WO2012108050A1 - 四重極型質量分析装置 - Google Patents
四重極型質量分析装置 Download PDFInfo
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- WO2012108050A1 WO2012108050A1 PCT/JP2011/052930 JP2011052930W WO2012108050A1 WO 2012108050 A1 WO2012108050 A1 WO 2012108050A1 JP 2011052930 W JP2011052930 W JP 2011052930W WO 2012108050 A1 WO2012108050 A1 WO 2012108050A1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
- H01J49/34—Dynamic spectrometers
- H01J49/42—Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
- H01J49/4205—Device types
- H01J49/421—Mass filters, i.e. deviating unwanted ions without trapping
- H01J49/4215—Quadrupole mass filters
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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
- H01J49/022—Circuit arrangements, e.g. for generating deviation currents or voltages ; Components associated with high voltage supply
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
- H01J49/34—Dynamic spectrometers
- H01J49/42—Stability-of-path spectrometers, e.g. monopole, quadrupole, multipole, farvitrons
- H01J49/4205—Device types
- H01J49/421—Mass filters, i.e. deviating unwanted ions without trapping
Definitions
- the present invention relates to a quadrupole mass spectrometer using a quadrupole mass filter as a mass separator for separating ions according to the mass to charge ratio m / z.
- the quadrupole mass spectrometer is a mass spectrometer that uses a quadrupole mass filter to separate ions according to the mass-to-charge ratio.
- FIG. 6 shows a schematic configuration of a quadrupole mass spectrometer.
- Various ions generated from the sample in the ion source 1 are introduced into a quadrupole mass filter 2 including four rod electrodes 2a, 2b, 2c, and 2d through an ion transport optical system (not shown).
- a voltage ⁇ (U + V ⁇ cos ⁇ t) in which a high frequency voltage ⁇ V ⁇ cos ⁇ t and a DC voltage ⁇ U are superimposed is applied from the quadrupole power supply unit 4 to the four rod electrodes 2a to 2d, and a specific value corresponding to the voltage is applied. Only ions having a mass to charge ratio selectively pass through the quadrupole mass filter 2. The detector 3 detects ions that have passed through and acquires a detection signal corresponding to the amount of ions.
- the control unit 5 when performing scan measurement over a predetermined mass-to-charge ratio range, changes the amplitude value V of the high-frequency voltage V ⁇ cos ⁇ t and the DC voltage value U so as to change while maintaining a certain relationship.
- the multipole power supply unit 4 is controlled. Thereby, the mass-to-charge ratio of ions passing through the quadrupole mass filter 2 is scanned within a predetermined mass-to-charge ratio range.
- the data processing unit 6 creates a mass spectrum with the horizontal axis representing the mass-to-charge ratio and the vertical axis representing the ion intensity.
- FIG. 7 is a schematic block diagram of a conventional general quadrupole power supply unit 4 (see Patent Documents 1 and 3).
- coils 10 and 12 having an inductance L and capacitors 11 and 13 having a capacitance C ′ are connected to the output stage of the quadrupole power supply unit 4.
- the capacitance C in the rod electrodes 2a to 2d is a combination of the capacitance C 'of the capacitors 11 and 13 and the floating capacitance of the rod electrodes 2a to 2d.
- the LC resonance circuit is formed by the series circuit of the synthesized capacitance C and inductance L, the rod electrodes 2a to 2d have a voltage in which a high frequency voltage and a DC voltage resonated by the LC resonance circuit are superimposed. Will be applied.
- (1) the frequency f of the high frequency voltage to be injected is fixed, and the inductances of the coils 10 and 12 or the capacitances of the capacitors 11 and 13 are adjusted to achieve tuning.
- the frequency variable tuning method (2) is often used.
- the conventional quadrupole power supply unit using the variable frequency tuning method has the following problems.
- FIG. 8 shows a circuit configuration of a quadrupole power supply unit 4 that employs a conventional frequency variable tuning method (see Patent Documents 1 and 2).
- a detection unit 4D including a diode bridge rectifier circuit 401 and detection capacitors 402 and 403 detects a voltage value (hereinafter referred to as “V voltage”) of a high-frequency voltage applied to the quadrupole mass filter 2.
- V voltage a voltage value of a high-frequency voltage applied to the quadrupole mass filter 2.
- the detection output converted to DC is fed back to the high frequency power supply unit 4A and the DC power supply unit 4B via the detection gain adjustment unit 4C.
- the detection gain adjustment unit 4C includes a V voltage detection resistor 404, a V voltage adjustment amplifier 405, and a V voltage adjustment variable resistor 406.
- the high frequency power supply unit 4A includes a buffer amplifier 407, an m / z axis adjustment variable resistor 408, a V voltage comparison amplifier 409, a multiplier 410, a high frequency voltage signal generator 411, a buffer amplifier 412, a drive circuit 413, and a high frequency transformer 414.
- the DC power supply unit 4B includes an inverting amplifier 415, a positive DC voltage amplifier 416, and a negative DC voltage amplifier 417.
- the frequency f of the high-frequency voltage supplied from the secondary coil of the high-frequency transformer 414 to the LC resonance circuit including the quadrupole mass filter 2 is determined by the frequency of the rectangular wave signal generated by the high-frequency voltage signal generator 411.
- the voltage value of the high-frequency voltage is determined by the voltage supplied from the V voltage comparison amplifier 409 to the multiplier 410.
