WO2017086393A1 - 分析装置及びその制御方法 - Google Patents

分析装置及びその制御方法 Download PDF

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Publication number
WO2017086393A1
WO2017086393A1 PCT/JP2016/084120 JP2016084120W WO2017086393A1 WO 2017086393 A1 WO2017086393 A1 WO 2017086393A1 JP 2016084120 W JP2016084120 W JP 2016084120W WO 2017086393 A1 WO2017086393 A1 WO 2017086393A1
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WIPO (PCT)
Prior art keywords
unit
drive circuit
field
temperature
ion
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Ceased
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PCT/JP2016/084120
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English (en)
French (fr)
Japanese (ja)
Inventor
プラカッシ スリダラ ムルティ
アヌープ アール． ヘッジ
佐藤　武
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Atonarp Inc
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Atonarp Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Atonarp Inc filed Critical Atonarp Inc
Priority to JP2017551925A priority Critical patent/JP6386195B2/ja
Priority to CN201680067410.5A priority patent/CN108352290B/zh
Priority to EP16866394.6A priority patent/EP3379562B1/en
Priority to US15/776,213 priority patent/US10847356B2/en
Priority to EP21168762.9A priority patent/EP3889996A1/en
Priority to EP20163789.9A priority patent/EP3686918B1/en
Publication of WO2017086393A1 publication Critical patent/WO2017086393A1/ja
Anticipated expiration legal-status Critical
Priority to US17/075,111 priority patent/US11011360B2/en
Priority to US17/235,023 priority patent/US11380533B2/en
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/14—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers
    • H01J49/147—Ion sources; Ion guns using particle bombardment, e.g. ionisation chambers with electrons, e.g. electron impact ionisation, electron attachment
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622—Ion mobility spectrometry
    • G01N27/623—Ion mobility spectrometry combined with mass spectrometry
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/022—Circuit arrangements, e.g. for generating deviation currents or voltages ; Components associated with high voltage supply
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/24—Vacuum systems, e.g. maintaining desired pressures

Definitions

  • the present invention relates to an analyzer such as a mass analyzer.
  • International Publication WO2015 / 029449 includes an ionization unit that ionizes molecules to be analyzed, a filter unit that selectively passes ions generated by the ionization unit, and a detection unit that detects ions that have passed through the filter unit.
  • An analysis apparatus wherein the detection unit includes a plurality of detection elements arranged in a matrix, and further includes a reconfiguration unit that switches a detection pattern including a detection element that enables detection among the plurality of detection elements.
  • An analytical device having the same is disclosed.
  • the ionization unit includes a plurality of ion sources, and the analyzer further includes a drive control unit that switches connection of the plurality of ion sources based on a change in the characteristics of the ion source.
  • Analyzing devices such as mass analyzers are always required to be smaller and more accurate.
  • One aspect of the present invention is an ionization unit that ionizes molecules to be analyzed, a filter unit that forms a field that selectively allows ions generated by the ionization unit to pass through, and a detector unit that detects ions that have passed through the filter unit. And an ion drive circuit that electrically drives the ionization unit, a field drive circuit that electrically drives the filter unit, a detector circuit that controls the sensitivity of the detector unit, and outputs of the ion drive circuit and the field drive circuit are controlled.
  • Control unit temperature detection unit for detecting the temperature around at least one of the ion drive circuit and field drive circuit, and temperature detection for the output setting of at least one of the ion drive circuit and field drive circuit Is an analysis device having a correcting unit for correcting, based on the temperature detected by knitting.
  • the correction unit may be implemented as one function of the control unit or may be implemented as an independent unit.
  • the correction unit may correct (compensate or adjust) all output settings of the ion drive circuit and the field drive circuit based on the detected temperatures.
  • Typical fields for selectively passing ions are an electric field, a magnetic field, and an electromagnetic field, and the field for selectively passing ions may include at least one of them.
