Quadrupole mass spectrometre

IPC classes for russian patent Quadrupole mass spectrometre (RU 2391740):

H01J49 - Particle spectrometers or separator tubes (for measuring gas pressure H01J0041100000)

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Method for serviceability check of ion-mobility spectrometer incorporating surface-ionized ion thermoemitter / 2263996

Proposed method for serviceability check of ion-mobility spectrometer incorporating surface-ionized ion thermoemitter, including spectrometer checkup dispensing with reference materials and for measuring spectrometer parameters in single cycle includes air pumping through spectrometer at volume velocity ranging between 2 and 10 l/min, application of dc voltage U_acc between thermoemitter plus and ion lens electrode minus, measurement of thermoemitter ion current I_te by means of external device, and setting of thermoemitter operating temperature T_op between 250 and 650 °C and U_acc between 30 and 600 V so as to provide for thermoemitter ion current I_te of (10^-11 - 10^-8) A; recording of ion drift spectrum; evaluation of half-width of ion current peak in drift spectrum at half its height ΔU, ion current peak maximum I_max, and compensating voltage U_c in ion current peak maximum; calculation of K_pc =(I_max/ I_te), and estimation of condition of ion mobility spectrometer incorporating surface-ionized ion thermoemitter by values of ΔU, K_pc, and U_c and shape of collector ion current peak including thermoemitter current I_te.

Ion spectrum measurement process and transit-time ion spectrometer / 2266587

Charge and mass composition is measured by accelerating ions in accelerating gap formed in vacuum chamber between input end of drift tube and plasma when negative-polarity voltage pulse of length shorter than transit time in drift tube of accelerated ions of plasma being analyzed is applied to drift tube at maximal Z/M_i ratio, where Z is ion charge in plasma; M_i is ion mass. Voltage pulse is supplied from negative-polarity accelerating-voltage pulse source whose high-voltage lead is electrically connected to drift tube and other lead, to vacuum-chamber ground. When in transit, accelerated ions are divided within drift tube into mass, charge, and energy clots and separated clots are recorded by detector.

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Proposed method for analyzing ions by specific charges in hyperboloid mass spectrometer of "three-dimensional ion trap" type includes introduction of ions into working space of analyzer, their entrapping by field, sorting out according to specific charges, followed by heir delivery to inlet of ion detector; ions are entrapped selectively by setting high-frequency supply voltage amplitude, and/or waveform, and/or frequency at which working point of ions being analyzed on stability diagram of at least one of coordinates on iso-β₀ line corresponding to β₀ =0 value, where β₀ is parameter of stability.

Method for analyzing ions by specific charges in hyperboloid mass spectrometer of type "three-dimensional trap" including introduction of ions being analyzed from outside / 2269180

Proposed method includes introduction of ions into working space of analyzer near its radial plane, their sorting out according to specific charges, and their delivery to ion detector input; parameters of high-frequency voltage applied to analyzer electrodes (waveform and/or amplitude, and/or frequency) are chosen so as to ensure that working point on one of coordinate axes of ions being analyzed is deep in stabilization zone and on other axis, near intersection point of mass spectrum line and stability zone boundary corresponding to β₀ = +1, where β₀ is parameter of stability.

Gas mixture analyzing device / 2272334

Proposed device has gas mixture ionizer with ion-optic system, stigmatically focused mass-spectrometer, solid-state converter, electrostatic analyzer, and recording unit, all arranged in tandem along motion direction of particles. Converter is made of ultra-thin diamond-like foil disposed at 45 deg. to motion direction of particles and in same plane as one of plates of electrostatic analyzer made in the form of flat capacitor. Converter is enclosed by cylinder to form combined Faraday cylinder whose axis coincides with motion direction of particles; cylinder, converter, and electrostatic analyzer plate are electrically insulated from one another; input of charged-particles recorder is disposed in same electrostatic analyzer plate as converter. Charged-particles converter can be made in the form of amplifier on microchannel strip or in the form of set of secondary electronic multipliers.