- the output voltage of the V voltage comparison amplifier 409 includes a detection output fed back from the detection unit 4D, a power supply control voltage (Qcont) corresponding to a target mass-to-charge ratio given from the control unit 5, and a variable resistor for adjusting the V voltage. 406 and the adjustment position of the variable resistor 408 for m / z axis adjustment.
- the V voltage adjustment variable resistor 406 has a function of adjusting a gain for amplifying the detection output fed back from the detection unit 4D, and the detection amplified by the V voltage adjustment amplifier 405 with the gain set by the resistor 406.
- the output voltage is input to the V voltage setting comparator including the m / z axis adjusting variable resistor 408 and the V voltage comparison amplifier 409, and the DC power supply unit 4B.
- the V voltage setting comparator comprising the m / z axis adjustment variable resistor 408 and the V voltage comparison amplifier 409 compares the detection output after gain adjustment with the power supply control voltage, and according to the comparison result.
- the multiplier 410 has a function of determining a multiplier (so-called gain).
- the V voltage is inversely proportional to the frequency f. For this reason, for example, the V voltage decreases as the frequency f increases.
- the V voltage changes when the frequency of the high frequency voltage is changed for tuning. For example, when the frequency f increases by 0.2% (1.2 MHz ⁇ 1.20024 MHz), the V voltage decreases by 0.2%. Then, the U / V that should be kept constant changes, and a phenomenon occurs in which the mass resolution becomes too high (sensitivity becomes low) in the high mass-to-charge ratio region.
- FIGS. 9A and 9B are actual measurement examples of peak profiles at a plurality of mass-to-charge ratios with respect to a standard sample.
- FIG. 9A shows a state in which the frequency f is optimally adjusted at 1.2 MHz
- FIG. I s a state in which the voltage is only increased to 1.20024 MHz (voltage adjustment is not performed). Comparing (a) and (b), it can be seen that in (b) the peak half-value width is narrow and the peak value is low in the region where the mass-to-charge ratio is high. This means that mass resolution is increased and detection sensitivity is decreased.
- FIG. 10A is an example of actual measurement when the V voltage is adjusted to return to the original state from the state of FIG. 9B, but there is a deviation in the m / z axis.
- FIG. 10B is an actual measurement example in the case where the U voltage is adjusted so that U / V is further constant from the state of FIG. 10A, but there is still a deviation in the m / z axis.
- the present invention has been made to solve these problems, and its main object is to provide a variable resistance even when the frequency is changed for tuning in a quadrupole power supply unit employing a variable frequency tuning system. It is an object of the present invention to provide a quadrupole mass spectrometer that can eliminate the need for mass peak shape adjustment or m / z axis adjustment by automatic adjustment or the like.
- a quadrupole mass filter including a plurality of electrodes and ions having a specific mass-to-charge ratio that selectively pass through the quadrupole mass filter.
- a quadrupole power source for applying a predetermined voltage to each electrode of the quadrupole mass filter, and a control means for instructing the quadrupole power source to a target voltage corresponding to a mass-to-charge ratio of ions to be measured.
- the quadrupole power source includes a detection means for direct-current detection of a high-frequency voltage applied to the quadrupole mass filter, a detection output adjustment means for adjusting a gain of a detection output by the detection means, and a variable frequency.
- the LC resonance circuit formed including a stray capacitance between the electrodes of the quadrupole mass filter increases the high frequency voltage superimposed by the superimposing means and applies it to the quadrupole mass filter.
- the detection output adjustment means in the quadrupole power supply includes amplification means for amplifying a voltage with a constant gain independent of the frequency of the high-frequency signal, and the frequency of the high-frequency signal is changed from a standard frequency for tuning.
- First correcting means for correcting the voltage according to the frequency change magnification at the input stage or output stage of the amplifying means so that the amplitude of the high-frequency voltage applied to the quadrupole mass filter is constant.
- the quadrupole power supply further includes second correction means for correcting the target voltage in accordance with a square of a magnification of the frequency change when the frequency for tuning changes. Yes.
- the frequency of the high-frequency signal generated by the high-frequency signal generating means for tuning the LC resonance circuit is set to, for example, the standard frequency (the stray capacitance of the quadrupole mass filter is previously
- the first correction unit reduces the gain by an amount corresponding to the degree of change in the frequency.
- the gain of the entire detection output adjusting means also decreases, so that feedback acts to increase the high frequency voltage output to compensate for the decrease, and the amplitude of the high frequency voltage applied to the quadrupole mass filter is the same as before the frequency change. Keep on level.
- the second correction unit corrects the target voltage by the square of the rate of change due to the frequency increase for tuning.
- the optimum state of ion selection according to the Matthew equation is maintained for an arbitrary mass-to-charge ratio, so that the occurrence of misalignment of the m / z axis can be avoided.
- a second invention made to solve the above-described problems is a quadrupole mass filter composed of a plurality of electrodes, and ions having a specific mass-to-charge ratio selectively pass through the quadrupole mass filter.
- the quadrupole power source includes a detection means for direct-current detection of a high-frequency voltage applied to the quadrupole mass filter, a detection output adjustment means for adjusting a gain of a detection output by the detection means, and a high-frequency signal that is variable in frequency.