  • each of the ion drive circuit and the field drive circuit varies slightly depending on the temperature of the substrate on which these circuits are mounted or the ambient temperature, and the present inventors compensate for them to drive each circuit. It was found that the linearity of the unit used can be improved and the detection accuracy can be improved. In addition, by adding a function to compensate the temperature of the output of these circuits, all or part of the analyzer including the ion drive circuit, field drive circuit, and control unit can be integrated into a handy type compact housing unit. Can be stored.
  • the analyzer has a detector circuit that controls the output sensitivity (gain) of the detector unit, the temperature detection unit includes a function to detect the temperature around the detector circuit, and the correction unit detects the sensitivity setting of the detector circuit as a temperature.
  • a unit (function) for correcting based on the temperature detected by the unit may be included.
  • Another aspect of the present invention includes a sensor housing in which an ionization unit, a filter unit, and a detector unit are accommodated in order, a chamber in which the sensor housing is accommodated, a decompression unit that decompresses the inside of the chamber, and an ionization of the sensor housing.
  • It is an analyzer having a capillary for flowing a gas containing a molecule to be analyzed in or near the unit.
  • the state in the chamber can be controlled more stably.
  • the chamber capacity is sufficiently large with respect to the sensor housing to keep the conditions in the sensor housing constant.
  • the pressure in the chamber is feedback controlled, it is desirable that the state in the sensor housing appears in the chamber, and it is desirable that the chamber capacity Vc be as close as possible to the sensor housing capacity Vh.
  • the ratio Vc / Vh is preferably in the range of 1.5 to 10, and more preferably in the range of 1.5 to 5. This method makes it possible to reduce the chamber size and greatly reduce the size of the entire system.
  • One of the different embodiments of the present invention is an analyzer that further includes a unit that stabilizes the emission current of the ionization unit via an ion drive circuit.
  • the control unit may include a function as a stabilizing unit, or may be an independent unit.
  • the analyzer includes an ionization unit that ionizes molecules to be analyzed, a filter unit that forms a field for selectively passing ions generated by the ionization unit, a detector unit that detects ions that have passed through the filter unit, and an ionization unit.
  • An ion drive circuit that electrically drives the unit, a field drive circuit that electrically drives the filter unit, a control unit that controls the output of the ion drive circuit and the field drive circuit, and at least one of the ion drive circuit and the field drive circuit
  • a temperature detection unit that detects a temperature around one circuit, and the control method includes correcting the output setting of at least one circuit based on the temperature detected by the temperature detection unit.
  • FIG. 1 shows an example of a gas analyzer (gas analysis system).
  • This analyzer 1 is a mass spectrometer having a built-in quadrupole mass sensor, and is intended to quantitatively analyze the components (molecules) of the gas 5 guided by the capillary 9.
  • the analysis system 1 includes a quadrupole mass sensor (hereinafter referred to as a sensor) 10, a control box 20 that drives the sensor 10 and analyzes data obtained from the sensor 10, a chamber 30 that houses the sensor 10, A turbo pump (turbomolecular pump) 31 and a diaphragm pump (rough pump) 32 which are connected to the chamber 30 by a communication pipe 38 and depressurize the interior of the chamber 30 (rough pressure pump) 31, and the internal pressure of the chamber 30 are monitored.
  • a quadrupole mass sensor hereinafter referred to as a sensor
  • a turbo pump turbomolecular pump
  • a diaphragm pump a diaphragm pump
  • a pressure gauge 33, a terminal block 35 for connecting wiring inside and outside the apparatus, and a power supply unit 36 are included, and these are housed in a rectangular housing (housing unit) 50.
  • the size of the housing unit 50 is about 300 mm ⁇ 150 mm ⁇ 150 mm, and conventional mass analyzers of a metric size are grouped into a size called a handy type that is compact and portable.
  • the sensor 10 includes an ionization unit 11 that ionizes molecules of the gas 5, an ion lens 12, a quadrupole filter 13, a Faraday cup 14 that is an ion detector, and a cylindrical (tubular) shape that sequentially stores these.
  • Sensor housing 19 The ionization unit 11 includes a filament serving as an ion source, and thermoelectrons emitted from the filament collide with molecules to be analyzed to be ionized.
