# US 11,360,059 B2 · Portable mems GC-MS system

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- Number: US 11,360,059 B2
- Document ID: US11360059B2
- Status: Granted
- Kind: B2
- Application number: 15/929,133
- Filed: 2019-05-31
- Published: 2020-12-03
- Granted: 2022-06-14
- Earliest claimed: 2019-05-31
- Assignees: Mass Tech, Inc.
- Applicants: Mass Tech, Inc.
- Inventors: Vladimir M. Doroshenko; Victor V. Laiko
- Web page: https://patentgrep.com/patent/US11360059B2

## CPC

- G01N 30/7206: {interfaced to gas chromatograph (interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04)}
- H01J 49/0013: {Miniaturised spectrometers, e.g. having smaller than usual scale, integrated conventional components}
- G01N 30/30: of temperature
- G01N 30/6095: {Micromachined or nanomachined, e.g. micro- or nanosize}
- H01J 49/0022: {Portable spectrometers, e.g. devices comprising independent power supply, constructional details relating to portability (small scale devices per se H01J49/0013 and H01J49/0018)}
- G01N 2030/0095: {Separation specially adapted for use outside laboratory, e.g. field sampling, portable equipments}
- G01N 2030/3015: {temperature gradients along column}
- G01N 2030/3053: {using resistive heating}
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)

## Abstract

A system and method for sample analysis using a portable gas chromatography (GC)-mass spectrometry (MS) is provided. The GC-MS system includes an injector configured to accept a sample containing a mixture of chemicals and release at least part of the sample for a separation by GC, a MEMS GC column with an integrated heater configured to accept and at least partly separate the mixture of chemicals, and a mass analyzer in a vacuum chamber configured to accept and mass-analyze the released separated chemicals. The MEMS GC column with the integrated heater is located mostly inside the MS vacuum chamber.

## Claims

### Claim 1

An apparatus for analysis of chemical samples using a gas chromatography (GC) interfaced with a mass spectrometer (MS), comprising:
an injector configured to inject a sample containing a mixture of chemicals;
a GC column configured to receive at least part of the sample and separate at least partly the mixture of chemicals contained in the at least part of the sample, said GC column having a GC column inlet to accept said at least part of the sample, and a GC column outlet to release the at least partly separated chemicals of the mixture;
a heater attached to the GC column,
a mass analyzer configured to mass-analyze the released at least partly separated chemicals; and
a vacuum system configured to generate a vacuum, the mass analyzer being located inside the vacuum system,
wherein most of an external surface of the GC column is located inside said vacuum system and exposed to the vacuum.

### Claim 2 (depends on 1)

The apparatus as recited in claim 1 wherein said heater is integrated with the GC column.

### Claim 3 (depends on 1)

The apparatus as recited in claim 1 wherein said GC column is a low-thermal mass capillary GC column.

### Claim 4 (depends on 1)

The apparatus as recited in claim 1 wherein said heater is an electric resistive heater.

### Claim 5 (depends on 1)

The apparatus as recited in claim 1 wherein said GC column is a Micro-Electro Mechanical Systems (MEMS) GC column.

### Claim 6 (depends on 5)

The apparatus as recited in claim 5 wherein said heater is one of an electric resistive film heater and an electric resistive platinum film heater.

### Claim 7 (depends on 1)

The apparatus as recited in claim 1 wherein said GC column has a planar shape and is disposed substantially parallel to a wall of said vacuum system.

### Claim 8 (depends on 1)

The apparatus as recited in claim 1 wherein said heater is configured to generate a negative temperature gradient from the GC column inlet toward the GC column outlet.

### Claim 9 (depends on 1)

The apparatus as recited in claim 1 wherein said GC column additionally includes a cooler configured to cool the GC column.

### Claim 10 (depends on 9)

The apparatus as recited in claim 9 wherein said cooler is a fan.

### Claim 11 (depends on 9)

The apparatus as recited in claim 9 wherein said cooler is a periodically activated cold finger cooler.