- a high-frequency power supply that outputs a high-frequency voltage having an amplitude based on a comparison between the output of the detection output adjusting unit and the target voltage and having a frequency that is the same as or proportional to the frequency of the high-frequency signal
- a DC power supply that outputs a DC voltage based on the output of the detection output adjusting means, and a superimposing means that superimposes a DC voltage from the DC power supply and a high-frequency voltage from the high-frequency power supply, and the quadrupole
- the quadrupole mass fill is increased by increasing the high frequency voltage superimposed by the superimposing means by an LC resonance circuit formed including a stray capacitance between the electrodes of the mass filter.
- the quadrupole power supply is a) When the frequency of the high-frequency signal is changed from the standard frequency for tuning, the output given from the detection adjusting means to the DC power source is changed by the amount corresponding to the change in the output of the high-frequency power source, and the quadruple A first correction for correcting the output given from the detection adjusting means to the DC power source according to the frequency change magnification so that the ratio between the amplitude of the high-frequency voltage applied to the polar mass filter and the DC voltage is constant.
- the first correction The means corrects the voltage applied from the detection adjusting means to the DC power supply so that the output from the DC power supply is lowered by the amount that the high-frequency voltage output is reduced as the frequency increases.
- the relationship (ratio) between the amplitude of the high-frequency voltage applied to the quadrupole mass filter and the DC voltage is kept the same as before the frequency change, and the mass resolution is kept in a good state.
- the second correction means corrects the target voltage by the cube of the rate of change due to the frequency increase for tuning.
- the optimum state of ion selection according to the Matthew equation is maintained for an arbitrary mass-to-charge ratio, so that the occurrence of misalignment of the m / z axis can be avoided.
- a target voltage to be a target of the high frequency voltage is given from the control means to the quadrupole power source, and the DC power source generates a DC voltage based on the detection output fed back.
- the control means generates a target voltage such that the relationship between the high voltage and the direct current voltage becomes constant separately, and supplies the target voltage to the high frequency power supply and the direct current power supply.
- a quadrupole mass filter including a plurality of electrodes, and ions having a specific mass-to-charge ratio selectively pass through the quadrupole mass filter.
- a quadrupole power source that applies a predetermined voltage, which is a superposition of a high-frequency voltage and a DC voltage, to each electrode of the quadrupole mass filter, and the amplitude of the high-frequency voltage and the voltage value of the DC voltage are measured while maintaining a certain relationship.
- control means for instructing The quadrupole power source includes a detection means for direct-current detection of a high-frequency voltage applied to the quadrupole mass filter, a detection output adjustment means for adjusting a gain of a detection output by the detection means, and a high-frequency signal that is variable in frequency.
- a high-frequency voltage having an amplitude based on a comparison between the output of the detection output adjusting unit and the first target voltage and having a frequency that is the same as or proportional to the frequency of the high-frequency signal.
- a quadrupole comprising: a high frequency power supply; a direct current power supply that outputs a direct current voltage corresponding to the second target voltage; and a superimposing unit that superimposes the direct current voltage from the direct current power supply and the high frequency voltage from the high frequency power supply.
- the high frequency voltage superimposed by the superimposing means is increased and applied to the quadrupole mass filter by the LC resonance circuit formed including the stray capacitance between the electrodes of the mass filter.
- the quadrupole power supply is a) first correction means for correcting the first target voltage according to the cube of the frequency change when the frequency of the high-frequency signal is changed from a standard frequency for tuning; b) second correction means for correcting the second target voltage according to the square of the magnification of the frequency change when the frequency changes for tuning; It is characterized by having.
- the first and second correction means in the quadrupole mass spectrometer according to the third invention are substantially the first and second corrections in the quadrupole mass spectrometer according to the first or second invention. It has the same effect as that of the means, and maintains the relationship (ratio) between the amplitude of the high-frequency voltage and the DC voltage as before the frequency change, and maintains the mass resolution. Further, by maintaining the optimum state of ion selection according to the Matthew equation for an arbitrary mass-to-charge ratio, the occurrence of m / z axis misalignment is avoided.
- the frequency of the high-frequency voltage is changed in order to tune the LC resonance circuit in the quadrupole power supply unit employing the variable frequency tuning method. Even in this case, correction is automatically performed in accordance with the amount of change in the frequency so that the mass resolution is maintained and no m / z axis deviation occurs. This eliminates the need for manual adjustment of variable resistance, mass peak shape adjustment by automatic tuning, and m / z axis adjustment even when frequency adjustment for tuning is performed, thus reducing the burden on the operator and analyzing work. Efficiency can be improved.
- the circuit block diagram of the quadrupole power supply part in the quadrupole-type mass spectrometer which is 1st Example of this invention.
- the circuit block diagram of the quadrupole power supply part in the quadrupole-type mass spectrometer which is 2nd Example of this invention.
- the circuit block diagram of the quadrupole power supply part in the quadrupole-type mass spectrometer which is 3rd Example of this invention.
- the circuit block diagram of the quadrupole power supply part in the quadrupole-type mass spectrometer which is 4th Example of this invention.
- the circuit block diagram of the quadrupole power supply part in the quadrupole-type mass spectrometer which is 5th Example of this invention.
- FIG. 1 is a schematic configuration diagram of a general quadrupole mass spectrometer.
- the schematic block diagram of the conventional quadrupole power supply part The circuit block diagram of the conventional quadrupole power supply part.
- the figure which shows the actual measurement example of the peak profile in the some mass to charge ratio with respect to a standard sample The figure which shows the actual measurement example of the peak profile in the some mass to charge ratio with respect to a standard sample.
- FIG. 1 is a circuit configuration diagram of a quadrupole power supply unit 4 in the quadrupole mass spectrometer of the present embodiment.