  • the quadrupole filter 13 is a filter unit that forms a field (field) through which ions are selectively passed. In this example, a quadrupole electric field is formed as a field through which ions are selectively passed.
  • the quadrupole filter 13 forms a quadrupole electric field having a DC component and a high-frequency component in a space surrounded by a set of four electrodes.
  • the ions pass along the central axis of the quadrupole electric field, the ions repeatedly receive a converging force and a diverging force in a direction orthogonal to the velocity.
  • the mass-to-charge ratio Ions selectively pass through the quadrupole electric field and reach the ion detector 14, and the amount of ions reached is measured as an ion current.
  • the sensor 10 is mounted such that the sensor housing 19 penetrates one wall surface of the cubic chamber 30 and almost the entire sensor housing 19 is accommodated in the chamber 30.
  • a capillary 9 is connected to the tip of the sensor housing 19 (on the side of the ionization unit 11), and the gas 5 introduced by the capillary 9 flows out into the chamber 30 through the sensor housing 19.
  • the sensor housing 19 has, for example, a gap for attaching the filament of the ionization unit 11, an opening 15 provided in the vicinity of the ion detector 14 or the filter unit 13, and communicates with the chamber 30 through them.
  • the interior of the housing 19 is basically maintained in the same reduced pressure atmosphere as the chamber 30.
  • the gas 5 introduced through the capillary 9 is first introduced into the sensor housing 19, released into the chamber 30, and then released out of the system by a turbo pump 31 or the like. Therefore, the gas circulating in the chamber 30 does not enter the sensor housing 19, and the component of the gas 5 supplied through the capillary 9 can be analyzed with high accuracy in real time.
  • the rear side of the sensor housing 19 is attached to the control box 20 via an attachment pipe 28 that stores wiring.
  • the control box 20 electrically connects a Pirani board 23 for controlling a pressure gauge (pressure monitor) 33, an ion drive board 24 equipped with an ion drive circuit 61 for electrically driving the ionization unit 11, and the quadrupole filter 13.
  • a field drive board 25 on which a field drive circuit 62 including an RF drive unit (RF unit) 62r to be driven is mounted, and a detector board 26 on which a detector circuit 63 for controlling the output sensitivity (gain) of the ion detector 14 is mounted.
  • the temperature sensor 27 is an infrared thermopile sensor, which detects the temperature in the control box 20 as a representative value (peripheral temperature of each circuit), but detects the infrared rays from each board to determine the temperature of each board. It may be detected as the ambient temperature of the circuit.
  • a temperature sensor such as an infrared sensor, a thermocouple, or a resistance temperature detector element is attached to each board, for example, the ion drive board 24, the field drive board 25, and the detector board 26, and the periphery of the circuit mounted on each board. You may acquire the temperature.
  • the analysis system 1 further controls the internal pressure of the chamber 30 and temperature control of a heater 39 for heating a vacuum system such as the chamber 30 and a pipe 38 connecting the chamber 30 and a turbo pump (turbomolecular pump) 31.
  • the vacuum / temperature control interface unit 55 that performs the above-described operation and the fan 53 that controls the temperature by ventilating the interior of the housing 50 are included.
  • the vacuum / temperature control interface unit 55 includes a function of monitoring the temperature of the chamber 30 by a temperature sensor, typically an infrared thermopile sensor 34, provided to measure the temperature inside the chamber 30.
  • FIG. 2 shows an electrical system configuration of the analyzer 1.
  • the microcontroller (control unit) 22 manages the operation of the analyzer 1 by controlling the outputs of the circuits 61, 62, and 63 according to the measurement target of the sensor 10, environmental conditions, etc. in cooperation with the CPU subsystem 21. Including a unit (function) 22x.
  • the operation management unit 22x includes a function (unit) for changing the mass-to-charge ratio passing through the filter unit 13 in order and operating the analyzer 1 in the scan mode.
  • the analysis apparatus 1 includes communication interfaces 21 y and 22 y of various standards such as USB, SD card, HDMI (registered trademark), Ethernet (registered trademark), RS485, and the like.