Mode of measuring of a common concentration of carbon and hydrocarbon oxides in oxygen with the aid of spectrometry of mobility of ions / 2273847

The mode includes the following operations: transformation of carbon and hydrocarbon oxide present in the flow of oxygen into dioxide; measuring of the concentration of carbon dioxide in oxygen after transformation; determination according to the results of measuring in accordance with the previous operation of the common initial concentration of carbon and hydrocarbon oxide.

Method and device for sorting out charged particles by specific charge / 2276426

Mass analyzer built around confined ion trap and designed to improve consumer properties as well as to extend service life of mass spectrometers using hyperboloid electrode systems has hyperboloid butt-end electrode and plane-confined annular one, cylindrical shielding and focusing electrodes, as well as semitransparent flat correcting electrode. Charged particles are produced due to electron shock in space between annular and correcting electrodes beyond working space of mass analyzer. Ions are entered in analyzer under action of accelerating voltage across correcting and focusing electrode; period and phase of accelerating voltage are coordinated with those of variable field and with original coordinates and speeds of charged particles. Sorted out ions are brought out through annular electrode hole and through semitransparent correcting electrode under action of positive voltage across butt-end electrode.

Method and device for sorting out charged particles by specific charge / 2276426

FIELD: physics.

SUBSTANCE: quadrupole mass spectrometre has an ion source, a quadrupole mass analyser which includes four field-forming electrodes in form of circular and hyperbolic cylinders lying in parallel and symmetrically about the central axis of the analyser, and an ion collector. Each of the field-forming electrodes of the analyser has a through slotted opening on the side of its input, parallel to the axis of the analyser and lying in its plane of symmetry. The beginning of each of the openings lies at a distance of (0.5-4.0)r₀ from the input faces of the analyser. The length of the opening along the axis inside the analyser is equal to (2.0-5.0)r₀ and the width of the opening is equal to (0.2-0.8)r₀, where r₀ is minimum distance from the axis of the mass spectrometre to each of the said field-forming electrodes of the analyser.

EFFECT: prevention of formation of semiconducting films and stray potential on electrodes of the mass analyser and therefore prevention of deterioration of analytical characteristics of the mass spectrometre with time.

2 cl, 6 dwg

The present invention relates to the field of mass spectrometry and will find application in addressing nanotechnology, nuclear physics, Geology, space research, organic and Bioorganic chemistry, immunology, biotechnology and medicine in the study of molecular, isotopic, elemental and structural composition of substances and materials.

As shown by long experience of operating a quadrupole mass spectrometers, from the input side of the analyzers on the inner surfaces of their preobrazuemyh electrodes made, for example, of molybdenum, when you work in the regime of intensive ion currents, especially when working with organic compounds, there is the appearance of dark deposits in the form of stripes parallel to the axis of the analyzer and lying in the planes of its symmetry.

A similar effect is observed in the manufacture preobrazuemyh electrodes of the analyzer from other metals and alloys, especially in the case of bombardment of the surface electrode ion currents with energies of several kilovolts. On the surfaces of the electrodes flow of ion-molecular reactions caused by the catalytic activity of the bombarded surfaces. Resulting from these processes, the semiconductor film is charged, causing the "wandering" of potential. These potentials claim shall indicate the working field mass analyzer and lead to deterioration of its analytical characteristics.

The number of internal instructions foreign quadrupole mass spectrometers, for example statements of the company Finnigan [1], provides recommendations, as without disassembly precision of the electrode Assembly analyzer (build made with micron precision and may not be reproduced by the user) using a tampon soaked in the recommended solvents, partially wash away these films on the inner surfaces of the electrodes from the entrance of ions into the analyzer to partially restore the analytical characteristics of the analyzer.

Known quadrupole mass spectrometer with an ion source with inductively coupled plasma ELAN 9000 company Perkin-Elmer (USA) [2], in which the electrodes of the quadrupole mass analyzer is made of ceramic material and have a metal coating made of gold. Ceramic electrodes are mounted in a ceramic washers that provides the same thermal expansion coefficient and geometric stability of an Assembly analyzer with temperature fluctuations. Gold-plated surface electrodes contribute to the preservation of the original analytical characteristics of the mass-analyzer - sensitivity, resolution, stability, amplitude and shape of the peaks, because gold does not possess catalytic properties and not Pref which leads to the formation of semiconductor films on the electrode surface during bombardment ion currents.