- the same components as those already described in FIG. 8 are denoted by the same reference numerals and detailed description thereof is omitted.
- the m / z axis correction coefficient Mcomp1 and the V voltage correction coefficient Vcomp1 are input from the control unit 5 to the quadrupole power supply unit 4 in the first embodiment. It has V voltage correction function and m / z axis correction function.
- the V voltage correction function added to the detection gain adjustment unit 4C is realized by the multiplier 421 multiplying the output Vdet ′ of the V voltage adjustment amplifier 405 by the V voltage correction coefficient Vcomp1.
- the V voltage monitor voltage Vmon is always constant due to the feedback function regardless of the change of the set frequency f.
- the V voltage is compensated for. It becomes a feedback operation that raises.
- the V voltage decreases as the set frequency f increases in the absence of the V voltage correction.
- the V voltage correction function the V voltage increases so as to compensate for the decrease. Keep the same as before the change.
- the m / z axis correction function added to the high frequency power supply unit 4A is realized by the multiplier 420 multiplying the power control voltage Qcont by the m / z axis correction coefficient Mcomp1.
- Mcomp1 (set frequency f / standard frequency f 0 ) 2 , that is, the square of the frequency change magnification. .
- the optimum voltage for an arbitrary mass-to-charge ratio needs to change the square of the frequency change. Since a square change of the frequency change occurs, an optimum V voltage is obtained for an arbitrary mass-to-charge ratio, and the m / z axis can be prevented from shifting even when the set frequency f changes.
- V voltage (at 1.20024 MHz) V voltage (at 1.2 MHz)
- the V voltage is an optimum voltage for an arbitrary mass-to-charge ratio, that is, a voltage that does not cause an m / z axis shift.
- the control unit 5 changes the set frequency f of the high-frequency voltage signal generator 411 from the standard frequency f 0 in order to tune the LC resonance circuit.
- V voltage correction coefficient Vcomp1 (standard frequency f 0 / set frequency f)
- the quadrupole power supply unit 4 corrects the detection output voltage and the power supply control voltage as described above. As a result, the mass resolution remains high even after the set frequency f is changed, and the m / z axis does not shift.
- the multipliers 420 and 421 are analog multipliers, but it is natural that the multiplication may be performed digitally in a CPU or the like. The same applies to the other embodiments described below.
- FIG. 2 is a circuit configuration diagram of the quadrupole power supply unit 4 in the quadrupole mass spectrometer of the second embodiment.
- the same components as those already described in FIGS. 1 and 8 are denoted by the same reference numerals, and detailed description thereof is omitted.
- the quadrupole mass spectrometer of the second embodiment is obtained by adding a U voltage correction function to the DC power supply unit 4B in place of the V voltage correction function provided in the apparatus of the first embodiment.
- the U voltage correction function added to the DC power supply unit 4B changes the U voltage so that the ratio between the V voltage and the U voltage is kept constant for the V voltage change caused by the change in the set frequency f.
- U voltage (at 1.2MHz) U voltage (at 1.20024MHz)
- the m / z axis correction function provided in the high frequency power supply unit 4A is realized by the multiplier 430 multiplying the power control voltage Qcont by the m / z axis correction coefficient Mcomp2.
- the V voltage is an optimum voltage for an arbitrary mass-to-charge ratio, that is, a voltage that does not cause an m / z axis shift.
- the controller 5 changes the set frequency f of the high-frequency voltage signal generator 411 from the standard frequency f 0 in order to tune the LC resonance circuit.
- the quadrupole power supply unit 4 corrects the U voltage control voltage and the power supply control voltage input to the DC power supply unit 4B as described above. Thereby, even after the set frequency f is changed, the mass resolution remains high, and the m / z axis is not displaced.
- FIG. 3 is a circuit configuration diagram of the quadrupole power supply unit 4 in the quadrupole mass spectrometer of the third embodiment.
- the same components as those already described in FIGS. 1, 2 and 8 are designated by the same reference numerals, and detailed description thereof is omitted.
- the V voltage monitor voltage Vmon output from the detection gain adjusting section 4C is used as the U voltage control voltage that is the input of the DC power supply section 4B.
- a U voltage control voltage dedicated to the DC power supply unit 4B is applied from the control unit 5 to the quadrupole power supply unit 4, and the quadrupole power supply unit 4 generates a DC voltage using this.
- V voltage correction and m / z axis correction are applied to the V voltage control voltage Vcont supplied from the control unit 5 in the high frequency power supply unit 4A, and supplied from the control unit 5 in the DC power supply unit 4B.
- M / z axis correction is applied to the U voltage control voltage Ucont.
- the V voltage correction function is realized by the multiplier 440 multiplying the V voltage control voltage Vcont by a V voltage correction coefficient Vcomp2 corresponding to the set frequency f.
- the multiplier 440 multiplies the V voltage control voltage Vcont by the m / z axis correction coefficient Mcomp3 corresponding to the set frequency f, and in the DC power supply unit 4B the multiplier 441. Is realized by multiplying the U voltage control voltage Ucont by the m / z axis correction coefficient Mcomp3.
- the multiplier 440 Since the multiplier 440 multiplies both the V voltage correction coefficient Vcomp2 and the m / z axis correction coefficient Mcomp3 by the V voltage control voltage Vcont, the multiplier 440 actually sets the V voltage control voltage Vcont to (the set frequency f / Standard frequency f 0 ) 3 is multiplied. Thereby, similarly to the first and second embodiments, high mass resolution can be maintained even after the set frequency f is changed, and the accuracy of the m / z axis can be maintained.