  • the microcontroller 22 is a pressure / temperature control unit (pressure / temperature control function) that feedback-controls the degree of vacuum and temperature of the chamber 30 based on information obtained from the pressure monitor 33 and the vacuum / temperature control interface unit 55. 22a is included.
  • the pressure / temperature control unit 22a controls the capacities of the pumps 31 and 32 in order to control the degree of vacuum.
  • the pressure / temperature control unit 22a mainly controls the turbo molecular pump 31 on the high vacuum side to control a predetermined vacuum. Control to keep the degree.
  • the pressure / temperature control unit 22a controls the output of the heater 39 so as to keep the temperature of the chamber 30 constant.
  • the measurement conditions are stabilized and the above-described problems are solved. That is, first, by reducing the volume of the chamber 30, fluctuations in conditions inside the chamber 30 can be captured more sensitively by the pressure monitor 33 and / or the temperature sensor 34. By improving the accuracy of feedback control based on the degree of vacuum and temperature of the chamber 30 in the control of the vacuum pumps 31 and 32 that are pressure reducing units, the conditions in the chamber 30 can be stabilized. Furthermore, by reducing the capacity of the chamber 30, it is possible to measure the fluctuation of the gas component in real time with higher accuracy. In addition, by reducing the capacity of the chamber 30, there is also an advantage that the analysis system 1 can be compactly packed so as to be portable. It is desirable that the volume Vc of the chamber 30 and the volume Vh of the sensor housing 19 satisfy the following conditions. 1.5 ⁇ Vc / Vh ⁇ 10 (1) The upper limit of condition (1) is preferably 8, more preferably 5, and even more preferably 3.
  • the pressure monitor 33 for monitoring the internal pressure of the chamber 30 is configured to monitor the pressure in the region outside the sensor housing 19 in the chamber 30.
  • the pressure of the gas 5 supplied from the capillary 9 fluctuates, the influence appears after flowing out into the chamber 30 through the sensor housing 19, and the chamber 30 has a small capacity, but the capacity with respect to the capillary 9 is small. Large and rapid pressure fluctuations are suppressed. Therefore, the monitored pressure fluctuation is suppressed, and in response to this, it is possible to suppress sudden control of the turbo pump 31 that controls the internal pressure of the chamber 30 among the vacuum pumps 31 and 32 that are pressure reducing units. 9 can smoothly cope with pressure fluctuations of the gas 5 supplied from the gas generator 9.
  • the microcontroller 22 further sets the output setting of the ion drive circuit 61 and the field drive circuit 62 and the sensitivity setting (gain setting) of the detector circuit 63 to the temperature around the circuit detected by the temperature detection unit (temperature sensor) 27.
  • a correction unit (correction function, compensation function, adjustment unit) 22b that performs correction (compensation and adjustment) based on each is included.
  • the correction unit 22b sets the output settings of the ion drive circuit 61 and the field drive circuit 62 and the gain settings of the detector circuit 63 in advance in the range of 0 ° C. to 80 ° C. every 10 ° C. Correction is performed with reference to the lookup table 69 in which the correction amount of the set value is stored. Instead of the lookup table 69, another correction value such as a function may be calculated or output.
  • the output (voltage and / or current) of the RF drive unit 62r may fluctuate slightly depending on the environmental temperature where the field drive circuit 62 including the RF drive unit 62r is installed, and the linearity with respect to the AMU may be reduced. This error can cause measurement errors.
  • the correction unit 22b refers to the compensation value (output set value, correction value, or difference) of the lookup table 69 obtained in advance based on the environmental temperature (ambient temperature) of the RF drive unit 62r, and the RF drive unit 62r
  • the output setting value base value, base curve
  • the output setting value is output from the RF drive unit 62r even if the environmental temperature fluctuates by changing the output setting value for the AMU within a predetermined range depending on the temperature.
  • the linearity of the RF voltage, DC + voltage, and DC ⁇ voltage with respect to the AMU is maintained.
  • this analyzer 1 although it is a quadrupole type mass analyzer, quantitative analysis that has been impossible in the past is made possible.
