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JEOL : Patent Issued for Time-Of-Flight Mass Spectrometer and Method of Controlling Same (USPTO 9536727)

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01/12/2017 | 10:18pm CET

By a News Reporter-Staff News Editor at Journal of Engineering -- JEOL Ltd. (Tokyo, JP) has been issued patent number 9536727, according to news reporting originating out of Alexandria, Virginia, by VerticalNews editors.

The patent's inventor is Satoh, Takaya (Tokyo, JP).

This patent was filed on September 12, 2013 and was published online on January 3, 2017.

From the background information supplied by the inventors, news correspondents obtained the following quote: "Field of the Invention

"The present invention relates to a time-of-flight mass spectrometer used in quantitative analysis and simultaneous qualitative analysis of trace compounds and also in structural analysis of sample ions. The invention also relates to a method of controlling this spectrometer.

"Description of the Related Art

"A mass spectrometer (MS) ionizes a sample in an ion source, separates the resulting ions in a mass analyzer at each value of m/z obtained by dividing the mass (m) by the charge number (z), and detects the separated ions by a detector. The results are represented in the form of a mass spectrum. On the horizontal axis of the spectrum, m/z values are plotted, while on the vertical axis, relative intensities are plotted. In this way, m/z values and relative intensities of compounds contained in the sample are obtained. Consequently, qualitative and quantitative information about the sample can be derived. Various methods are available as ionization method, mass separation method, and ion detection method for mass spectrometers.

"A time-of-flight (TOF) mass spectrometer is an instrument that finds the mass-to-charge ratio (m/z) of each ion by accelerating ions with a given accelerating voltage, causing them to fly, and calculating the m/z from the time taken for each ion to reach a detector. In the TOF mass spectrometer, ions are accelerated by a constant pulsed voltage V.sub.a. At this time, from the law of conservation of energy, the following Eq. (1) holds.

"##EQU00001## where v is the velocity of the ion, m is the mass of the ion, z is the valence number of the ion, and e is the elementary charge.

"From Eq. (1), the velocity v of the ion is given by

".times..times. ##EQU00002##

"Therefore, the flight time T required for the ion to reach a detector, placed behind at a given distance of L, is given by

".times..times..times. ##EQU00003##

"As can be seen from Eq. (3), the flight time T differs according to m/z of each ion. TOFMS is an instrument for separating ions employing this principle.

"A linear TOF mass spectrometer in which ions are made to fly linearly from an ion source to a detector and a reflectron TOF mass spectrometer in which a reflectron field is placed between an ion source and a detector to improve energy focusing and to prolong the flight distance have enjoyed wide acceptance. It is known that reflectron TOF mass spectrometers are used to estimate the compositions of unknown substances, because they can measure the m/z values of unknown substances with errors on the order of ppm with respect to m/z values computationally found from composition formulas.

"The mass resolution R of a TOF mass spectrometer is defined as follows:

".times..times..DELTA..times..times. ##EQU00004## where T is the total flight time and .DELTA.T is a peak width.

"That is, if the peak width .DELTA.T is made constant and the total flight time T can be lengthened, the mass resolution can be improved. However, in the related art linear or reflectron type TOFMS, increasing the total flight time T (i.e., increasing the total flight distance) will lead directly to an increase in instrumental size. A multi-pass time-of-flight mass spectrometer has been developed to realize high mass resolution while avoiding an increase in instrumental size (non-patent document 1). This instrument uses four toroidal electric fields each consisting of a combination of a cylindrical electric field and a Matsuda plate. The total flight time T can be lengthened by accomplishing multiple turns in an 8-shaped circulating orbit. In this apparatus, the spatial and temporal spread at the detection surface has been successfully converged up to the first-order term using the initial position, initial angle, and initial kinetic energy.

"However, the TOFMS in which ions revolve many times in a closed trajectory suffers from the problem of 'overtaking'. That is, because ions revolve multiple times in a closed trajectory, lighter ions moving at higher speeds overtake heavier ions moving at smaller speeds. Consequently, the fundamental concept of TOFMS that ions arrive at the detection surface in turn first from the lightest one does not hold.

"The spiral-trajectory TOFMS has been devised to solve this problem. The spiral-trajectory TOFMS is characterized in that the starting and ending points of a closed trajectory are shifted from the closed trajectory plane in the vertical direction. To achieve this, in one method, ions are made to impinge obliquely from the beginning (patent document 1). In another method, the starting and ending points of the closed trajectory are shifted in the vertical direction using a deflector (patent document 2). In a further method, laminated toroidal electric fields are used (patent document 3).

"Another TOFMS has been devised which is based on a similar concept but in which the trajectory of the multi-pass TOF-MS (patent document 4) where overtaking occurs is zigzagged (patent document 5).