- FIG. 4 is a circuit configuration diagram of the quadrupole power supply unit 4 in the quadrupole mass spectrometer of the fourth embodiment.
- the same components as those already described in FIGS. 1 to 3 and 8 are designated by the same reference numerals, and detailed description thereof is omitted.
- U voltage correction and m / z axis correction are performed on the U voltage control voltage Ucont supplied from the control unit 5 in the DC power supply unit 4B, and V applied from the control unit 5 in the high frequency power supply unit 4A.
- M / z axis correction is applied to the voltage control voltage Vcont.
- the U voltage correction function is realized by the multiplier 451 multiplying the U voltage control voltage Ucont by a U voltage correction coefficient Ucomp2 corresponding to the set frequency f.
- the multiplier 450 in the high frequency power supply unit 4A multiplies the V voltage control voltage Vcont by the m / z axis correction coefficient Mcomp4 corresponding to the set frequency f and the multiplier 451 in the DC power supply unit 4B. Is realized by multiplying the U voltage control voltage Ucont by the m / z axis correction coefficient Mcomp4.
- the multiplier 451 Since the multiplier 451 multiplies both the U voltage correction coefficient Ucomp2 and the m / z axis correction coefficient Mcomp4 by the U voltage control voltage Ucont, the multiplier 451 actually uses the U voltage control voltage Ucont (set frequency f). / Standard frequency f 0 ) 2 is multiplied. Thereby, similarly to the first and second embodiments, high mass resolution can be maintained even after the set frequency f is changed, and the accuracy of the m / z axis can be maintained.
- FIG. 5 is a circuit configuration diagram of the quadrupole power supply unit 4 in the quadrupole mass spectrometer of the fifth embodiment.
- the same components as those already described in FIGS. 1 to 4 and 8 are designated by the same reference numerals, and detailed description thereof is omitted.
- the U voltage control voltage Ucont supplied from the control unit 5 in the DC power supply unit 4B is subjected to U voltage correction and m / z axis correction, and the V voltage supplied from the control unit 5 in the high frequency power supply unit 4A.
- V voltage correction and m / z axis correction are applied to the voltage control voltage Vcont.
- the multiplier 461 sets the U voltage / m / z axis correction coefficient U / Mcomp corresponding to the set frequency f to the U voltage control voltage Ucont. Multiply.
- the multiplier 460 multiplies the V voltage control voltage Vcont by a V voltage / m / z axis correction coefficient V / Mcomp corresponding to the set frequency f.
- tuning is performed by the LC resonance circuit including each rod electrode of the quadrupole mass filter 2 to generate a high-frequency voltage having a large amplitude. Even when the frequency is changed to be applied to the power supply, the correction of the voltage according to the change in the frequency is automatically performed by the quadrupole power supply unit 4, so that the mass resolution is adjusted by manual adjustment of the variable resistors 406 and 408 or the like. And m / z misalignment adjustment is not required.