  • a quadrupole electric field but also a voltage or current that forms (drives) a field (field) such as an electric field, a magnetic field, or an electromagnetic field that selectively allows ions to pass through or is retained, AMU, mass-to-charge ratio, ions
  • a field such as an electric field, a magnetic field, or an electromagnetic field that selectively allows ions to pass through or is retained
  • AMU mass-to-charge ratio
  • ions When controlling by the characteristics of ions or molecules such as mobility, the signal or information that controls the voltage or current to be driven by the temperature around the circuit is relatively controlled by the temperature or temperature difference, thereby controlling the field.
  • the temperature dependence of the voltage or current for driving can be suppressed, and a more accurate field can be formed in the filter unit 13.
  • the sensitivity and tendency with respect to the environmental temperature may differ from the field drive circuit 62, but the output may fluctuate.
  • the filament voltage and / or the filament current of the ionization unit 11 may fluctuate, and the setting of the voltage and current value, for example, the base curve or the base value is corrected by the temperature by the correction unit 22b. Or you can compensate.
  • the detector circuit 63 can correct or compensate the gain of the Faraday cup and / or the electron multiplier which is the detector 14 and the amplification amount (gain) of the output signal by temperature.
  • the compensation unit 22b compensates the set values for these circuits 61 and 63 in the same manner as the field drive circuit 62 to ensure linearity.
  • the microcontroller (control unit) 22 further includes a stabilization unit 22c that stabilizes an emission current Ea indicating the ionization capability of the ionization unit 11 via the ion drive circuit 61.
  • the emission current Ea is controlled to 0.1%, that is, the nA level.
  • the amount of ions input to the filter unit 13 can be kept substantially constant. For this reason, the amount of various ions separated by the filter unit 13 and detected by the detector unit 14, that is, the content (content ratio) in the gas 5 can be obtained quantitatively with high accuracy.
  • the ionization unit 11 of this example is a system that outputs thermoelectrons using a filament.
  • the stabilization unit 22c measures, for example, an ion box current as the emission current Ea, and the emission current Ea is equal to the target current Et.
  • a first stabilization unit (convergence unit) 22d that controls the filament voltage Fv stepwise in accordance with a preset look-up table or the like so as to be within ⁇ 1%, and the emission current Ea is ⁇ 0.
  • a second stabilization unit (feedback control unit) 22e that moves the filament voltage Fv by a minute amount ( ⁇ f) by feedback control so as to be within 1%.
  • An example of feedback control is PID (proportional-integral-derivative control).
  • FIG. 3 shows a more detailed configuration of the ion drive circuit 61 and the detector circuit 63 in a block diagram.
  • the ionization unit 11 includes a filament 11f disposed in the ion box 11b and a repeller electrode 11r.
  • the gas 5 input to the sensor 10 by the capillary 9 is ionized by the ionization unit 11, and the generated ion stream (ionized gas) 3 is transferred to the field (quadrupole electromagnetic field) 13 f of the filter unit 13 by the ion lens 12.
  • the field 13 f the field 13 f of the filter unit 13 by the ion lens 12.
  • Ions separated or selected by the field 13f arrive at the detector unit 14 and are observed as an ion current flowing between the collector 14c.
  • the ion drive circuit 61 includes a driver unit 61a that supplies power to the elements constituting the ionization unit 11, and a monitor / control unit 61b that monitors and controls the ionization unit 11.
  • the driver unit 61a supplies filament driving power to the two filaments 11f via the filament output control units 71a and 71b, sets the repeller voltage of the repeller electrode 11r, and further, the ion box 11b and the ion lens 12 Set the voltage.
  • Filament output control units 71a and 71b each include a MOSFET switch for immediately shutting down each filament power.
  • the ion drive circuit 61 includes a circuit 72 that measures the filament voltage Vf and the filament current If. In this example, the ion drive circuit 61 feeds back to the microcontroller 22 via the monitor / control unit 61b.
