# US 9,752,966 B2 · Cryofocused sampling of volatiles from air using peltier-assisted capillary microextraction

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- Number: US 9,752,966 B2
- Document ID: US9752966B2
- Status: Granted
- Kind: B2
- Application number: 15/246,866
- Filed: 2016-08-25
- Published: 2016-12-29
- Granted: 2017-09-05
- Earliest claimed: 2016-08-25
- Assignees: The Florida International University Board of Trustees
- Applicants: Jose Almirall; Anamary Tarifa
- Inventors: Jose Almirall; Anamary Tarifa
- Web page: https://patentgrep.com/patent/US9752966B2

## CPC

- G01N 1/24: Suction devices {(G01N1/22 - G01N1/2294 take precedence)}
- G01N 1/2273: {Atmospheric sampling}
- G01N 1/405: {by adsorption or absorption}
- G01N 33/0047: {Organic compounds}
- H01J 49/0027: {Methods for using particle spectrometers}
- H01J 49/0422: {for gaseous samples (interfaces to gas chromatographs G01N30/7206)}
- H01J 49/0431: {for liquid samples (interfaces to liquid chromatographs G01N30/7233)}
- G01N 2001/2229: {Headspace sampling, i.e. vapour over liquid}
- G01N 2001/2282: {with cooling means}
- G01N 2030/062: {extracting sample from raw material}
- G01N 2030/122: {cryogenic focusing}
- 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 CMV sampling device includes a thermoelectric cooler, a vacuum pump, and one or more holders for one or more capillary microextractor of volatiles (CMV) tubes. The holder thermally contacts the thermoelectric cooler and the vacuum pump is fluidly connected to the CMV tube. The CMV device is useful for sampling of volatile organic compounds from air. The sampling can be carried out rapidly to achieve a sample within the CMV tube that may be placed into a thermal desorption unit (TDU) coupled to an inlet port for introduction of the volatiles into an analytical instrument, such as, a gas chromatograph (GC), an ion mobility spectrometer (IMS), a liquid chromatograph (LC), and/or a mass spectrometer (MS) for analysis of one or more volatiles.

## Claims

### Claim 1

A CMV sampling device, comprising a thermoelectric cooler, a vacuum pump, and at least one holder for a capillary microextractor of volatiles (CMV) tube and at least one CMV tube, wherein the thermoelectric cooler thermally contacts the holder, and wherein the vacuum pump is fluidly connected to the CMV tube.

### Claim 2 (depends on 1)

The CMV sampling device according to claim 1, wherein the CMV tube comprises a polydimethylsiloxane (PDMS) gel on glass fibers within a glass tube.

### Claim 3 (depends on 1)

The CMV sampling device according to claim 1, further comprising an aluminum block as a heat sink.

### Claim 4 (depends on 1)

The CMV sampling device according to claim 1, wherein the vacuum pump can draw 1 L/min.

### Claim 5 (depends on 1)

The CMV sampling device according to claim 1, wherein the thermoelectric cooler is a single stage Peltier cooler.

### Claim 6

A method for the sampling of volatile organic compounds from air, comprising:
providing a CMV sampling device comprising at least one capillary microextractor of volatiles (CMV) tube fluidly connected to a vacuum pump and at least one holder for the (CMV) tube thermally contacting a thermoelectric cooler;
powering the vacuum pump to produce an air flow of the air of a site suspected of containing a target volatile organic compound through the CMV tube; cooling the at least one holder and the at least one CMV tube to a temperature below the ambient temperature of the air; and
maintaining the air flow and the cooling for a prescribed period of time.

### Claim 7 (depends on 6)

The method of claim 6, wherein the air flow and cooling is maintained for a period of 1 to 10 minutes.

### Claim 8 (depends on 6)

The method of claim 6, wherein the temperature is −15 to 5° C.

### Claim 9 (depends on 6)

A method for analyzing volatile organic compounds from air, comprising:
acquiring a sample according to the method of claim 6;
placing the CMV tube into a thermal desorption unit (TDU);
coupling the TDU to an inlet port of an instrument for analysis of a volatile; and
heating the TDU to a temperature sufficient for desorbing the diagnostic volatile from the CMV, wherein the diagnostic volatile is introduced into the instrument for analysis of a volatile.

### Claim 10 (depends on 9)

The method of claim 9, wherein the instrument for analysis of a volatile comprises a gas chromatograph (GC), an ion mobility spectrometer (IMS), a liquid chromatograph (LC), a mass spectrometer (MS), or any combination thereof.