# US 12,002,672 B2 · Apparatus and methods for reduced neutral contamination in a mass spectrometer

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- Number: US 12,002,672 B2
- Document ID: US12002672B2
- Status: Granted
- Kind: B2
- Application number: 16/630,007
- Filed: 2018-06-29
- Published: 2021-03-25
- Granted: 2024-06-04
- Earliest claimed: 2017-07-11
- Assignees: DH Technologies Development Pte. Ltd.
- Applicants: DH Technologies Development Pte. Ltd.
- Inventors: Bruce Collings; Pascal Martin
- Web page: https://patentgrep.com/patent/US12002672B2

## CPC

- H01J 49/067: {Ion lenses, apertures, skimmers}
- H01J 49/0031: {Step by step routines describing the use of the apparatus (H01J49/0081 takes precedence)}
- H01J 49/4225: {Multipole linear ion traps, e.g. quadrupoles, hexapoles}
- H01J 49/426: {Methods for controlling ions}
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)

## Abstract

Apparatus and methods for controlling contamination of components contained within the high-vacuum chambers of mass spectrometer systems are provided. The apparatus and methods employ a beam of neutral gas injected in a contra-flow configuration to incoming particle stream from the ionization chamber. The contra-flow can be in the directly opposite counter-flow direction (e.g., 180 degrees) or at a cross-flow angle to the incoming ion stream (e.g., flowing at an angle between about 10 degrees and 170 degrees). The contra-flow disrupts the axial gas flow and diverts neutral molecules and other undesirable contaminants before they reach the high vacuum stages (e.g., beyond the IQ0 orifice) of the spectrometer. By reducing the transmission of contaminants into the sensitive components housed deep within the mass spectrometer, the present invention can increase throughput, improve robustness, and/or decrease the downtime typically required to vent/disassemble/clean the fouled components.

## Claims

### Claim 1

Apparatus for reducing contamination in a mass spectrometer comprising:
an ionization chamber for generating a beam of ions;
an ion guide having a plurality of rods arranged in a multipole configuration and spaced from one another to provide a channel through which an ion stream comprising ions generated in the ionization chamber can be transmitted to one or more downstream mass analyzers, the ion guide channel comprising a guide inlet aperture in communication with said ionization chamber and a guide exit aperture for passing ions to said downstream mass analyzers,
a power supply for providing voltage to one or more of said plurality of rods for confining the ions within an internal volume of the ion guide channel;
a curtain gas inlet for introducing an internal curtain gas into the ion guide channel at a volumetric flow rate of at least 0.1 standard liter per minute (slpm) flowing in a contra flow direction to the ion stream, such that the internal curtain gas flow facilitates removal of neutral molecules from the ion stream.

### Claim 2 (depends on 1)

The apparatus of claim 1 wherein the curtain gas inlet and ion guide channel are configured such that the internal curtain gas is directed in the contra-flow direction to ions passing through the ion guide channel.

### Claim 3 (depends on 1)

The apparatus of claim 1 wherein the internal curtain gas is introduced in a direction at least orthogonal to the direction of ions passing through the ion guide channel.

### Claim 4 (depends on 1)

The apparatus of claim 1 wherein the internal curtain gas is introduced in a direction from about 10 degrees to about 180 degrees contrary to the direction of ions passing through the ion guide channel.

### Claim 5 (depends on 1)

The apparatus of claim 1 wherein the internal curtain gas is introduced in a direction substantially parallel but opposite to the direction of ions passing through the ion guide channel.

### Claim 6

Apparatus for reducing contamination in a mass spectrometer, comprising:
an ionization chamber for generating a beam of ions;
an ion guide having a quadrupole rod set including a plurality of rods arranged in a quadrupole configuration and spaced from one another to provide a channel through which ions generated in the ionization chamber can be transmitted to one or more downstream mass analyzers, the ion guide channel comprising a guide inlet aperture in communication with said ionization chamber and a guide exit aperture for passing ions to said downstream mass analyzers,
a power supply for providing voltage to one or more of said plurality of rods for confining the ions within an internal volume of the ion guide channel; and
a curtain gas inlet for introducing an internal curtain gas into the ion guide channel at a volumetric flow rate of at least 0.1 standard liter per minute (slpm), such that the internal curtain gas flow facilitates removal of the neutral molecules,
wherein the ion guide channel inlet aperture is configured to allow generation of a supersonic free jet expansion comprising a barrel shock of predetermined diameter downstream of the inlet aperture, and wherein a cross-section of the ion guide channel defined by a radial distance between two radially opposed rods of the quadrupole rod set is sized to be at least 50% of the predetermined diameter of the barrel shock of the supersonic jet expansion.

