment of an inductively coupled plasma mass spectrometer, comprising a control module, which is bidirectionally electrically connected to an online calibration module, a detection and signal processing module, a cooling module, and a vacuum module; the control module is unidirectionally electrically connected to a gas control module and a mass analysis module; the detection and signal processing module is unidirectionally electrically connected to a data storage and management module; and the cooling module is unidirectionally electrically connected to the vacuum module. Specifically, real-time automatic calibration can be achieved through a bidirectional connection between the control module and the online calibration module. The control module dynamically adjusts calibration parameters based on detection data to ensure long-term instrument stability. A bidirectional data exchange between the control module and the detection and signal processing module supports real-time signal adjustment. A bidirectional connection between the control module and the cooling module monitors coolant temperature and flow rate, dynamically adjusts cooling power, ensures the thermal stability of the RF generator and quartz torch, and prevents plasma flameout or signal drift caused by temperature fluctuations. A bidirectional connection between the control module and the vacuum module allows for real-time adjustment of the pump speed based on vacuum feedback, maintaining a high vacuum environment along the ion transport path to ensure collision-free ion transport and improve mass spectrometry resolution. A connection between the control module and the gas control module precisely controls the argon flow rate, maintaining plasma stability and sample transport efficiency. Since the quadrupole requires a high vacuum (10⁻⁻⁴), this feature is crucial. 5 –10⁻ 6 Operating at a vacuum level of (Pa), insufficient vacuum can cause ions to collide with gas molecules, thus altering the screening effect of the RF / DC voltage. By connecting the control module and the mass analysis module, the quadrupole RF / DC voltage parameters can be set to determine the ion screening range and achieve selective detection of target elements. The connection between the detection and signal processing module and the data storage and management module allows for one-way transmission of processed mass spectrometry data to the database, supporting result traceability, report generation, and long-term data accumulation. The cooling module provides water cooling for the turbomolecular pump of the vacuum module, ensuring the temperature stability of the pump body during high-speed operation, extending pump life, and improving pumping efficiency.

[0027] Reference Figure 1The online calibration module is electrically connected to the sample introduction module, and the gas control module is electrically connected to the sample introduction module. The sample introduction module includes a double-layer atomization system. The atomizer used in the double-layer atomization system is used to ensure the atomization efficiency of the sample and to actively cool and coordinate with the vertical optical path. Specifically, the online calibration module can control parameters such as the solenoid valve and peristaltic pump speed of the sample introduction module through electrical signal commands, thereby realizing the timed and quantitative introduction of standard solutions and ensuring the automation of the calibration process. The gas control module can precisely adjust the opening of the gas pipeline valve of the sample introduction module through electrical signals, matching the carrier gas flow rate and atomization efficiency in real time, avoiding the decrease in atomization stability due to gas fluctuations. The dual-layer atomization system uses an atomizer that atomizes the sample solution into fine droplets through the inner atomizing nozzle, while the outer auxiliary airflow provides additional cooling effect, reducing thermal interference, improving atomization efficiency, and reducing the interference of the sample matrix on the optical path.

[0028] Reference Figure 1 The sample introduction module is electrically connected to the ion source module, which is electrically connected to the gas control module. The plasma outlet of the ion source module is connected to the input of the ion extraction interface module via a sampling cone. The ion extraction interface module is connected to the vacuum module via a vacuum pipeline and to the mass analysis module via an ion transmission channel. The mass analysis module is bidirectionally electrically connected to the vacuum module and electrically connected to the detection and signal processing module. The mass analysis module includes a quadrupole mass filter, which filters ions with a specific mass-to-charge ratio (m / z) using RF / DC voltage. Specifically, the sample introduction module controls the sample injection rate via electrical signals and is triggered synchronously with the ion source module. The sample introduction module only begins to deliver sample aerosol after the ion source RF generator is activated, thus ensuring that the sample aerosol and plasma generation timing are matched and avoiding signal delay. The connection between the ion source module and the gas control module can adjust the plasma gas flow rate via electrical signals to maintain plasma stability. The ion source module can control the sampling cone voltage of the ion extraction interface module, thereby optimizing the ion transmission efficiency from atmospheric pressure to vacuum. The cooling module can remove heat from the RF generator and quartz torch, thereby maintaining plasma stability and extending torch life. The vacuum module can dynamically adjust the mechanical pump speed through feedback from the vacuum gauge of the ion extraction interface module. Through the design of a novel quadrupole mass spectrometer filter combined with a high-precision mass resolution algorithm, non-target ions can be effectively filtered out, reducing matrix effect interference and significantly improving the detection limit. Through modular electrical interconnection and fluid pipeline coordination, the entire process from sample introduction to signal detection is automated.

