Vacuum electro-spray ion source and mass spectrometer

• US 10,475,634 B2
• Filed: 05/16/2018
• Issued: 11/12/2019
• Est. Priority Date: 04/12/2017
• Status: Active Grant

• Current Assignee: Tsinghua University
• Original Assignee: Tsinghua University
• Inventors: Yu, Quan, Zhang, Qian, Wang, Xiaohao, Qian, Xiang, Ni, Kai
• Primary Examiner(s): Smith, David E
• Application Number:
  US15/981,490
• Publication Number:
  US 20180301328A1
• Time in Patent Office: 545 Days
• CPC Class Codes: H01J 49/0404 Capillaries used for transferring samples or ions electrospray nozzles H01J49/167
• CPC Class Codes: H01J 49/0431 for liquid samples interfaces to liquid chromatographs G01N30/7233
• CPC Class Codes: H01J 49/045 with means for using a nebulising gas, i.e. pneumatically assisted
• CPC Class Codes: H01J 49/0495 Vacuum locks; Valves valves per se F16K
• CPC Class Codes: H01J 49/165 Electrospray ionisation
• CPC Class Codes: H01J 49/167 Capillaries and nozzles specially adapted therefor; electrostatic spraying per se B05B5/00

Abstract

The vacuum electro-spray ion source comprises a hollow capillary, a vacuum cavity, a gas inlet pipe, a gas supply device and an adjusting device, wherein a first end of the hollow capillary is a sampling port, and a second end is used as a spray nozzle for vacuum electro-sprays and stretches into the vacuum cavity; the air pressure in the vacuum cavity is ranged from 10 to 200 Pa; one end of the gas inlet pipe stretches into the vacuum cavity, and the other end is connected with the gas supply device; and the adjusting device is configured for adjusting the gas inlet pipe to allow the gas to flow therein intermittently. The ion source may achieve electro-spray ionization in the vacuum environment, so that losses during ion transmission may be reduced to improve the signal intensity and detection limit during detection.

Claims

1. A vacuum electro-spray ion source, comprising:

a hollow capillary,

a vacuum cavity,

a gas inlet pipe,

a gas supply device

an adjusting device; and

a three-way connector,

wherein a first end of the hollow capillary is a sampling port, and a second end is used as a spray nozzle for vacuum electro-sprays and stretches into the vacuum cavity;

the air pressure in the vacuum cavity is within a range of 10<sup>−

4</sup> to 200 Pa;

one end of the gas inlet pipe stretches into the vacuum cavity, and the other end is connected with the gas supply device; and

the adjusting device is configured for adjusting the gas inlet pipe to allow the gas to flow therein intermittently,

wherein the gas inlet pipe comprises a first hollow pipe and a second hollow pipe;

the second end of the hollow capillary sequentially passes through a first interface and a second interface of the three-way connector, and stretches into the vacuum cavity;

an end of the first hollow pipe is connected with an end of the second hollow pipe within the three-way connector, and the other end of the first hollow pipe passes through the second interface, and stretches into the vacuum cavity;

the other end of the second hollow pipe passes through a third interface of the three-way connector to be connected with the gas supply device, and

wherein the gas inlet pipe further comprises a third hollow pipe and a silica gel collapsible hose;

the adjusting device comprises a pinch valve;

an end of the third hollow pipe is connected with an end of the second hollow pipe within the pinch valve via the silica gel collapsible hose, and the other end of the third hollow pipe is connected with the gas supply device, wherein the pinch valve is used for controlling the circulation of gas flows between the third hollow pipe and the second hollow pipe.

2. The vacuum electro-spray ion source of claim 1, wherein the hollow capillary passes through an inner portion of the first hollow pipe within the three-way connector, and then, passes through the second interface at the same position with the first hollow pipe, and stretches into the vacuum cavity.

3. The vacuum electro-spray ion source of claim 2, wherein, in the vacuum cavity, a port of the hollow capillary is flush with respect to a port of the first hollow pipe or spaced apart less than 1 cm from a port of the first hollow pipe.

4. The vacuum electro-spray ion source of claim 1, wherein a gas supplied by the gas supply device is helium.

5. The vacuum electro-spray ion source of claim 1, wherein the sampling port of the hollow capillary is directly placed in a liquid sample, wherein the liquid sample is placed in an atmospheric environment and inserted therein with an electrode which is loaded with high voltage power.

6. The vacuum electro-spray ion source of claim 5, wherein the high voltage power is negative high voltage power in a range from −

5,000 V to −

1,000 V, or positive high voltage power in a range from 1,000 V to 5,000 V.

7. A mass spectrometer, comprising the vacuum electro-spray ion source of claim 1, wherein the vacuum cavity of the vacuum electro-spray ion source is in communication with a vacuum cavity of the mass spectrometer.

8. The mass spectrometer of claim 7, wherein a vacuum in the vacuum cavity of the vacuum electro-spray ion source is maintained by a mechanical pump, a vacuum in the vacuum cavity of the mass spectrometer is maintained by a turbo-molecular pump, and the mechanical pump is connected with the turbo-molecular pump and acts as a foreline pump of the turbo-molecular pump.