CN114883172A - Sample introduction control device and method for triple quadrupole mass spectrometer - Google Patents

Sample introduction control device and method for triple quadrupole mass spectrometer Download PDF

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Publication number
CN114883172A
CN114883172A CN202210583600.XA CN202210583600A CN114883172A CN 114883172 A CN114883172 A CN 114883172A CN 202210583600 A CN202210583600 A CN 202210583600A CN 114883172 A CN114883172 A CN 114883172A
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China
Prior art keywords
sample
ball valve
peristaltic pump
controlling
controller
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CN202210583600.XA
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Chinese (zh)
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成晓亮
鲁涵
徐强
张伟
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Zhejiang Pinyu Precision Technology Co ltd
Nanjing Pinsheng Medical Technology Co ltd
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Zhejiang Pinyu Precision Technology Co ltd
Nanjing Pinsheng Medical Technology Co ltd
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Priority to CN202210583600.XA priority Critical patent/CN114883172A/en
Publication of CN114883172A publication Critical patent/CN114883172A/en
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/26Mass spectrometers or separator tubes
    • H01J49/34Dynamic spectrometers
    • H01J49/42Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
    • H01J49/4205Device types
    • H01J49/422Two-dimensional RF ion traps
    • H01J49/4225Multipole linear ion traps, e.g. quadrupoles, hexapoles
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/025Detectors specially adapted to particle spectrometers
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/02Details
    • H01J49/04Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0431Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

The embodiment of the application provides a sampling control device and method of a triple quadrupole mass spectrometer. The front ball valve, the rear ball valve and the bidirectional peristaltic pump are controlled by the controller to change the sample conveying liquid path so as to clean the conveying liquid path and switch samples. The liquid level signal fed back by the liquid level sensor is analyzed through the controller, the waste liquid is pushed to the check valve and the waste liquid port from the sample conveying liquid path according to the waste liquid accumulation condition, the purity of the conveying liquid path is guaranteed, and therefore the purity degree of the sample after the sample passes through the conveying liquid path is guaranteed. The controller receives a sample temperature detection signal fed back by the temperature sensor, and sends a temperature adjusting signal to the temperature adjuster according to the sample temperature condition to keep the sample in a good physical state.

Description

Sample injection control device and method for triple quadrupole mass spectrometer
Technical Field
The application relates to the technical field of medical instruments, in particular to a sample injection control device and method of a triple quadrupole mass spectrometer.
Background
The triple quadrupole mass spectrometer is a detection instrument used in the fields of biology, aquatics, environmental science and technology and medical treatment. The mass-to-charge ratio of a sample to be tested is detected by means of substance gasification, electron bombardment and the like, so that the components of the sample to be tested are determined, and in order to improve the accuracy of a test result, a specific sample feeding device is adopted to provide the sample to be tested for a triple quadrupole mass spectrometer.
The sample introduction control device of the triple quadrupole mass spectrometer receives a sample to be tested through a sample introduction port of the device, so that the sample pollution is avoided in order to improve the purity degree of a conveying liquid path, cleaning liquid is injected into the sample conveying liquid path to wash impurities, and finally the impurities enter the triple quadrupole mass spectrometer through the sample introduction port of the triple quadrupole mass spectrometer. In this kind of sampling device, the link of washing conveying liquid way has been added, but there is the washing liquid waste liquid to get rid of incomplete condition to lead to the sample that awaits measuring to mix with the waste liquid after getting into sampling device, and then influence the test result.
When a sample to be detected enters the sample feeding device, the temperature of the sample to be detected and the ambient temperature can affect the physical state of the sample to be detected. Under the condition of higher or lower temperature, the sample to be detected can volatilize and degrade, so that the sample to be detected is insufficient in quantity; the sample to be tested is difficult to decompose due to abnormal temperature after entering the mass spectrometer, and the test result is influenced.
Disclosure of Invention
The application provides a sampling control device and method of a triple quadrupole mass spectrometer, which aim to solve the problem that the test result of the triple quadrupole mass spectrometer is inaccurate due to the fact that the quality of a sample to be tested is easily affected.
In a first aspect, an embodiment of the present application provides a sample injection control device for a triple quadrupole mass spectrometer, including: a sample introduction device and a control device; the sampling device comprises: the device comprises a communication pipeline, a waste liquid port, a one-way valve, a sample injection port, a two-way peristaltic pump, a ball valve, an ion source injection port and a cleaning liquid port; the control device includes: a controller, a sensor and a temperature regulator.