"As described previously, in a mass spectrometer, ions generated in an ion source are separated according to m/z value in a mass analyzer and detected. The results are expressed in the form of a mass spectrum in which the m/z values of ions and their relative intensities are graphed. This measurement may hereinafter be referred to as an MS measurement in contrast with an MS/MS measurement. In the MS/MS measurement, certain ions generated in an ion source are selected by a first stage of mass analyzer (hereinafter referred to as MS1). The selected ions are referred to precursor ions. These ions spontaneously fragment or are caused to fragment, and the generated, fragmented ions (referred to as product ions) are mass analyzed by a subsequent stage of mass analyzer (referred to as MS2). An instrument enabling this is referred to as an MS/MS instrument. In MS/MS measurements, the m/z values of precursor ions, the m/z values of product ions generated in plural fragmentation paths, and information about relative intensities are obtained and so structural information about the precursor ions can be obtained. Various types of MS/MS instrument exist which can perform MS/MS measurements and in which two of the aforementioned mass spectrometers are combined. Furthermore, various fragmentation methods exist such as collision induced dissociation (CID) using collision with gas, photodissociation, and electron capture dissociation.

"Dissociation information about an MS/MS instrument utilizing CID differs according to collisional energy, i.e., the magnitude of kinetic energy of ions impinging on a collisional cell. In the case of currently available MS/MS instruments, CIDs are classified into two types: CIDs of low energies on the order of tens of eV and CIDs of high energies from several kV to tens of keV. The difference depends on the configuration of the instrument. High-energy CID has the advantage that, when a peptide having tens of amino acids chained together is fragmented, side chain information may be obtained. It is possible to distinguish between leucine and isoleucine having the same molecular weight."

Supplementing the background information on this patent, VerticalNews reporters also obtained the inventor's summary information for this patent: "In view of the problems described so far, the present invention has been made. According to some embodiments of the present invention, a TOF mass spectrometer can be offered in which the variable range of collisional energies can be made wider than conventional. Also, a method of controlling this TOF mass spectrometer can be offered. Furthermore, according to some embodiments of the invention, a TOF mass spectrometer capable of efficiently observing fragmentations of multivalent ions and a method of controlling this mass spectrometer can be offered.

"(1) A time-of-flight (TOF) mass spectrometer associated with the present invention has: an ion source for ionizing a sample to thereby produce ions; a first mass analyzer for separating the produced ions according to flight time corresponding to mass-to-charge ratio; an ion gate for selecting precursor ions from ions separated and selected by the first mass analyzer; a conductive box through which the precursor ions selected by the ion gate pass; a collisional cell for fragmenting the precursor ions passed through the conductive box into product ions; a second mass analyzer for separating the precursor ions passed through the collisional cell and the product ions generated by the collisional cell according to flight time corresponding to mass-to-charge ratio; a detector for detecting ions separated by the second mass analyzer; and a potential control portion for controlling the electric potential on the conductive box. When precursor ions enter the conductive box, the potential control portion sets the potential on the conductive box at a first potential. When the potential on the conductive box is varied, the potential control portion varies the potential on the conductive box from the first potential to a second potential while the precursor ions are passing through the conductive box.

"According to this TOF mass spectrometer associated with the present invention, precursor ions exiting from the conductive box possess kinetic energies corresponding to the difference between the second potential and the potential on the collisional cell prior to arrival at the collisional cell. Accordingly, the kinetic energies of the precursor ions on incidence of the collisional cell can be varied greatly according to the set value of the second potential. Hence, the variable range of collisional energies of the precursor ions can be made wider than conventional.

"(2) In one feature of this TOF mass spectrometer associated with the present invention, when the potential on the conductive box is varied, the potential control portion may vary the potential from the first potential to the second potential to decelerate the precursor ions before entering the collisional cell by the potential difference between the conductive box and the collisional cell.

"According to this TOF mass spectrometer associated with the present invention, precursor ions are decelerated before entering the collisional cell. Therefore, the kinetic energies possessed by the precursor ions on entering the collisional cell are smaller than the kinetic energies possessed by the precursor ions on entering the conductive box. Therefore, the collisional energies of the precursor ions can be varied according to the second potential in a wide range whose upper limit is defined by the kinetic energy of the precursor ions on entering the conductive box.

"(3) In a further feature of this TOF mass spectrometer associated with the present invention, the first potential may be the same as the potential on the first mass analyzer.

"(4) In a yet other feature of this TOF mass spectrometer associated with the present invention, the potential on the collisional cell may be the same as the potential on the first mass analyzer.

"(5) In an additional feature of this TOF mass spectrometer associated with the present invention, the potential control portion may vary a set range of the second potential according to valence numbers of the precursor ions.

"(6) In a yet other feature of this TOF mass spectrometer associated with the present invention, the potential control portion may set the second potential within a range in which the difference in absolute value between the second potential and the potential on the collisional cell is between V.sub.a.times.(1-1/z) and V.sub.a, where z is the valence number of precursor ions and V.sub.a is the accelerating potential difference between the ion source and the first mass analyzer.