### Claim 12 (depends on 11)

The apparatus as recited in claim 11 wherein said cold finger is configured to be physically detached from the GC column during said analysis and in thermal contact with the GC column after the analysis is completed.

### Claim 13 (depends on 11)

The apparatus as recited in claim 11 wherein a thermal mass of said cold finger is substantially higher than a thermal mass of said GC column.

### Claim 14 (depends on 1)

The apparatus as recited in claim 1 wherein said mass analyzer is at least one of quadrupole, quadrupole ion trap, Orbitrap, time-of-flight, and Fourier transform ion cyclotron resonance mass analyzer type.

### Claim 15 (depends on 1)

The apparatus as recited in claim 1 wherein said mass analyzer is a MEMS mass analyzer.

### Claim 16 (depends on 1)

The apparatus as recited in claim 1 wherein said mass analyzer includes an ion source configured to generate ions from molecules of the separated at least partly chemicals of the mixture released from the GC column outlet.

### Claim 17 (depends on 16)

The apparatus as recited in claim 16 wherein said ion source is at least one of electron impact, photoionization, gas discharge, glow discharge, and chemical ionization type.

### Claim 18 (depends on 16)

The apparatus as recited in claim 16 wherein said ion source includes an ionization chamber.

### Claim 19 (depends on 18)

The apparatus as recited in claim 18 wherein said ionization chamber is heated.

### Claim 20 (depends on 18)

The apparatus as recited in claim 18 wherein said GC column outlet is adjacent to said ionization chamber.

### Claim 21 (depends on 18)

The apparatus as recited in claim 18 wherein said mass analyzer includes an ion guide configured to extract said ions from the ionization chamber for further mass-analysis.

### Claim 22 (depends on 5)

The apparatus as recited in claim 5 wherein said MEMS GC column is designed as a thin chip having two major sides and at least a first one of said major sides is mostly located inside the vacuum system.

### Claim 23 (depends on 22)

The apparatus as recited in claim 22, wherein
the vacuum system comprises a wall with an aperture; and
a second one of said major sides is disposed sealed against the wall and surrounding the aperture.

### Claim 24 (depends on 1)

The apparatus as recited in claim 1 wherein said injector includes at least one of a split injector, programmed temperature vaporizer, and cold on-column injector.

### Claim 25 (depends on 1)

The apparatus as recited in claim 1 wherein said injector is a MEMS injector having an integrated injector heater.

### Claim 26 (depends on 25)

The apparatus as recited in claim 25 wherein said MEMS injector with the integrated MEMS heater is mostly located inside said vacuum system.

### Claim 27 (depends on 1)

The apparatus as recited in claim 1, wherein the vacuum system comprises a wall with an aperture; and
the injector is disposed sealed within the aperture.

### Claim 28 (depends on 1)

The apparatus as recited in claim 1, wherein the vacuum system comprises a wall with an aperture; and
the GC column is disposed sealed against the wall and surrounding the aperture.

### Claim 29

A method for analysis of chemical samples using a gas chromatography (GC) column interfaced with a mass spectrometer (MS), comprising the steps of:
generating a vacuum;
positioning most of an external surface of the GC column to be exposed to the vacuum;
injecting a sample containing a mixture of chemicals into the GC column;
heating said GC column in the vacuum so the chemicals of the mixture are at least partly separated by the GC column; and
mass-analyzing the chemicals separated by the GC column.

### Claim 30 (depends on 29)

The method as recited in claim 29, wherein the GC column has a planar structure with an inlet portion and a peripheral portion surrounding the inlet portion, the method comprising:
heating the GC column with a heater integrated with the GC column at a position on the GC column corresponding to the inlet portion and not integrated with the GC column in the peripheral portion.

### Claim 31 (depends on 29)

The method as recited in claim 29, wherein the GC column comprises a chip, the method comprising:
heating the chip inside the vacuum.

### Claim 32 (depends on 1)

The apparatus as recited in claim 1, wherein the GC inlet and GC outlet are located within the vacuum system.

### Claim 33 (depends on 22)

The apparatus as recited in claim 22 wherein said thin chip is located entirely inside the vacuum system.