The waste liquid port is connected with the one-way valve through the communication pipeline; the one-way valve is connected with the sample injection port through the communication pipeline; the sample injection port is connected with the front ball valve through the communicating pipeline; the front ball valve is connected with the bidirectional peristaltic pump through the communicating pipeline; the bidirectional peristaltic pump is connected with the rear ball valve through the communication pipeline; the rear ball valve is connected with the ion source sample inlet through the communicating pipeline; the rear ball valve is connected with the cleaning liquid port through a communication pipeline.
The front ball valve, the rear ball valve and the bidirectional peristaltic pump are all electrically connected with the controller.
The sensor includes: photoelectric sensor, temperature sensor and liquid level sensor; the temperature sensor is arranged inside the sample injection port; the liquid level sensor is arranged inside the one-way valve; the temperature regulator is arranged at the sample injection port; the photoelectric sensor is arranged at the sample injection port and used for detecting whether a sample to be detected enters the sample injection port or not.
The controller is configured to:
if a detection signal fed back by the photoelectric sensor is received, judging that a sample to be detected enters the sample injection port, and switching to a sample injection mode;
sending a first control instruction for cleaning a conveying liquid path to the front ball valve, the bidirectional peristaltic pump and the rear ball valve; the first control instruction comprises: controlling the front ball valve to rotate to be communicated with the sample injection port; controlling the rear ball valve to rotate to be communicated with the cleaning liquid port; controlling the bidirectional peristaltic pump to reversely creep;
after the cleaning time is detected to reach a time threshold value, sending a second control instruction for conveying the sample to be detected to the rear ball valve and the bidirectional peristaltic pump; the second control instruction comprises: controlling the rear ball valve to rotate to be communicated with the ion source sample inlet; and controlling the positive peristalsis of the bidirectional peristaltic pump.
In a second aspect, an embodiment of the present application provides a sample injection control method for a triple quadrupole mass spectrometer, including:
if the controller receives a detection signal fed back by a photoelectric sensor arranged at the sample injection port, the sample to be detected at the sample injection port is judged to enter, and the sample injection mode is switched;
sending a first control instruction for cleaning a conveying liquid path to a front ball valve, a bidirectional peristaltic pump and a rear ball valve; the first control instruction comprises: controlling the front ball valve to rotate to be communicated with the sample injection port; controlling the rear ball valve to rotate to be communicated with the cleaning liquid port; controlling the bidirectional peristaltic pump to reversely creep;
after the cleaning time is detected to reach a time threshold value, sending a second control instruction for conveying the sample to be detected to the rear ball valve and the bidirectional peristaltic pump; the second control instruction comprises: controlling the rear ball valve to rotate to be communicated with the ion source sample inlet; and controlling the positive peristalsis of the bidirectional peristaltic pump.
According to the technical scheme, the embodiment of the application provides a sample introduction control device and method of a triple quadrupole mass spectrometer. The front ball valve, the rear ball valve and the bidirectional peristaltic pump are controlled by the controller to change the sample conveying liquid path so as to clean the conveying liquid path and switch samples. The liquid level signal fed back by the liquid level sensor is analyzed through the controller, the waste liquid is pushed to the check valve and the waste liquid port from the sample conveying liquid path according to the waste liquid accumulation condition, the purity of the conveying liquid path is guaranteed, and therefore the purity degree of the sample after the sample passes through the conveying liquid path is guaranteed. The controller receives a sample temperature detection signal fed back by the temperature sensor, and sends a temperature adjusting signal to the temperature adjuster according to the sample temperature condition to keep the sample in a good physical state.
Drawings
In order to more clearly explain the technical solution of the present application, the drawings needed to be used in the embodiments are briefly described below, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a sample injection control device of a triple quadrupole mass spectrometer provided in this embodiment;
fig. 2 is a sample injection mode flowchart of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment;
fig. 3 is a flow chart of waste liquid discharge control of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment;
fig. 4 is a sample switching mode control flowchart of the sampling control device of the triple quadrupole mass spectrometer provided in this embodiment;
fig. 5 is a flowchart of temperature control of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment.
Detailed Description
Reference will now be made in detail to embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following examples do not represent all embodiments consistent with the present application. But merely as exemplifications of systems and methods consistent with certain aspects of the application, as recited in the claims.