  • the ion driver circuit 61 includes circuits 73 and 74 for measuring the ion box current I1 and the ion lens current I2, respectively. In this example, the ion driver circuit 61 feeds back to the microcontroller 22 via the monitor / control unit 61b.
  • the filament output control units 71a and 71b control the voltage Vf supplied to each filament 11f as an output, and monitor the filament current If.
  • the filament voltage Vf is controlled so as to be increased or decreased stepwise when the analyzer 1 is started and stopped.
  • the filament voltage Vf is controlled to a voltage that can emit thermoelectrons capable of ionizing molecules to be measured.
  • the emission current Ea is controlled to be constant.
  • the ion box current I1 and / or the ion lens current I2 can be referred to. Since the ion box current I1 is close to the filament 11f, the current value is large, and a change as the emission current Ea is easily captured.
  • the emission current Ea excluding the influence of thermoelectrons from the ion box current I1 is obtained.
  • the filament voltage Vf is controlled such that the emission current Ea is constant, for example, the error is 0.1% or less or less than 0.1% with respect to the target current Et, that is, the error is nA level.
  • Such emission current control may be realized by the stabilization unit 22 c of the microcontroller 22 as described above, or may be realized by the monitor / control unit 61 b of the ion driver circuit 61.
  • the monitor / control unit 61b receives the correction signal S1 based on the temperature of the ion drive circuit 61 itself or its surroundings from the correction unit 22b, and corrects the reference voltage of the filament voltage Vf.
  • the RF unit (RF power amplifier) 62 r receives the correction signal S 1, corrects the output settings such as the voltage and frequency that are the reference of the RF output, and includes the field drive circuit 62. Suppresses fluctuations due to the temperature around the substrate.
  • the detector circuit 63 includes an amplifier 75 that amplifies the ion current I3 obtained by the detector 14 and a gain controller 76 that controls the gain of the amplifier 75.
  • the gain controller 76 receives the correction signal S1 and determines the gain of the amplifier 75.
  • the setting is corrected by the temperature around the circuit board including the detector circuit 63, and the influence of the temperature around the circuit board on the output of the amplifier 75 is suppressed.
  • the amplifier 75 can employ, for example, a combination of TIA (transimpedance amplifier) and VGA (variable gain amplifier) that can adjust the gain and has high linearity.
  • FIG. 4 is a flowchart showing an outline of control (processing) performed by the microcontroller (control unit) 22 of the analyzer 1.
  • the operation management unit 22x operates the analyzer 1 in the scan mode, and sequentially detects molecules (components) having different mass-to-charge ratios.
  • the field drive circuit 62 controls the quadrupole electric field 13f of the filter unit 13 so that ions having different mass-to-charge ratios pass through the filter unit 13 in order and reach the detector unit 14.
  • step 81 the temporal change of the component of the gas 5 is monitored, or the average value of the component is often acquired at an appropriate time interval, and the scan is repeated.
  • the correction unit 22b performs a process of correcting the set value according to the temperature around each of the circuits 61 to 63.
  • the stabilization unit 22c performs processing for maintaining the emission current Ea constant.
  • FIG. 5 shows in more detail a process 82 for correcting circuit output settings (setting values, basic parameters, base curves, etc.) according to the ambient temperature of the circuit (board).
  • step 85 the temperature of the board on which the respective circuits 61 to 63 are mounted or the ambient temperature is detected.
  • the correction unit 22 b refers to the lookup table 69, and sets a basic set value for calculating the output set value of the ion drive circuit 61, for example, the filament voltage Vf, with respect to the detected temperature. If it is necessary to change, a correction instruction (correction signal) S1 is output to the ion drive circuit 61 in step 86a.
  • step 87 if it is necessary to correct or change the setting value of the field drive circuit 62, in this example, the RF unit 62r, based on the detected circuit ambient temperature, the field drive circuit 62 is corrected in step 87a. Give instructions.
  • step 88 if it is necessary to correct or change the sensitivity (gain) of the detector circuit 63 based on the detected circuit ambient temperature, a correction instruction is issued to the detector circuit 63 in step 88a.