The disadvantages of the use of gold-plated electrodes should include greater technological complexity of applying precision uniform layer of gold on each of the electrodes, the overcoming of education wolnoobraznosti layer and maintaining the accuracy of the diameter of the electrodes within 1 μm (when the length of the electrodes is of the order of 200 mm and an average diameter of 7-10 mm). When the hyperbolic profile of the electrodes technology precision gold plating is further complicated because it is difficult to form the working electrode surface.

Known quadrupole mass spectrometer (UK application No. 2.099.216, firm VG) [3], in order to improve the parameters of the mass analyzer at its electrodes sprayed amorphous carbon. This reduces the probability of formation of parasitic electric fields resulting from bombardment of the electrodes of the ion currents and due to other causes contamination of the surfaces of the electrodes of the analyzer.

The disadvantage of this mass spectrometer is the fragility of coal deposition, it is easy damage that requires very careful work with elements and nodes, which are coated. Because of the vibrations and accidental bumps portion of the coating can flake off and get on those or other insulators analyzer, an ion source and multiplier and cause electrical breakdowns, leaks, etc., Thu is unacceptable for normal operation of the mass spectrometer.

The closest known mass spectrometric devices of the new generation, selected as a prototype, is the appliance company Agilent (USA) (The Agilent 5975C Series GC/MSD) [4]. In this device, released for commercial sale in 2007, applied the latest quadrupole mass analyzer, made of quartz in the form of a monolithic block with four hyperbolic surfaces facing the axis of the analyzer. On these surfaces through mnogokomponentnoe coated layer of gold with a view to long-term preservation of high analytical characteristics of the analyzer. A small temperature coefficient of expansion of quartz gives the characteristics of the analyzer stability in case of significant fluctuations in temperature.

The disadvantage of this analyzer is an extremely complex technology of manufacture and gilding. The application of precision composite and gold layers within micron precision and control sizes obtained by linear and angular parameters require unique expensive means of production and control of the internal structure of the monoblock mass analyzer.

The objective of the invention is to eliminate the appearance of semi-conducting films and "stray" stray potentials on the electrodes of the mass analyzer and, thus, the causes of deterioration over time analytical the features of the mass spectrometer, such as sensitivity, resolution, stability, amplitudes and shapes of the peaks, and in the end increase the resource of his work.

This problem is solved due to the fact that in the known quadrupole mass spectrometer containing the ion source, quadrupole mass analyzer consists of four preobrazuemyh electrodes in the form of a circular or hyperbolic cylinder, parallel to and symmetrically about the Central axis of the analyzer, and ion collector, each of preobrazuemyh electrodes of the analyzer from its input supplied through a slit hole parallel to the axis of the analyzer and lying in the plane of its symmetry. The beginning of each of the holes is located at a distance (0.5-4.0)r₀from the input ends of the analyzer. The length of the hole axis direction inside the analyzer is (2.0-5.0)r₀and the width of the holes (0.2-0.8)r₀where r₀is the radius of the field analyzer. In the case of circular small diameter electrodes each provided with a slot in a hollow groove directed toward the axis of the analyzer depth of not less than r₀. On the outer side of the analyzer over each through slot opening has an electrode whose potential relative to the electrode potential analyzer negative when working with positive ions and positive when dealing with the negative ions and is selected such if substantial sagging of the electric field inside the slot does not exceed (0.5-0.7)r₀.

The invention is illustrated by drawings, in which:

- figure 1 shows a General view of the inventive quadrupole mass spectrometer,

- figure 2 shows the stability triangle crossed by the line scan of the masses

- figure 3 shows a cross-section preobrazuemyh electrodes of the analyzer through the center slot and indicates the plane of symmetry and the radius field analyzer r₀,

- figure 4 shows the depth at which the SAG potential of the electrode to the inside slot, collecting ions that have passed through this hole,

- figure 5 shows the dimensions of the slits (grooves),

- figure 6 shows the location of the slits (grooves) in the case of hyperbolic electrodes.