[0029] Reference Figure 2 , Figure 3 and Figure 4The ion source module includes a radio frequency generator and a quartz torch. The vacuum module includes a mechanical pump, a turbomolecular pump, and a vacuum gauge. The radio frequency generator is connected to the cooling module through a stainless steel water-cooling pipeline. The induction coil of the radio frequency generator is coaxially wrapped around the quartz torch. The quartz torch ionizes argon gas through the electromagnetic field of the radio frequency generator to generate plasma. The mechanical pump is connected to the ion extraction interface module through a metal vacuum pipeline. The turbomolecular pump is connected to the cooling module through a metal heat sink. The turbomolecular pump is connected to the mass analysis module through an independent vacuum pipeline. The vacuum gauge is connected to the mechanical pump and the turbomolecular pump for signal connection respectively. Specifically, since the RF generator generates high heat during operation, it needs to be cooled by circulating water to remove the heat and maintain a stable operating temperature. The selected stainless steel pipes are corrosion-resistant and have good thermal conductivity, meeting the safety requirements of high-frequency electromagnetic field environments. The quartz torch tube, as a plasma container, couples RF energy through an induction coil to ionize argon gas and form high-temperature plasma, atomizing and ionizing the elements in the sample. The mechanical pump is connected to the ion extraction interface module through a metal vacuum pipeline, which can quickly establish a pre-vacuum, thereby providing working conditions for the turbomolecular pump and ensuring that ions can smoothly enter the vacuum system from the atmospheric pressure environment. The turbomolecular pump is connected to the mass analysis module through an independent vacuum pipeline, which evacuates the quadrupole region to a high vacuum, reducing collisions between ions and gas molecules and ensuring ion transmission efficiency and mass resolution. The vacuum level of each module can be monitored in real time by a vacuum gauge, and then fed back to the control systems of the mechanical pump and turbomolecular pump for dynamic adjustment, thereby shortening the vacuum recovery time and ensuring long-term analytical stability.