  • the correction unit 22b may correct only the output or sensitivity of one or two of the circuits 61 to 63 whose output or sensitivity is greatly affected by the ambient temperature.
  • FIG. 6 shows the process 83 for stabilizing the emission current Ea of the ionization unit 11 in more detail.
  • the operation management unit 22x sets the filament voltage Vf to the target value, and the ion drive circuit 61 drives (drives) the ionization unit 11 with the set filament voltage Vf.
  • the target value is set by a sequence that raises or lowers the filament voltage Vf in stages if the analyzer 1 is being started or is being prepared to stop.
  • a predetermined emission current Ea is set to a voltage at which a predetermined emission current Ea is obtained according to the life management schedule of the filament 11f.
  • step 92 the stabilization unit 22c calculates a difference ⁇ E between the target emission current value Et and the actual emission current value Ea. If the difference ⁇ E does not fall within 1% in step 93, the filament voltage Vf is increased or decreased stepwise at a predetermined interval in step 94 (convergence processing).
  • step 93 If it is determined in step 93 that the difference ⁇ E is less than 1%, the convergence process is terminated, and the process proceeds to the feedback control in step 95.
  • the PID loop is executed.
  • step 96 the filament voltage Vf is corrected by obtaining the difference ⁇ Vf of the filament voltage Vf that is the output of the PID control.
  • step 97 the difference ⁇ E of the emission current Ea is recalculated. If the difference ⁇ E is less than 0.1% in step 98, the ion drive circuit 61 drives (drives) the ionization unit 11 with the set filament voltage Vf. )
  • step 98 If it is determined in step 98 that the difference ⁇ E is 0.1% or more, if the difference ⁇ E is less than 1% in step 99, the process moves to step 95 to correct the filament voltage Vf by feedback control. On the other hand, if the difference ⁇ E is 1% or more, the process returns to step 92 so that the emission current Ea converges to the target value Et in a short time by a convergence process in which the filament voltage Vf is corrected stepwise. With these processes, in steady measurement, the error of the emission current Ea of the analyzer 1 can be reduced to less than 0.1%, and the emission current Ea can be managed at approximately nA level.
  • the analytical apparatus 1 capable of quantitative analysis can be provided.
  • the filter unit 13 of the analyzer 1 has been described based on an example in which a quadrupole electric field is formed as a field 13f for ion separation or selection.
  • the field 13f has a sector magnetic field type and an electric field magnetic field two. It may be an electric field or a magnetic field such as a double convergence type or a time-of-flight type.
  • the filter unit 13 may form an electric field and a magnetic field (electromagnetic field) as the ion selection field 13f like a Wien filter.
  • the filter unit 13 may form an electric field of a type for selecting ions based on ion mobility instead of the mass to charge ratio as the field 13f.
  • the filter unit 13 may be a non-vacuum type filter unit 13 such as FAIMS. There may be.
  • the filter unit 13 may be formed by combining a plurality of types of different fields 13r.
  • the analyzer 1 includes a housing (housing unit) 50 in which the sensor 10, the control box 20, the vacuum pumps 31 and 32, etc. are integrated into a handy type size.
  • the control box 20 can be separated from the control box 20 and housed in each of the more compact housings, and the circuit group can maintain accuracy with respect to fluctuations in ambient temperature, so that various arrangements can be handled.
  • An example of the sensor 10 is a compact one having a size of about several centimeters, but the sensor 10 may be a MEMS type that is even smaller.
  • the analyzer 1 may be a handy type, and may be a portable terminal or a wearable size.

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PCT/JP2016/084120 2015-11-17 2016-11-17 分析装置及びその制御方法 Ceased WO2017086393A1 (ja)

Priority Applications (8)

Application Number Priority Date Filing Date Title
JP2017551925A JP6386195B2 (ja) 2015-11-17 2016-11-17 分析装置及びその制御方法
CN201680067410.5A CN108352290B (zh) 2015-11-17 2016-11-17 分析装置及其控制方法
EP16866394.6A EP3379562B1 (en) 2015-11-17 2016-11-17 Analysis device and control method therefor
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