# US 2017/0284976 A1 · Gas chromatographic "in-column" spectroscopic analysis

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- Number: US 2017/0284976 A1
- Document ID: US20170284976A1
- Status: Published application
- Kind: A1
- Application number: 15/464,378
- Filed: 2017-03-21
- Published: 2017-10-05
- Earliest claimed: 2013-03-15
- Assignees: The Govt. of the U.S.A., as represented by the Secretary of the Navy
- Applicants: The Govt. of the U.S.A., as represented by the Secretary of the Navy
- Inventors: R. Andrew McGill; Robert Furstenberg; Viet K. Nguyen; Chris Kendziora; Michael Papantonakis; Todd H. Stievater
- Web page: https://patentgrep.com/patent/US20170284976A1

## CPC

- G01N 30/74: Optical detectors {(measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J)}
- B01J 20/285: based on polymers
- G01N 21/0332: {with temperature control (control of temperature G05D23/00; cryostats F17C3/08)}
- G01N 21/3504: for analysing gases, e.g. multi-gas analysis
- G01N 21/39: using tunable lasers
- G01N 21/552: Attenuated total reflection
- G01N 21/7746: {the waveguide coupled to a cavity resonator}
- G01N 30/02: Column chromatography
- G01N 30/6034: {joining multiple columns}
- G01N 21/658: {enhancement Raman, e.g. surface plasmons}
- G01N 30/6082: {transparent to radiation}
- G01N 2021/4761: {Mirror arrangements, e.g. in IR range}
- G01N 2030/025: {Gas chromatography}
- 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)
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

A chemical detector for rapid, simultaneous detection of multiple chemicals including chemical warfare agents, toxic industrial chemicals, and explosives having one or more gas chromatography columns each with a chemosorbent or a chemo-reactive stationary phase and an infrared-transparent base, a bright infrared light source, a mechanism to direct the light source to any point along any of the columns, and an infrared sensor. Another disclosed detector has one or more gas chromatography columns each on the surface of a substrate having at least one infrared-transparent waveguide pattern, a bright infrared light source, and at least one ring resonator for each column, where each ring resonator is coated with a chemosorbent or a chemo-reactive stationary phase, and where each ring resonator spectroscopically probes the stationary phase. Also disclosed are the related methods for chemical detection.

## Claims

### Claim 1

A chemical detector for simultaneous detection of multiple chemicals including chemical warfare agents, toxic industrial chemicals, and explosives, comprising:
one or more gas chromatography columns, wherein each column comprises one or more chemosorbent or chemo-reactive stationary phases, and wherein each column has an infrared-transparent base;
an infrared light source;
a moveable mirror to direct the light source to the more than one gas chromatography columns, wherein the light source can be directed to any point along any of the columns or to a preconcentrator or collector device, wherein in-column chemical detection can occur at all points along every column; and
an infrared sensor.

### Claim 2 (depends on 1)

The chemical detector of claim 1, wherein when there is more than one column, each column is operated in parallel.

### Claim 3 (depends on 1)

The chemical detector of claim 1, wherein at least one stationary phase comprises a carbosilane material with hydrogen bond acidic functionalization.

### Claim 4 (depends on 1)

The chemical detector of claim 1, wherein the infrared-transparent base comprises an attenuated total reflection (ATR) crystal.

### Claim 5 (depends on 1)

The chemical detector of claim 1, wherein the infrared light source comprises one or more optionally tunable infrared lasers, and more preferably the bright infrared light source comprises one or more quantum cascade lasers (QCLs).

### Claim 6 (depends on 1)

The chemical detector of claim 1, additionally comprising a focusing lens used with the moveable mirror to direct the light source.

### Claim 7 (depends on 1)

The chemical detector of claim 1, additionally comprising an analyte preconcentrator comprising sorbent coated structures positioned before or at the inlet end of at least one of the columns.

### Claim 8 (depends on 1)

The chemical detector of claim 1, additionally comprising one or more independently controlled heating elements along one or more columns.

### Claim 9

A method for simultaneous detection of multiple chemicals including chemical warfare agents, toxic industrial chemicals, and explosives, comprising:
injecting a vapor-phase analyte sample into one or more gas chromatography columns, wherein each column comprises one or more chemosorbent or chemo-reactive stationary phases, and wherein each column has an infrared-transparent base;
directing an infrared light source to a point at one of the columns, wherein the light source can be directed to any point along any of the columns or to a preconcentrator or collector device, wherein in-column chemical detection can occur at all points along every column; and
using an infrared sensor to detect for the presence of chemicals.

### Claim 10 (depends on 9)

The method of claim 9, wherein when there is more than one column, each column is operated in parallel.

### Claim 11 (depends on 9)

The method of claim 9, wherein at least one stationary phase comprises a carbosilane material with hydrogen bond acidic functionalization.

### Claim 12 (depends on 9)

The method of claim 9, wherein the infrared-transparent base comprises an attenuated total reflection (ATR) crystal.

### Claim 13 (depends on 9)

The method of claim 9, wherein the infrared light source comprises one or more optionally tunable infrared lasers, and more preferably the bright infrared light source comprises one or more quantum cascade lasers (QCL).