The triple quadrupole mass spectrometer is a detection instrument used in the fields of biology, aquatics, environmental science and technology and medical treatment. The mass-to-charge ratio of a sample to be tested is detected by means of substance gasification, electron bombardment and the like, so that the components of the sample to be tested are determined, and in order to improve the accuracy of a test result, a specific sample feeding device is adopted to provide the sample to be tested for a triple quadrupole mass spectrometer. When using sampling device, can lead to the quality of testing sample to go wrong and then influence the test result because the waste liquid discharge in the liquid way is not clean, the improper scheduling factor of introduction port temperature leads to. In order to solve the problem, the application provides a sample injection control device and a sample injection control method of a triple quadrupole mass spectrometer.
Fig. 1 is a schematic structural diagram of a sample injection control device of a triple quadrupole mass spectrometer. The sample introduction control device comprises a sample introduction device and a control device. The sampling device includes: the device comprises a communication pipeline 14, a waste liquid port 4, a one-way valve 5, a sample injection port 1, a two-way peristaltic pump 8, a front ball valve 6, a rear ball valve 7, an ion source injection port 3 and a cleaning liquid port 2. The control device includes: a controller 13, a sensor and a temperature regulator 12. The communicating pipe 14 is used for connecting the waste liquid port 4, the one-way valve 5, the sample injection port 1, the two-way peristaltic pump 8, the front ball valve 6, the rear ball valve 7, the ion source injection port 3 and the cleaning liquid port 2 to form a sample conveying liquid path. The edge of the inlet of the sample injection port 1 is provided with a groove for mounting a sensor.
The front ball valve 6, the rear ball valve 7 and the bidirectional peristaltic pump 8 are electrically connected with the controller 13 and can receive and identify signals sent by the controller 13, so that operations such as liquid path communication, conveying liquid path cleaning, sample conveying and the like are realized. The one-way valve 5 allows only one-way passage of waste liquid and other substances in the conveying liquid path for waste liquid discharge. The ion source sample inlet 3 is an inlet for a sample to enter the triple quadrupole mass spectrometer. The cleaning liquid port 2 is an inlet for the solution for cleaning the conveying liquid path to enter the conveying liquid path. The sensor is used for detecting whether a sample enters the sample injection port 1 or not, the one-way valve 5 and the liquid level in the conveying liquid path, so that the controller 13 can receive a detection signal fed back by the sensor to control the sample injection device. The temperature regulator 12 is used to change the temperature at the sample inlet or the sample temperature to avoid the influence of the sample due to improper temperature.
Fig. 2 is a sample injection mode flowchart of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment. The working flow of the sample injection device is described below with reference to the embodiment and fig. 1 and 2. In one embodiment, a sample to be detected enters the sample injection device from the sample injection port 1, the sample to be detected blocks an optical signal emitted by the photoelectric sensor 9 arranged at the sample injection port 1, the photoelectric sensor 9 generates a change in a signal fed back to the controller 13, and the controller 13 determines that the sample enters the sample injection port 1, so that the sample injection mode is switched.
When the triple quadrupole mass spectrometer is used for testing, various samples can be tested, and the sample inlets are required to be switched continuously, so that the number of the sample inlets can be automatically added according to the testing requirement. The photoelectric sensor 9 is used for detecting whether a sample enters the sample inlet and feeding back a signal to the controller 13, and the controller 13 judges whether the sample introduction device enters a sample introduction mode by receiving the feedback signal, so that the sample introduction device is an automatic device which takes the controller 13 as a core and takes each part as a controlled unit, the operation amount of workers is reduced, and the test efficiency is improved.
The sensor for detecting whether the sample enters the sample inlet 1 includes, but is not limited to, the photoelectric sensor 9, and other sensors with similar functions may also be used to detect the sample inlet condition of the sample inlet 1. The sensors can also be selected specifically according to the physical/chemical properties of the sample to be tested. For example, when a sample needing to be protected from light is moved to the sample inlet, in order to ensure the integrity of the sample, an ultrasonic sensor, a pneumatic sensor, or an electromechanical sensor may be used instead of the photoelectric sensor 9 for detection. In the same way, the sample inlets can be classified according to the difference of the sensors so as to adapt to more types of samples to be detected.
Before the controller 13 is not switched to the sample injection mode, although the front ball valve 6 and the rear ball valve 7 are connected to the communication pipeline 14, the valves of the front ball valve 6 and the rear ball valve 7 are in a closed state, and the delivery liquid paths of the sample injection device are not communicated. After the controller 13 switches to the sample injection mode, a first control command is issued. Wherein, the first control instruction is used for communicating the conveying liquid path and the sample. The device comprises a communication instruction sent by a controller 13 to a front ball valve 6 and a rear ball valve 7, so that the valves of the front ball valve 6 and the rear ball valve 7 are in a communication state, and a conveying liquid path of the sample feeding device is also switched to the communication state. After the sample enters the sample introduction device, the conveying liquid path is cleaned in order to avoid sample pollution, and therefore the rear ball valve 7 is communicated with the cleaning liquid port 2 firstly, so that the cleaning liquid flows into the conveying liquid path. When the conveying liquid path is communicated, the controller 13 also sends a signal of reverse peristalsis to the bidirectional peristaltic pump 8. The bidirectional peristaltic pump 8 introduces the cleaning liquid at the cleaning liquid port 2 into the conveying liquid path through reverse peristaltic motion to contact with the sample, and cleaning of the conveying liquid path is realized through peristaltic motion.