"According to this TOF mass spectrometer associated with the present invention, the kinetic energies of ions exiting from the collisional cell can be held below the kinetic energies per valence given to the ions by the accelerating potential difference V.sub.a. Therefore, if a reflectron field capable of pushing back ions of kinetic energies per valence given by the accelerating potential difference V.sub.a is mounted in the second mass analyzer, all the ions can be pushed back by the reflectron field and reach the detector. As a result, fragmentations of multivalent ions can be efficiently observed, as well as fragmentations of monovalent ions.

"(7) In a still other feature of this TOF mass spectrometer associated with the present invention, the second mass analyzer may contain a reflectron field. A maximum kinetic energy per valence of ions capable of being pushed back by the reflectron field may be comparable to the kinetic energy per valence given to ions by the accelerating potential difference between the ion source and the first mass analyzer.

"According to this TOF mass spectrometer associated with the present invention, almost all ions having kinetic ions which are less than the kinetic energy per valence given to ions by the accelerating potential difference between the ion source and the first mass analyzer on entering the second mass analyzer can be pushed back by the reflectron field and reach the detector.

"(8) In a yet further feature of this TOF mass spectrometer associated with the present invention, a reacceleration portion for reaccelerating ions may be mounted between the collisional cell and the second mass analyzer.

"According to this TOF mass spectrometer associated with the present invention, where a reflectron field is produced in the second mass analyzer, for example, if product ions have low kinetic energies, kinetic energy is added to them by the reacceleration portion. Therefore, the product ions can be pushed back by the reflectron field and made to reach the detector.

"(9) In an additional feature of this TOF mass spectrometer associated with the present invention, the second mass analyzer may contain a reflectron field. A maximum kinetic energy per valence of ions capable of being pushed back by the reflectron field may be comparable to the sum of the kinetic energy per valence given to ions by the accelerating potential difference between the ion source and the first mass analyzer and the kinetic energy per valence given to ions by reacceleration made by the reacceleration portion.

"According to this TOF mass spectrometer associated with the present invention, all of ions having kinetic energies which are less than the kinetic energy per valence given to ions by the accelerating potential difference between the ion source and the first mass analyzer on entering the reacceleration portion can be pushed back by the reflectron field and reach the detector.

"(10) In an additional feature of this TOF mass spectrometer associated with the present invention, the reflectron field has a potential distribution that may contain a parabolic portion.

"According to this TOF mass spectrometer associated with the present invention, a sufficient length of free space can be secured in the second mass analyzer while maintaining the kinetic energy focusing.

"(11) In an additional feature of this TOF mass spectrometer associated with the present invention, the collisional cell and the first mass analyzer may be at ground potential.

"(12) Furthermore, the present invention provides a method of controlling a time-of-flight (TOF) mass spectrometer having: an ion source for ionizing a sample to thereby produce ions; a first mass analyzer for separating the produced ions according to flight time corresponding to mass-to-charge ratio; an ion gate for selecting precursor ions from ions separated and selected by the first mass analyzer; a conductive box through which the precursor ions selected by the ion gate pass; a collisional cell for fragmenting the precursor ions passed through the conductive box into product ions; a second mass analyzer for separating the precursor ions passed through the collisional cell and the product ions generated in the collisional cell according to flight time corresponding to mass-to-charge ratio; and a detector for detecting ions separated by the second mass analyzer. The method starts with setting the potential on the conductive box at a first potential when the precursor ions enter the conductive box. When the potential on the conductive box is varied, this potential is varied from the first potential to a second potential while the precursor ions are passing through the conductive box.

"Other features and advantages of the present invention will become apparent from the following more detailed description, taken in conjunction with the accompanying drawings, which illustrate, by way of example, the principles of the invention."

For the URL and additional information on this patent, see: Satoh, Takaya. Time-Of-Flight Mass Spectrometer and Method of Controlling Same. U.S. Patent Number 9536727, filed September 12, 2013, and published online on January 3, 2017. Patent URL: http://patft.uspto.gov/netacgi/nph-Parser?Sect1=PTO1&Sect2=HITOFF&d=PALL&p=1&u=%2Fnetahtml%2FPTO%2Fsrchnum.htm&r=1&f=G&l=50&s1=9536727.PN.&OS=PN/9536727RS=PN/9536727

Keywords for this news article include: JEOL Ltd., Technology Companies, Scientific and Technical Instrument Companies.

Our reports deliver fact-based news of research and discoveries from around the world. Copyright 2017, NewsRx LLC

(c) 2017 NewsRx LLC, source Science Newsletters

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Sales 2017 101 023 M
EBIT 2017 -
Net income 2017 143 M
Debt 2017 13 664 M
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