- High frequency voltage signal generator 412 ... Buffer amplifier 413 ... Drive circuit 414 ... High frequency transformer 415 ... Inverting amplifier 416 ... Positive DC voltage amplifier 417 ... Negative DC voltage Amplifiers 420, 421, 430, 431, 440, 441, 450, 451, 460, 461 ... multiplier 5 ... control unit 6 ... Over data processing unit 10 ... coil 11 ... capacitor
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Abstract
Description
[V電圧モニタ電圧Vmon]∝[V電圧検波電圧Vdet]
=[検波用コンデンサ402、403に流れる電流i]×[V電圧検波用抵抗404の抵抗値R]
∝[V電圧]×2πf×[検波用コンデンサ402、403のキャパシタンスC]×[V電圧検波用抵抗404の抵抗値R]
∝[V電圧]・f
となる。
au=ax=-ay=4eU/(mω2r0 2) …(1)
qu=qx=-qy=2eU/(mω2r0 2)
例えば上述のように周波数fが0.2%上昇した場合、V電圧とU電圧の最適値は、周波数f=1.20024MHzにおけるV電圧(又はU電圧)×(1.20024/1.2)2となる。したがって、周波数fを高くしたときに、それに伴って下がった分だけ電圧を上げてV電圧を元のV電圧に戻すように調整しただけでは、m/z軸のずれが生じることになる。図10(a)は図9(b)の状態からV電圧を元に戻すように調整した場合の実測例であるが、m/z軸にずれが発生している。
前記四重極電源にあって前記検波出力調整手段は、前記高周波信号の周波数に依らない一定のゲインで電圧を増幅する増幅手段と、同調のために前記高周波信号の周波数が標準周波数から変化されたときに前記四重極マスフィルタに印加される高周波電圧の振幅が一定になるように、前記増幅手段の入力段又は出力段で周波数変化の倍率に応じて電圧を補正する第1の補正手段と、を含み、さらに前記四重極電源は、同調のための前記周波数の変化時に、その周波数変化の倍率の二乗に応じて前記目標電圧を補正する第2の補正手段を備えることを特徴としている。
前記四重極電源は、前記四重極マスフィルタに印加される高周波電圧を直流検波する検波手段と、該検波手段による検波出力のゲインを調整する検波出力調整手段と、周波数可変である高周波信号を生成する信号生成手段を含み、前記検波出力調整手段の出力と前記目標電圧との比較に基づく振幅を有し前記高周波信号の周波数と同一又はそれに比例する周波数を有する高周波電圧を出力する高周波電源と、前記検波出力調整手段の出力に基づいて直流電圧を出力する直流電源と、該直流電源による直流電圧と前記高周波電源による高周波電圧とを重畳する重畳手段と、を有し、前記四重極マスフィルタの電極間の浮遊容量を含んで形成されるLC共振回路により前記重畳手段により重畳された高周波電圧を増大させて前記四重極マスフィルタに印加するとともに、前記高周波信号の周波数を調整することで前記LC共振回路を同調させる四重極型質量分析装置において、
前記四重極電源は、
a)同調のために前記高周波信号の周波数が標準周波数から変化されたときに、前記高周波電源の出力が変化した分だけ前記検波調整手段から前記直流電源に与えられる出力を変化させて前記四重極マスフィルタに印加される高周波電圧の振幅と直流電圧との比が一定になるように、前記検波調整手段から前記直流電源に与えられる出力を周波数変化の倍率に応じて補正する第1の補正手段と、
b)同調のための前記周波数の変化時に、その周波数変化の倍率の三乗に応じて前記目標電圧を補正する第2の補正手段と、
を備えることを特徴としている。
前記四重極電源は、前記四重極マスフィルタに印加される高周波電圧を直流検波する検波手段と、該検波手段による検波出力のゲインを調整する検波出力調整手段と、周波数可変である高周波信号を生成する信号生成手段を含み、前記検波出力調整手段の出力と前記第1目標電圧との比較に基づく振幅を有し前記高周波信号の周波数と同一又はそれに比例する周波数を有する高周波電圧を出力する高周波電源と、前記第2目標電圧に応じた直流電圧を出力する直流電源と、該直流電源による直流電圧と前記高周波電源による高周波電圧とを重畳する重畳手段と、を有し、前記四重極マスフィルタの電極間の浮遊容量を含んで形成されるLC共振回路により前記重畳手段により重畳された高周波電圧を増大させて前記四重極マスフィルタに印加するとともに、前記高周波信号の周波数を調整することで前記LC共振回路を同調させる四重極型質量分析装置において、
前記四重極電源は、
a)同調のために前記高周波信号の周波数が標準周波数から変化されたときに、周波数変化の三乗に応じて前記第1目標電圧を補正する第1の補正手段と、
b)同調のための前記周波数の変化時にその周波数変化の倍率の二乗に応じて前記第2目標電圧を補正する第2の補正手段と、
を備えることを特徴としている。
本発明の一実施例(以下「第1実施例」という)である四重極型質量分析装置について、添付図面を参照して詳細に説明する。
第1実施例の四重極型質量分析装置の全体構成は図6で説明した従来の装置と同じであるので説明を省略する。本実施例の四重極型質量分析装置の特徴は四重極電源部4の回路構成にある。図1は本実施例の四重極型質量分析装置における四重極電源部4の回路構成図である。図中、既に説明した図8中の構成要素と同一のものについては同一符号を付して詳しい説明を省略する。
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)
である。これに対し乗算器421によりV電圧補正を行うと、
Vcomp1・Vdet’=Vmon(一定値)
であるので、
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)/Vcomp1=V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)/(1.2MHz/1.20024MHz)=V電圧(at 1.2MHz)
となる。即ち、高周波電圧の周波数が1.2MHz→1.20024MHzに変化した場合でもV電圧は一定に保たれる。
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)
であり、周波数f=1.20024MHzのときの任意の質量電荷比における最適なV電圧は、
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)×(1.20024MHz/1.2MHz)2
である。したがって、出力電圧は最適電圧とは異なり、これによりm/z軸はずれることになる。これに対し乗算器420による上述したm/z軸補正を行うと、
V電圧(at 1.20024MHz)=Qcont×Mcomp1=V電圧(at 1.2MHz)×(1.20024MHz/1.2MHz)2