The front ball valve 6 is used for connecting the sample injection port 1 with the conveying liquid path and participating in controlling the connection/disconnection of the conveying liquid path, and because the number of the sample injection ports 1 can be changed according to the sample types tested by actual needs, the front ball valve is suitable for a plurality of sample injection ports 1, and the types of the front ball valve 6 can be changed accordingly. For example, when the number of the sample injection ports 1 is greater than two, a three-way ball valve or a four-way ball valve may be used instead of a common ball valve. When the number of the sample injection ports 1 is increased to be more, a plurality of three-way ball valves and four-way ball valves can be used in groups to communicate the sample injection ports with the liquid conveying path. The multi-way ball valve avoids the problem that a single sample injection port needs to be cleaned/replaced before receiving a sample to be tested at each time, and ensures that the purity of the sample also improves the testing efficiency.
In the cleaning process, the bidirectional peristaltic pump 8 continuously performs reverse peristalsis, the reverse peristalsis is beneficial to obtaining cleaning liquid from the cleaning liquid port 2, and meanwhile, liquid can be driven to flow in a liquid conveying path by means of peristalsis, so that the purpose of preventing sample pollution is achieved. In order to ensure the efficiency of the test, the cleaning time should not be too long, so that a time threshold is set in the controller 13 for controlling the cleaning time of the transport liquid path. Different time thresholds can be set for different types of samples so as to achieve better cleaning effect of the conveying liquid path. After entering the sample injection port, the sample can be temporarily left at the sample injection port, the time for cleaning the conveying liquid path reaches a preset time threshold, and then the sample enters the conveying liquid path through the sample injection port.
And (3) taking cleaning of a conveying liquid path by reverse peristalsis of the bidirectional peristaltic pump 8 as a timing starting standard, starting timing by the controller 13, and sending a second control instruction to the rear ball valve 7 and the bidirectional peristaltic pump 8 when cleaning time reaches a preset time threshold. The second control instruction is used to feed the sample into the ion source inlet 3. The method comprises the following steps: after control, the ball valve 7 and the cleaning liquid port 2 are switched to a turn-off state, and are switched to a communication state with the ion source sample inlet 3; controlling the positive peristalsis of the bidirectional peristaltic pump 8.
And the rear ball valve 7 is communicated with the ion source sample inlet 3 and is used for conveying a sample to the triple quadrupole mass spectrometer. The forward peristalsis of the bidirectional peristaltic pump 8 is also used for pushing the sample to move to the ion source sample inlet 3, and the purpose of preventing the sample from being polluted is achieved by accelerating the flow of the cleaning liquid in the conveying liquid path. The peristaltic speed of the bi-directional peristaltic pump 8 may also be adjusted based on signals from the controller 13.
The sampling control device of triple quadrupole mass spectrometer that this application embodiment provided still is provided with the sample and switches the mode to testing for many samples. In a multi-sample testing environment, the sample injection port 1 can be replaced, but the conveying liquid path is difficult to replace, and time is wasted. Therefore, it is necessary to discharge the waste liquid in the transport path after each sample transport. The sample switching mode can be switched to the controller 13 by an operator outside the device, and can also be automatically judged by the controller 13 according to the condition of the liquid level in the conveying liquid path, and can also be automatically judged by the controller 13 according to whether the sample enters the triple quadrupole mass spectrometer.
Fig. 3 is a waste liquid discharge control flow chart of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment. Fig. 4 is a sample switching mode control flowchart of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment. The waste liquid discharge and the mode switching will be described with reference to fig. 3 and 4 and the embodiment. In one embodiment, the operator has determined that a sufficient amount of sample has entered the triple quadrupole mass spectrometer and switches from the controller 13 which externally controls the sample introduction device to the sample switching mode. After the controller 13 switches to the sample switching mode, a third control instruction is sent to the rear ball valve 7 and the bidirectional peristaltic pump 8. The third control instruction is used for transferring the waste liquid in the conveying liquid path to the interior of the one-way valve 5 and the communication pipeline 14 close to the one-way valve 5. The method comprises the following steps: after control, the ball valve 7 and the ion source sample inlet 3 are switched to a turn-off state, and are switched to a communication state with the cleaning liquid port 2; controlling the bidirectional peristaltic pump 8 to reversely peristaltically. After the rear ball valve 7 and the cleaning liquid port 2 are switched to a communicated state, cleaning liquid can be supplemented properly to clean the conveying liquid path.