Declared quadrupole mass spectrometer (figure 1) consists of an ion source (1), preobrazuemyh electrodes (2) mass analyzer, supplied through slotted holes (3)arranged in parallel along the axis (4) of the analyzer by the input analyzer, lying in the planes of its symmetry, and the receiver ions (5).

In the case when the mass analyzer is used preobrazilsya electrodes of small diameter (d_e<5 mm), through the slotted holes can lead to the loss of rigidity of the electrode when otnositel the wide slotted holes. In this case, the through holes may be replaced by blind grooves facing toward the axis of the analyzer and having a depth of not less than r₀where r₀the radius field of the analyzer.

The device operates as follows. Ion beam produced from the ion source, is input to the mass analyzer along the axis preobrazuemyh electrodes. Ions, on the transmission which is configured of the mass analyzer, reach the exit of the analyzer and arrive at the receiver ions. Ions with masses greater noise mass and significantly less noise masses, who constitute the major part of the total ion current, rejected field preobrazuemyh electrodes and through the slotted holes are outside of the analyzer.

The reason for the appearance of semi-conductive films on the working surfaces of the electrodes of the analyzer is illustrated in figure 2, which presents the stability triangle in the coordinates of a and q, and apply a line scanner, which marked the location of the ions of different masses in the areas of X - and Y-stability when the scan of the mass spectrometer. For example, considered the moment when the mass analyzer is configured to allow mass 100 Amu In this case, all the masses, large 100 Amu, unstable Y, so at the entrance to the mass analyzer of their amplitudes grow exponentially, and they reach the Y-electrodes directly is near the entrance inside the area analyzer. These masses are in the field of X-stability. Therefore, the flow of these ions is a flat on the x-coordinate of the beam with the exponential increase of the amplitudes of these ions on the y coordinate because of a difference of masses and initial energies of the ions formed by the length of the beam along the Y-electrodes, and in the area of the bombing on Y-electrodes formed long trail along the Z-coordinate having a small width and symmetrical relative to the plane Y0Z.

All ions with masses less than 100 Amu, on the contrary, the fragile X-coordinate, and their trajectories at the entrance to the mass analyzer grow on this coordinate is also exponentially. At the same time trajectories of these ions stable Y-coordinate as the line scan for the ions of these masses is in the Y-stability. In the end, these ions create a flat beam bombarding X-electrodes. He also has a length due to differences in mass and range of ions on the initial velocities, creating on the X-electrodes trace in the form of a strip of small width, parallel to the axis 0Z analyzer and symmetrical relative to the plane X0Z.

In the process of scanning the mass range from light weight to heavy (this case is shown in figure 2) with the configuration of ions on the sequential transmission of more heavy weight fractions of light and heavy mass falling on the X - and Y-electr the water, change, but the nature of the process is preserved.

Deep analyzer are only those ions that are close in mass to noise Jonah, and Jonah, with zero coordinates and angles of the entrance. But such ions in the total ion current, which is included in the mass analyzer, a little, and they do not play a major role in the creation of semi-conductive films on the electrodes of the analyzer.

In figure 2 the arrows indicate the movement of ions of different masses along the line scan when the scan mass spectrum due to the increase of the amplitude V of the variable component of the potential φ=±(U+Vcosωt)applied to the electrodes of the analyzer as:

where e is the particle charge, m is the mass of the particle, ω is the circular frequency of the applied high-frequency voltage, r₀- the minimum distance from the axis of the analyzer, to each of the electrodes (radius field analyzer).

Figure 3 shows a cross-section of the electrodes of the analyzer through the center slot. 3, and illustrates the location of the through slot, figure 3, b shows the location of the holes made in the form of grooves, figure 3, shows the arrangement of electrodes on each of the through slot and the polarity of the potentials applied to the electrodes, for the case of operation with positive ions.