となり、高周波電圧の周波数が1.2MHz→1.20024MHzに変化した場合でもV電圧は任意の質量電荷比に対して最適な電圧、つまりm/z軸ずれの生じない電圧となる。
次に、本発明の別の実施例(以下「第2実施例」という)である四重極型質量分析装置について、添付図面を参照して詳細に説明する。
図2は第2実施例の四重極型質量分析装置における四重極電源部4の回路構成図である。図中、既に説明した図1、図8中の構成要素と同一のものについては同一符号を付して詳しい説明を省略する。
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)
であり、
Ucont=Vmon=一定値
であるから、
U電圧(at 1.2MHz)=U電圧(at 1.20024MHz)
となり、V電圧とU電圧との比は、
V電圧/U電圧(at 1.20024MHz)=[V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)]/U電圧(at 1.2MHz)=[V電圧/U電圧(at 1.2MHz)]×(1.2MHz/1.20024MHz)]
となる。即ち、V電圧とU電圧との比は周波数変化に伴って変化してしまう。
これに対し乗算器422による上述したU電圧補正を行うと、
U電圧(at 1.20024MHz)=U電圧(at 1.2MHz)/Ucomp1=U電圧(at 1.2MHz)/(1.2MHz/1.20024MHz)
となり、V電圧とU電圧との比は、
V電圧/U電圧(at 1.20024MHz)=[V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)]/[U電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)]=V電圧/U電圧(at 1.2MHz)
となる。即ち、1.2MHz→1.20024MHzに周波数が変化しても、V電圧とU電圧との比は一定となる。
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)
であり、周波数f=1.20024MHzのときの任意の質量電荷比における最適なV電圧は、
V電圧(at 1.20024MHz)=V電圧(at 1.2MHz)×(1.20024MHz/1.2MHz)2
である。したがって、出力電圧は最適電圧とは異なり、これによりm/z軸はずれることになる。これに対し乗算器430によりm/z軸補正を行うと、
V電圧(at 1.20024MHz)=Qcont×Mcomp2=V電圧(at 1.2MHz)×(1.2MHz/1.20024MHz)×(1.20024MHz/1.2MHz)3=V電圧(at 1.2MHz)×(1.20024MHz/1.2MHz)2
となり、高周波電圧の周波数が1.2MHz→1.20024MHzに変化した場合でもV電圧は任意の質量電荷比に対して最適な電圧、つまりm/z軸ずれの生じない電圧となる。
次に、本発明の別の実施例(以下「第3実施例」という)である四重極型質量分析装置について、添付図面を参照して詳細に説明する。
図3は第3実施例の四重極型質量分析装置における四重極電源部4の回路構成図である。図中、既に説明した図1、図2、図8中の構成要素と同一のものについては同一符号を付して詳しい説明を省略する。
次に、本発明の別の実施例(以下「第4実施例」という)である四重極型質量分析装置について、添付図面を参照して詳細に説明する。
図4は第4実施例の四重極型質量分析装置における四重極電源部4の回路構成図である。図中、既に説明した図1~図3、図8中の構成要素と同一のものについては同一符号を付して詳しい説明を省略する。
さらに本発明の別の実施例(以下「第5実施例」という)である四重極型質量分析装置について、添付図面を参照して詳細に説明する。
図5は第5実施例の四重極型質量分析装置における四重極電源部4の回路構成図である。図中、既に説明した図1~図4、図8中の構成要素と同一のものについては同一符号を付して詳しい説明を省略する。
これにより、第1及び第2実施例と同様に、設定周波数f変更後も高い質量分解能を維持し、m/z軸の精度も保つことができる。
2…四重極マスフィルタ
2a、2b、2c、2d…ロッド電極
3…検出器
4…四重極電源部
4A…高周波電源部
4B…直流電源部
4C…検波ゲイン調整部
4D…検波部
401…ダイオードブリッジ整流回路
402、403…検波用コンデンサ
404…V電圧検波用抵抗
405…V電圧調整用アンプ
406…V電圧調整用可変抵抗
407…バッファアンプ
408…m/z軸調整用可変抵抗
409…V電圧比較用アンプ
410…乗算器
411…高周波電圧用信号発生器
412…バッファアンプ
413…ドライブ回路
414…高周波トランス
415…反転アンプ
416…正極性直流電圧用アンプ
417…負極性直流電圧用アンプ
420、421、430、431、440、441、450、451、460、461…乗算器
5…制御部
6…データ処理部
10…コイル
11…コンデンサ
Claims (3)
- 複数の電極からなる四重極マスフィルタと、特定の質量電荷比を有するイオンが前記四重極マスフィルタを選択的に通過するように所定の電圧を該四重極マスフィルタの各電極に印加する四重極電源と、測定対象であるイオンの質量電荷比に応じた目標電圧を前記四重極電源に指示する制御手段と、を具備し、
前記四重極電源は、前記四重極マスフィルタに印加される高周波電圧を直流検波する検波手段と、該検波手段による検波出力のゲインを調整する検波出力調整手段と、周波数可変である高周波信号を生成する信号生成手段を含み、前記検波出力調整手段の出力と前記目標電圧との比較に基づく振幅を有し前記高周波信号の周波数と同一又はそれに比例する周波数を有する高周波電圧を出力する高周波電源と、前記検波出力調整手段の出力に基づいて直流電圧を出力する直流電源と、該直流電源による直流電圧と前記高周波電源による高周波電圧とを重畳する重畳手段と、を有し、前記四重極マスフィルタの電極間の浮遊容量を含んで形成されるLC共振回路により前記重畳手段により重畳された高周波電圧を増大させて前記四重極マスフィルタに印加するとともに、前記高周波信号の周波数を調整することで前記LC共振回路を同調させる四重極型質量分析装置において、
前記四重極電源にあって前記検波出力調整手段は、前記高周波信号の周波数に依らない一定のゲインで電圧を増幅する増幅手段と、同調のために前記高周波信号の周波数が標準周波数から変化されたときに、前記四重極マスフィルタに印加される高周波電圧の振幅が一定になるように、前記増幅手段の入力段又は出力段で周波数変化の倍率に応じて電圧を補正する第1の補正手段と、を含み、さらに前記四重極電源は、同調のための前記周波数の変化時に、その周波数変化の倍率の二乗に応じて前記目標電圧を補正する第2の補正手段を備えることを特徴とする四重極型質量分析装置。 - 複数の電極からなる四重極マスフィルタと、特定の質量電荷比を有するイオンが前記四重極マスフィルタを選択的に通過するように所定の電圧を該四重極マスフィルタの各電極に印加する四重極電源と、測定対象であるイオンの質量電荷比に応じた目標電圧を前記四重極電源に指示する制御手段と、を具備し、