The controller 13 for controlling the sample injection device from the outside can be controlled by a key arranged outside the sample injection device, and can also be continuously controlled by setting a remote control mode. The key control mode is suitable for the conveying process of a common sample, and the remote control mode is more suitable for the situation that the sample has irritation, toxicity and the like and is not convenient for an operator to approach. The control modes of the remote control include but are not limited to: infrared, Bluetooth, wifi and other wireless communication technologies; also included, but not limited to: local area networks, buses, etc. The purpose of protecting the operator is realized through a remote control mode.
In an embodiment, the controller 13 may also determine the pressure based on a signal fed back from the liquid level sensor 11 disposed inside the check valve 5 and inside the communication pipe 14 close to the check valve 5. When a sample enters the triple quadrupole mass spectrometer, the rear ball valve 7 and the cleaning liquid port 2 are in a closed state, so that cleaning liquid does not enter a conveying liquid path any more, and the liquid level is kept consistent. When the controller 13 analyzes that the signal value fed back by the liquid level sensor 11 is kept unchanged within the preset time, the controller 13 judges that the sample is completely conveyed, automatically switches to a sample switching mode, prepares to clean the conveying liquid path, and discharges waste liquid. The preset time can be used for carrying out data statistics according to the time consumed by the conveying liquid path for conveying samples with the same category, volume and mass, and forming a data table for calling.
The sample introduction device does not necessarily have a transparent structure for protecting the sample, and therefore the position of the sample in the transport liquid path may not be visible. After the sample got into triple quadrupole mass spectrograph, triple quadrupole mass spectrograph can have the response, goes to adjust the mode of sampling device this moment again and can waste certain operating time unavoidably, influences the efficiency of test. Therefore, the liquid level sensor 11 is arranged in the conveying liquid path, information feedback is carried out from the inside of the sample feeding device through the link of confirming sample conveying through liquid level detection, and the controller 13 judges the conveying process to realize mode switching, so that the mode switching of the controller 13 is closely connected with the successful conveying of the sample, and the sample feeding efficiency and the testing efficiency are also improved without supervision of an operator.
In one embodiment, a sensor is provided at the ion source inlet 3 for sensing whether a sample enters, and the sensor feeds back a detection signal at the ion source inlet 3 to the controller 13. The sensor for sensing the sample is selected similar to the sensor at the sample injection port 1, and has the function of identifying that the sample enters the triple quadrupole mass spectrometer from the ion source injection port 3. And the sensors can also be selected specifically according to the physical/chemical characteristics of the sample to be tested. The controller 13 receives a detection signal fed back by a sensor at the ion source injection port 3, analyzes the information that the sample enters the triple quadrupole mass spectrometer, automatically switches to a sample switching mode, prepares for cleaning a liquid conveying path, and discharges waste liquid.
The method of arranging the sensor at the ion source injection port 3 can directly and accurately identify that the sample enters the triple quadrupole mass spectrometer. The liquid level sensor 11 may not be accurate in mode switching time when it is used because the type of the sample is rare and thus the preset time required for transferring the sample cannot be confirmed. In this application scenario, the method of setting a sensor at the ion source injection port 3 to identify a sample may replace a mode of reading a feedback signal of the liquid level sensor 11 to switch the operation modes.
After the controller 13 switches to the sample switching mode, the bidirectional peristaltic pump 8 receives a signal of reverse peristalsis, and starts reverse peristalsis to transfer the waste liquid in the conveying liquid path to the inside of the one-way valve 5 and the communication pipeline 14 close to the one-way valve 5. When the waste liquid is concentrated inside the check valve 5 and at the communicating pipe close to the check valve 5, the controller 13 further determines whether to discharge the waste liquid by the liquid level sensor 11 provided inside the check valve 5. The specific judgment method is as follows: a derived liquid level threshold value is set in the controller 13, the controller 13 analyzes the liquid level signal fed back by the liquid level sensor 11, and if the obtained liquid level value inside the check valve 5 is greater than or equal to the derived liquid level threshold value, it is determined that the derivation of the waste liquid can be started. The controller 13 issues a fourth control command to the forward ball valve 6 and the bidirectional peristaltic pump 8. The fourth control instruction is used to derive waste liquid and prepare the controller 13 to switch back to the sample entry mode. The method comprises the following steps: controlling the front ball valve 6 to be communicated with a new sample port; controlling the bidirectional peristaltic pump 8 to reversely peristaltically.