### Claim 7 (depends on 1)

The apparatus of claim 1, further comprising an internal curtain gas supply for flowing curtain gas into the ion guide channel, where internal curtain gas flow is effective to prevent at least a portion of unwanted molecules within a sample from transiting to the ion guide channel exit aperture.

### Claim 8 (depends on 7)

The apparatus of claim 7, wherein the curtain gas supply is operatively coupled to a controller adapted to adjust the volumetric flow rate of curtain gas.

### Claim 9

A method for controlling contamination in a mass spectrometer system, comprising:
generating one or more ionized species from a sample within an ionization chamber;
directing an ion stream comprising ions generated in the ionization chamber through a channel of an ion guide having a plurality of rods arranged in a multipole configuration and spaced from one another to provide the channel to one or more downstream mass analyzers, the ion guide channel comprising an inlet aperture in communication with said ionization chamber and an exit aperture for passing ions to said downstream mass analyzers; and
introducing an internal curtain gas into the ion guide channel at a volumetric flow rate of at least 0.1 standard liter per minute (slpm) flowing in a contra flow direction to the ion stream, such that internal curtain gas flow facilitates removal of neutral molecules from the ion stream.

### Claim 10 (depends on 9)

The method of claim 9 wherein the curtain gas inlet and ion guide channel are configured such that the internal curtain gas is directed in a counter-flow direction to ions passing through the ion guide channel and into a diversion port for evacuating the internal curtain gas and neutral molecules entrained therewith.

### Claim 11 (depends on 9)

The method of claim 9 wherein the internal curtain gas is introduced in a cross-flow direction at least orthogonal to the direction of ions passing through the ion guide channel.

### Claim 12 (depends on 11)

The method of claim 11 wherein the internal curtain gas is introduced is a cross-flow direction from about 10 degrees to about 170 degrees counter to the direction of ions passing the ion guide channel.

### Claim 13 (depends on 9)

The method of claim 9 wherein the internal curtain gas is introduced in a direct counter-flow direction substantially parallel but opposite to the direction of ions passing through the ion guide channel.

### Claim 14 (depends on 9)

The method of claim 9 wherein internal curtain gas flow is effective to prevent at least a portion of unwanted molecules within a sample from transition to the ion guide channel exit aperture.

### Claim 15 (depends on 14)

The method of claim 14 wherein supply of the curtain gas is controlled by a controller adapted to adjust the volumetric flow rate of the curtain gas.

### Claim 16 (depends on 1)

The apparatus of claim 1 wherein said volumetric flow rate is at least 0.2 standard liter per minute (slpm).

### Claim 17 (depends on 1)

The apparatus of claim 1 wherein said internal curtain gas is introduced into said ion guide at a pressure greater than about 1 Torr.

### Claim 18 (depends on 1)

The apparatus of claim 1 further comprising a de-clustering region positioned between said ionization chamber and said ion guide.

### Claim 19 (depends on 1)

The apparatus of claim 1, further comprising:
a gas curtain chamber disposed between said ionization chamber and said ion guide,
a first gas source for providing a curtain gas flow into said gas curtain chamber,
a second gas source for providing said internal curtain gas into said ion guide channel.

### Claim 20 (depends on 19)

The apparatus of claim 19, wherein said first and second gas sources are independently controlled.

### Claim 21 (depends on 1)

The apparatus of claim 1, wherein said ionization chamber comprises a curtain plate defining a curtain plate aperture through which the ion stream can pass, wherein the ion guide defines a longitudinal axis, and wherein the apparatus further comprises another ion guide, positioned downstream of the ion guide and upstream of the one or more mass analyzers, receiving ions exiting the ion guide, said other ion guide comprising another plurality of rods arranged in a quadrupole configuration and spaced from one another for radially focusing the received ions.

### Claim 22 (depends on 1)

The apparatus of claim 1, further comprising a vacuum chamber comprising the ion guide and located downstream of the ionization chamber, the ion guide maintained at a pressure of between 1 Torr to 7.5 Torr, wherein the ion guide is configured to capture and focus ions using a combination of gas dynamics and radio frequency fields.

### Claim 23 (depends on 1)

The apparatus of claim 1, wherein the internal curtain gas is introduced into the ion guide channel at a volumetric flow rate of between 0.1 slpm and 1 slpm.