前記四重極電源は、前記四重極マスフィルタに印加される高周波電圧を直流検波する検波手段と、該検波手段による検波出力のゲインを調整する検波出力調整手段と、周波数可変である高周波信号を生成する信号生成手段を含み、前記検波出力調整手段の出力と前記目標電圧との比較に基づく振幅を有し前記高周波信号の周波数と同一又はそれに比例する周波数を有する高周波電圧を出力する高周波電源と、前記検波出力調整手段の出力に基づいて直流電圧を出力する直流電源と、該直流電源による直流電圧と前記高周波電源による高周波電圧とを重畳する重畳手段と、を有し、前記四重極マスフィルタの電極間の浮遊容量を含んで形成されるLC共振回路により前記重畳手段により重畳された高周波電圧を増大させて前記四重極マスフィルタに印加するとともに、前記高周波信号の周波数を調整することで前記LC共振回路を同調させる四重極型質量分析装置において、
前記四重極電源は、
a)同調のために前記高周波信号の周波数が標準周波数から変化されたときに、前記高周波電源の出力が変化した分だけ前記検波調整手段から前記直流電源に与えられる出力を変化させて前記四重極マスフィルタに印加される高周波電圧の振幅と直流電圧との比が一定になるように、前記検波調整手段から前記直流電源に与えられる出力を周波数変化の倍率に応じて補正する第1の補正手段と、
b)同調のための前記周波数の変化時に、その周波数変化の倍率の三乗に応じて前記目標電圧を補正する第2の補正手段と、
を備えることを特徴とする四重極型質量分析装置。 - 複数の電極からなる四重極マスフィルタと、特定の質量電荷比を有するイオンが前記四重極マスフィルタを選択的に通過するように高周波電圧と直流電圧とを重畳した所定の電圧を該四重極マスフィルタの各電極に印加する四重極電源と、高周波電圧の振幅と直流電圧の電圧値とが一定の関係を保ちつつ測定対象であるイオンの質量電荷比に応じた電圧が前記四重極マスフィルタに印加されるように、前記四重極電源に対し高周波電圧の振幅に関する第1目標電圧と直流電圧に関する第2目標電圧とを指示する制御手段と、を具備し、
前記四重極電源は、前記四重極マスフィルタに印加される高周波電圧を直流検波する検波手段と、該検波手段による検波出力のゲインを調整する検波出力調整手段と、周波数可変である高周波信号を生成する信号生成手段を含み、前記検波出力調整手段の出力と前記第1目標電圧との比較に基づく振幅を有し前記高周波信号の周波数と同一又はそれに比例する周波数を有する高周波電圧を出力する高周波電源と、前記第2目標電圧に応じた直流電圧を出力する直流電源と、該直流電源による直流電圧と前記高周波電源による高周波電圧とを重畳する重畳手段と、を有し、前記四重極マスフィルタの電極間の浮遊容量を含んで形成されるLC共振回路により前記重畳手段により重畳された高周波電圧を増大させて前記四重極マスフィルタに印加するとともに、前記高周波信号の周波数を調整することで前記LC共振回路を同調させる四重極型質量分析装置において、
前記四重極電源は、
a)同調のために前記高周波信号の周波数が標準周波数から変化されたときに、周波数変化の三乗に応じて前記第1目標電圧を補正する第1の補正手段と、
b)同調のための前記周波数の変化時にその周波数変化の倍率の二乗に応じて前記第2目標電圧を補正する第2の補正手段と、
を備えることを特徴とする四重極型質量分析装置。
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US7078686B2 (en) * | 2004-07-23 | 2006-07-18 | Agilent Technologies, Inc. | Apparatus and method for electronically driving a quadrupole mass spectrometer to improve signal performance at fast scan rates |
GB0524042D0 (en) * | 2005-11-25 | 2006-01-04 | Micromass Ltd | Mass spectrometer |
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- 2011-02-10 WO PCT/JP2011/052930 patent/WO2012108050A1/ja active Application Filing
- 2011-02-10 CN CN201180067394.7A patent/CN103370766B/zh active Active
- 2011-02-10 US US13/983,498 patent/US8907274B2/en active Active
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JP2002033075A (ja) * | 2000-07-18 | 2002-01-31 | Shimadzu Corp | 質量分析装置 |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2014076244A2 (en) * | 2012-11-16 | 2014-05-22 | Thermo Fisher Scientific (Bremen) Gmbh | Rf transformer |
WO2014076244A3 (en) * | 2012-11-16 | 2015-01-22 | Thermo Fisher Scientific (Bremen) Gmbh | Rf transformer |
US8957391B2 (en) | 2012-11-16 | 2015-02-17 | Thermo Fisher Scientific (Bremen) Gmbh | RF transformer |
WO2015177886A1 (ja) * | 2014-05-21 | 2015-11-26 | 株式会社島津製作所 | 高周波電圧生成装置 |
JPWO2015177886A1 (ja) * | 2014-05-21 | 2017-04-20 | 株式会社島津製作所 | 高周波電圧生成装置 |
WO2023067658A1 (ja) * | 2021-10-18 | 2023-04-27 | 株式会社島津製作所 | 質量分析装置および検波ユニット |
Also Published As
Publication number | Publication date |
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US20130313427A1 (en) | 2013-11-28 |
US8907274B2 (en) | 2014-12-09 |
CN103370766A (zh) | 2013-10-23 |
EP2674963B1 (en) | 2016-11-16 |
EP2674963A1 (en) | 2013-12-18 |
JPWO2012108050A1 (ja) | 2014-07-03 |
JP5527439B2 (ja) | 2014-06-18 |
EP2674963A4 (en) | 2015-11-25 |
CN103370766B (zh) | 2015-11-25 |
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