The ball valve 6 is communicated with a new sample port before control for the next sample conveying, and a new conveying liquid path is formed after the waste liquid is discharged. The control of the bidirectional peristaltic pump 8 to continue reverse peristalsis is to discharge the waste liquid in the one-way valve 5 and the waste liquid in the communication pipeline 14 close to the one-way valve 5 to the waste liquid port 4 through the power generated by peristalsis so as to realize the purpose of cleaning a conveying liquid path.
The sample injection control device provided by the embodiment is used for detecting the waste liquid residue in the conveying liquid path to a certain extent after the waste liquid is discharged from the conveying liquid path, so that a new sample is prevented from being polluted through the conveying liquid path. Therefore, before switching to the sample injection mode again, a sample injection level threshold is configured in the controller 13 to detect a waste liquid cleaning condition in the conveying liquid path. The concrete mode is as follows: the controller 13 receives and analyzes the liquid level signal fed back by the liquid level sensor 11, if the obtained liquid level inside the one-way valve 5 and the obtained liquid level inside the communicating pipeline 14 close to the one-way valve 5 are smaller than the sample injection liquid level threshold value, it is determined that the cleaning of the waste liquid in the liquid conveying path meets the standard, and the controller 13 is switched to the sample injection mode again. If the liquid level value obtained by analyzing the liquid level signal fed back by the liquid level sensor 11 is greater than or equal to the sample injection liquid level threshold value, determining that the waste liquid removal is not completed, continuously analyzing the liquid level signal fed back by the liquid level sensor 11 until the liquid level value obtained by analysis is less than the sample injection liquid level threshold value, and switching to a sample injection mode.
This link of waste liquid detection is favorable to the clearance of carrying the liquid way, can set up a plurality of level sensor 11 according to factors such as the length of carrying the liquid way, width, capacity to ensure that the detected value of feedback is effective. Corresponding processing algorithms can also be adopted according to the different quantity of the liquid level sensors 11, and the processing algorithms need to be formulated and finely adjusted according to actual conditions, which is not repeated herein.
In addition, when the sample enters the sample inlet 1, the temperature of the sample to be measured and the environmental temperature will affect the physical state of the sample. Under the condition of higher or lower temperature, the sample to be tested can volatilize and degrade, so that the sample to be tested is insufficient in quantity, and the test can not be realized. And the sample to be tested is difficult to decompose due to abnormal temperature after entering the mass spectrometer, so that the testing accuracy is influenced. In response to this problem, the embodiment of the present application provides a temperature sensor 10 at the sample inlet 1 for detecting the temperature of the sample and the temperature at the sample inlet 1. Fig. 5 is a flowchart of temperature control of the sample injection control device of the triple quadrupole mass spectrometer provided in this embodiment. The temperature control will be described with reference to fig. 5. The controller 13 receives and analyzes the temperature detection signal fed back from the temperature sensor 10, and determines whether or not the sample is within a proper temperature range.
The standard temperature of the sample is set in the controller 13 in advance according to the temperature range of the different kinds of samples. Each sample type corresponds to a sample standard temperature, and the sample standard temperature is a temperature range with an upper limit value and a lower limit value. The controller 13 determines whether the analyzed temperature value is within the sample standard temperature range. Under the condition that the temperature value is lower than the standard temperature of the sample, controlling the temperature regulator 12 to heat the sample and the sample inlet; and under the condition that the temperature value is higher than the standard temperature of the sample, controlling the temperature regulator 12 to cool the sample and the sample inlet. The device is suitable for heating or cooling, and the shape of the controlled component for heating or cooling can be selected according to the shapes of the sample injection port 1 and the conveying liquid path, so that the influence of the temperature on the sample is reduced to the minimum. Further, the controller 13 always performs a temperature control function, and even in the case where the sample temperature is within the sample standard temperature range, temperature detection is performed on the sample/sample injection port. Therefore, the temperature state of the sample and the sample injection port can be detected in real time, and the temperature can be controlled in time, so that the quality of the sample can be better ensured.