Applied potentials, slack through the slotted hole is, must not penetrate into the working region of the mass analyzer, so as not to cause distortion of his working field. Therefore, the magnitude of the potential depends on the geometric dimensions of the slot so that the distorting effect of the SAG did not affect the analytical characteristics of the analyzer. The dimensions of the slits and grooves obtained experimentally in the long-term tests, the electrodes of the analyzer, we offer you mass spectrometer must be the following value: beginning of holes from the input end of the electrode analyzer l₁=(0.5-4.0), the length of the holes l₂=(2.0-5.0)r₀the width of the holes b=(0.2-0.8)r₀where r₀is the radius of the field of the quadrupole mass analyzer, i.e. the minimum distance from its axis to each of the electrodes of the analyzer (figure 5).

The location of the slot when using a mass analyzer electrodes in the shape of a hyperbolic cylinder (6) fully complies with the requirements of their location in the electrodes of circular cross-section in units of r₀where r₀- the minimum distance from the axis of the analyzer, to each of its electrodes, including requirements for the installation of electrodes for cracks and the value attached to them capacity.

In the proposed quadrupole mass spectrometer, through careful study of ion trek the oriy noise and no noise ions, as well as consideration of the fact of the formation of sludge in the form of longitudinal narrow strip on each of the electrodes of the mass analyzer near its input end inside the analyzer is proposed to provide the electrodes of the analyzer in place of the formation of these residues slots, which will "fall through" ions that create the sludge at specified locations on the surfaces preobrazuemyh electrodes of the analyzer, which is the semi-conducting films.

Thus, the exception occurrence of semi-conductive films and "stray" stray potentials on the electrodes removes the very cause of the deterioration over time of the analytical characteristics of the mass analyzer. Technologically, the opening of the through slit or groove, for example, length (5.0-10.0) mm and width (1.0-2.0) mm molybdenum preobrazuem electrode is much easier in comparison with the process precision of the gilding surface as a separate preobrazuemyh electrodes, and, especially, monoblock. The presence of such cracks in the electrodes, the diameter of which exceeds 5 mm, does not reduce their stiffness and does not affect the diameter of the electrodes.

Long experience quadrupole mass spectrometer MS, in the mass analyzer were performed through the slotted holes showed that for at least 10 years characteristics of the mass spectrometer, the electrodes are made of molyb is s, was unchanged and has not deteriorated compared to the original.

Literature

1. Gas Chromatograph. / Mass Spectrometer. / Data System. Model 4021. The user guide. Finnigan Instr. Ltd., U.K., 1978.

2. Instruction manual mass spectrometer ELAN 9000 company Perkin-Elmer (USA), 1999, Walthen, USA.

3. UK application No. 2099216. "A method of improving the parameters of the mass spectrometer and the floor, realizing this method, the company VG, 1982.

4. The prospectus of the company Agilent Technologies, 2007. "Mass spectrometer S Series GC/MSD".

1. Quadrupole mass spectrometer containing the ion source, quadrupole mass analyzer, comprising four preobrazuemyh electrode in the form of a circular or hyperbolic cylinder, parallel to and symmetrically about the Central axis of the analyzer, and ion collector, characterized in that each of preobrazuemyh electrodes of the analyzer from its input supplied through a slit hole parallel to the axis of the analyzer and lying in the plane of its symmetry, the beginning of each of the holes is located at a distance (0,5-4,0)r₀from the input ends of the analyzer, the length of the hole along the axis inside the analyzer is (2,0-5,0)r₀and the width of the holes (0,2-0,8)r₀where r₀- the minimum distance from the axis of the mass analyzer to each of preobrazuemyh electrodes of the analyzer.

2. Quadrupole mass-Spa is trometer according to claim 1, characterized in that on the outer side of the analyzer over each through slot opening has an electrode whose potential relative to the electrode potential analyzer negative when working with positive ions and positive when working with negative ions and the magnitude of the positive potential is selected such that the slack of the electric field inside the slot does not exceed (0,5-0,7)r₀.