[0030] Working Principle: First, through bidirectional interaction between the control module and the online calibration module, the mass axis and sensitivity can be dynamically calibrated in real time to ensure long-term detection accuracy. The radio frequency generator in the ion source module applies a high-frequency electromagnetic field to the argon gas inside the quartz torch tube via an induction coil, ionizing the argon gas to form high-temperature plasma. Simultaneously, the radio frequency generator is connected to the cooling module through stainless steel water-cooling pipes, ensuring the stable generation and maintenance of the high-temperature plasma within the quartz torch tube, ionizing the sample. At the same time, the sample aerosol is introduced into the plasma center channel through an atomizer to generate an ion beam. The ion beam is then transmitted to the mass analysis module via the ion extraction interface module. The ion beam then enters the quadrupole mass filter... Target ions are screened according to a specific mass-to-charge ratio (m / z) in an RF / DC electric field. The ion signal is converted into an electrical pulse and noise is reduced by the detection and signal processing module. The data is stored in the management module. An integrated online calibration system performs automatic calibration periodically to reduce signal drift and ensure long-term accuracy. Furthermore, a dynamic mass axis correction algorithm is used to adjust the mass spectrometry detection window in real time to avoid element signal overlap. The cooling module monitors the heat dissipation status and triggers a protection mechanism when the temperature exceeds the limit. The ion extraction interface module is connected to a mechanical pump through a metal vacuum pipeline to introduce ions from the atmospheric pressure environment into a low vacuum region (1-10 Pa), and then pumped to a high vacuum (10⁻⁻⁴ Pa) by a turbomolecular pump. 5 -10⁻ 6 The mass analysis module (Pa) uses a turbomolecular pump to maintain a stable operating temperature by naturally dissipating heat through metal heat sinks, and monitors the vacuum level of each module in real time through a vacuum gauge and feeds back to control the pump speed to ensure the stability of the gradient vacuum environment. In environmental monitoring scenarios, the frequency of the RF generator is optimized to 40.7MHz to ensure stable plasma combustion. Argon is used as the working gas, and a dual-layer atomization system is employed. The inner atomizing nozzle has an orifice diameter of 50μm, while the outer auxiliary airflow rate is 0.6L / min, effectively improving the atomization efficiency of the sample. The resolution of the quadrupole mass spectrometer filter is set to 10,000m / Δm. Combined with the mass resolution algorithm, this significantly reduces signal interference from non-target elements. The online calibration system automatically performs a calibration every 2 hours to continuously optimize the instrument's status. In vertical observation mode, the beam passes through the central region of the plasma, minimizing matrix influence and achieving a detection limit as low as the ppt level. This design is widely used in environmental monitoring, semiconductor manufacturing, biomedicine, and other fields to meet the needs of high-precision elemental analysis.

[0031] Finally, it should be noted that the above are merely preferred embodiments of the present utility model and are not intended to limit the present utility model. Although the present utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present utility model should be included within the protection scope of the present utility model.

Claims

1. An inductively coupled plasma mass spectrometer, comprising a control module, characterized in that: The control module is bidirectionally electrically connected to an online calibration module, a detection and signal processing module, a cooling module, and a vacuum module. The control module is unidirectionally electrically connected to a gas control module and a quality analysis module. The detection and signal processing module is unidirectionally electrically connected to a data storage and management module. The cooling module is unidirectionally electrically connected to the vacuum module.

2. The inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The online calibration module is electrically connected to the sample introduction module, and the gas control module is electrically connected to the sample introduction module. The sample introduction module includes a dual-layer atomization system. The atomizer used in the dual-layer atomization system is used to ensure the atomization efficiency of the sample and to actively cool and coordinate with the vertical optical path.

3. An inductively coupled plasma mass spectrometer according to claim 2, characterized in that: The sample introduction module is electrically connected to an ion source module, and the ion source module is electrically connected to a gas control module.

4. An inductively coupled plasma mass spectrometer according to claim 3, characterized in that: The plasma outlet of the ion source module is connected to the input of the ion extraction interface module via a sampling cone.

5. An inductively coupled plasma mass spectrometer according to claim 4, characterized in that: The ion extraction interface module is connected to the vacuum module via a vacuum pipeline, and the ion extraction interface module is connected to the quality analysis module via an ion transmission channel.

6. An inductively coupled plasma mass spectrometer according to claim 1, characterized in that: The quality analysis module is bidirectionally electrically connected to the vacuum module, and the quality analysis module is electrically connected to the detection and signal processing module.

7. An inductively coupled plasma mass spectrometer according to claim 4, characterized in that: The ion source module includes a radio frequency generator and a quartz torch. The vacuum module includes a mechanical pump, a turbomolecular pump, and a vacuum gauge. The radio frequency generator is connected to the cooling module via a stainless steel water-cooling pipeline. The induction coil of the radio frequency generator coaxially surrounds the quartz torch. The quartz torch ionizes argon gas through the electromagnetic field of the radio frequency generator to generate plasma. The mechanical pump is connected to the ion extraction interface module via a metal vacuum pipeline. The turbomolecular pump is connected to the cooling module via a metal heat sink. The turbomolecular pump is connected to the mass analysis module via an independent vacuum pipeline. The vacuum gauge is connected to the mechanical pump and the turbomolecular pump via signal connections.

Images