The embodiment of the application also provides a sampling control method of the triple quadrupole mass spectrometer, which is suitable for a sampling control device of the triple quadrupole mass spectrometer, and the sampling control method is suitable for a sample sampling mode and a sample switching mode of the sampling control device. The method for providing the sample feeding mode comprises the following steps:
if the controller 13 receives a detection signal fed back by an infrared sensor arranged at the sample injection port 1, the sample to be detected at the sample injection port is judged to enter, and the sample injection mode is switched;
sending a first control instruction for cleaning a conveying liquid path to the front ball valve 6, the bidirectional peristaltic pump 8 and the rear ball valve 7; the first control instruction comprises: controlling the front ball valve 6 to rotate to be communicated with the sample injection port 1; controlling the rear ball valve 7 to rotate to be communicated with the cleaning liquid port 2; controlling the bidirectional peristaltic pump 8 to reversely creep;
after the cleaning time is detected to reach a time threshold value, a second control instruction for conveying the sample to be detected is sent to the rear ball valve 7 and the bidirectional peristaltic pump 8; the second control instruction comprises: controlling the rear ball valve 7 to rotate to be communicated with the ion source sample inlet 3; controlling the bidirectional peristaltic pump 8 to peristaltically move in the forward direction.
The method provided for the sample switching mode includes:
if the controller 13 receives the sample switching signal, switching to a sample switching mode;
sending a third control instruction for transferring waste liquid to the rear ball valve 7 and the bidirectional peristaltic pump 8; the third control instruction includes: controlling the rear ball valve 7 to rotate to be communicated with the cleaning liquid port 2; controlling the bidirectional peristaltic pump 8 to reversely peristaltically.
According to the technical scheme, the embodiment of the application provides a sample introduction control device and method of a triple quadrupole mass spectrometer. The controller 13 controls the front ball valve 6, the rear ball valve 7 and the bidirectional peristaltic pump 8 to change the sample conveying liquid path so as to clean the conveying liquid path and switch samples. The liquid level signal fed back by the liquid level sensor 11 is analyzed through the controller 13, the waste liquid is pushed to the check valve 5 and the waste liquid port 4 from the sample conveying liquid path according to the waste liquid accumulation condition, the purity of the conveying liquid path is guaranteed, and therefore the purity degree of the sample after the conveying liquid path is guaranteed. The controller 13 receives the sample temperature detection signal fed back by the temperature sensor 10 and sends a temperature adjusting signal to the temperature regulator 12 according to the sample temperature condition to keep the sample in a good physical state.
The embodiments provided in the present application are only a few examples of the general concept of the present application, and do not limit the scope of the present application. Any other embodiments extended according to the scheme of the present application without inventive efforts will be within the scope of protection of the present application for a person skilled in the art.

Claims (9)

1. The utility model provides a triple quadrupole mass spectrometer's appearance controlling means that advances which characterized in that includes: a sample introduction device and a control device; the sampling device comprises: the device comprises a communication pipeline, a waste liquid port, a one-way valve, a sample injection port, a two-way peristaltic pump, a front ball valve, a rear ball valve, an ion source injection port and a cleaning liquid port; the control device includes: a controller, a sensor and a temperature regulator;
the waste liquid port is connected with the one-way valve through the communication pipeline; the one-way valve is connected with the sample injection port through the communication pipeline; the sample injection port is connected with the front ball valve through the communicating pipeline; the front ball valve is connected with the bidirectional peristaltic pump through the communicating pipeline; the bidirectional peristaltic pump is connected with the rear ball valve through the communicating pipeline; the rear ball valve is connected with the ion source sample inlet through the communicating pipeline; the rear ball valve is connected with the cleaning liquid port through the communicating pipeline;
the front ball valve, the rear ball valve and the bidirectional peristaltic pump are all electrically connected with the controller;
the sensor includes: photoelectric sensor, temperature sensor and liquid level sensor; the temperature sensor is arranged inside the sample injection port; the liquid level sensor is arranged inside the one-way valve; the photoelectric sensor is arranged in the inlet groove of the sample injection port and used for feeding back a detection signal when a sample to be detected enters the sample injection port;
the controller is configured to:
if a detection signal fed back by the photoelectric sensor is received, sending a first control instruction for cleaning a conveying liquid path to the front ball valve, the bidirectional peristaltic pump and the rear ball valve; the first control instruction is used for controlling the front ball valve and the sample injection port to be switched to a communicated state, controlling the rear ball valve to rotate and the cleaning liquid port to be switched to a communicated state, and controlling the bidirectional peristaltic pump to reversely wriggle;
after the cleaning time is detected to reach a time threshold value, sending a second control instruction for conveying the sample to be detected to the rear ball valve and the bidirectional peristaltic pump; and the second control instruction is used for controlling the rear ball valve and the ion source sample inlet to be switched to a communicated state and controlling the bidirectional peristaltic pump to peristaltically move forwards.
2. The sample injection control device of a triple quadrupole mass spectrometer of claim 1, wherein the controller is configured to:
when a sample to be detected is replaced, if a sample switching signal is received, sending a third control instruction for transferring waste liquid to the rear ball valve and the bidirectional peristaltic pump; and the third control instruction is used for controlling the rear ball valve and the cleaning liquid port to be switched to a communication state and controlling the bidirectional peristaltic pump to reversely creep.
3. The sample injection control device of a triple quadrupole mass spectrometer of claim 2, wherein the controller is further configured to:
when a sample to be detected is replaced, receiving a liquid level value fed back by the liquid level sensor;
analyzing a liquid level signal fed back by the liquid level sensor, and if the obtained liquid level value in the one-way valve is larger than or equal to a derived liquid level threshold value, sending a fourth control instruction for deriving waste liquid to the front ball valve and the bidirectional peristaltic pump; and the fourth control instruction is used for controlling the front ball valve and the new sample port to be switched to a communication state and controlling the bidirectional peristaltic pump to reversely creep.
4. The sample injection control device of a triple quadrupole mass spectrometer of claim 3, wherein the controller is further configured to:
and the front ball valve and the bidirectional peristaltic pump receive the liquid level signal fed back by the liquid level sensor during execution of the fourth control instruction, and judge whether the liquid level inside the one-way valve reaches a sample injection liquid level threshold value.
5. The sample injection control device of a triple quadrupole mass spectrometer of claim 4, wherein the controller is further configured to:
and analyzing the liquid level signal fed back by the liquid level sensor, and if the obtained liquid level value in the one-way valve is smaller than the sample injection liquid level threshold value, sending a control instruction for stopping creeping to the two-way peristaltic pump to wait for the sample to enter.
6. The sample injection control device of a triple quadrupole mass spectrometer of claim 1, wherein the controller is further configured to:
and judging that the sample inlet receives the sample temperature fed back by the temperature sensor when the sample to be measured enters, and if the sample temperature is not within the sample standard temperature interval, sending a control instruction to the temperature regulator to regulate the sample temperature.
7. The sample injection control device of a triple quadrupole mass spectrometer of claim 6, wherein the controller is further configured to:
analyzing a temperature signal fed back by the temperature sensor, and if the obtained sample temperature is greater than the upper limit value of the sample standard temperature interval, sending a cooling signal to the temperature regulator;
and if the obtained sample temperature is less than the lower limit value of the sample standard temperature interval, sending a heating signal to the temperature regulator.
8. A sample introduction control method of a triple quadrupole mass spectrometer is characterized by comprising the following steps:
if the controller receives a detection signal fed back by a photoelectric sensor arranged at the sample injection port, the sample to be detected at the sample injection port is judged to enter, and the sample injection mode is switched;
sending a first control instruction for cleaning a conveying liquid path to a front ball valve, a bidirectional peristaltic pump and a rear ball valve; the first control instruction comprises: controlling the front ball valve to rotate to be communicated with the sample injection port; controlling the rear ball valve to rotate to be communicated with the cleaning liquid port; controlling the bidirectional peristaltic pump to reversely creep;
after the cleaning time is detected to reach a time threshold value, sending a second control instruction for conveying the sample to be detected to the rear ball valve and the bidirectional peristaltic pump; the second control instruction comprises: controlling the rear ball valve to rotate to be communicated with an ion source sample inlet; and controlling the positive peristalsis of the bidirectional peristaltic pump.
9. The method according to claim 8, when the sample to be measured is replaced, further comprising:
if the controller receives a sample switching signal, switching to a sample switching mode;
sending a third control instruction for transferring waste liquid to the rear ball valve and the bidirectional peristaltic pump; the third control instruction includes: controlling the rear ball valve to rotate to be communicated with the cleaning liquid port; and controlling the bidirectional peristaltic pump to reversely peristaltically.
CN202210583600.XA 2022-05-25 2022-05-25 Sample introduction control device and method for triple quadrupole mass spectrometer Pending CN114883172A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210583600.XA CN114883172A (en) 2022-05-25 2022-05-25 Sample introduction control device and method for triple quadrupole mass spectrometer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210583600.XA CN114883172A (en) 2022-05-25 2022-05-25 Sample introduction control device and method for triple quadrupole mass spectrometer

Publications (1)

Publication Number Publication Date
CN114883172A true CN114883172A (en) 2022-08-09

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Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
CN (1) CN114883172A (en)

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