IP Library › Granted Patent US 11,067,548

Granted Patent B2

US 11,067,548 · App. 15/479,122 · Granted Jul 20, 2021

Multi-capillary column pre-concentration system for enhanced sensitivity in gas chromatography (GC) and gas chromatography-mass spectrometry (GCMS)

Inventor: Daniel B. Cardin (Simi Valley, CA)

G01N30/14 B01L3/502 G01N1/405 G01N1/44 G01N30/12 G01N30/30 G01N30/461 G01N30/7206 B01L2200/10 B01L2300/0627 B01L2300/0838 B01L2300/16 B01L2300/18 G01N30/40 G01N30/6078 G01N2030/121 G01N2030/128 G01N2030/143

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Quick Facts

Patent No.: US 11,067,548
App. No.: 15/479,122
Granted: Jul 20, 2021
Kind: B2

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USPTO Patent Center↗ Full Patent PDF↗

Abstract

A multi-capillary column pre-concentration trap for use in various chromatography techniques (e.g., gas chromatography (GC) or gas chromatography-mass spectrometry (GCMS)) is disclosed. In some examples, the trap can include a plurality of capillary columns connected in series in order of increasing strength (i.e., increasing chemical affinity for one or more sample compounds). A sample can enter the trap, flowing from a sample vial to a relatively weak column to the relatively strongest column of the trap by way of any additional columns included in the trap, for example. In some examples, the trap can be heated and backflushed so that the sample exits the trap through the head of the relatively weak column. Next, the sample can be injected into a chemical analysis device for performing the chromatography technique (e.g., GC or GCMS) or it can be injected into a secondary multi-capillary column trap for further concentration.

Claims (111)

1. A first trap for pre-concentrating a sample before chemical analysis, the first trap comprising a first primary capillary column, a second primary capillary column, and a third primary capillary column connected in series with increasing affinity, wherein:

the first primary capillary column has an interior surface coated by a first sorbent, the first primary capillary column having a length between 0.2 and 5 meters, the first primary capillary column with the first sorbent having a first affinity for one or more compounds of the sample, wherein the first primary capillary column having the interior surface coated by the first sorbent is configured to adsorb one or more compounds while the first primary capillary column has a temperature between 20 and 50 degrees Celsius;

the second primary capillary column has an interior surface coated by a second sorbent, the second sorbent having a higher affinity for the one or more compounds than an affinity the first sorbent has for the one or more compounds, the second primary capillary column having a length between 0.2 and 5 meters, the second primary capillary column with the second sorbent having a second affinity for the one or more compounds of the sample, the second affinity greater than the first affinity, wherein the second primary capillary column having the interior surface coated by the second sorbent is configured to adsorb one or more compounds while the second primary capillary column has a temperature between 20 and 50 degrees Celsius;

the third primary capillary column has an interior surface coated by a third sorbent, the third sorbent having a higher affinity for the one or more compounds than the affinity the second sorbent has for the one or more compounds, the third primary capillary column having a length between 0.2 and 5 meters, the third primary capillary column with the third sorbent having a third affinity for the one or more compounds of the sample, the third affinity greater than the second affinity, wherein the second primary capillary column is coupled between the first primary capillary column and the third primary capillary column in series, wherein the third primary capillary column having the interior surface coated by the third sorbent is configured to adsorb one or more compounds while the third primary capillary column has a temperature between 20 and 50 degrees Celsius; and

one or more valves configured to:

during an adsorption process during which the first primary capillary column, the second primary capillary column and the third primary capillary column are at an adsorption temperature between 20 and 50 degrees Celsius, facilitate the sample to flow through the first primary capillary column, the second primary capillary column, and the third primary capillary column in a first direction, the first direction being from the first primary capillary column to the third primary capillary column, and

during a desorption process, facilitate a desorption gas to flow through the first primary capillary column, the second primary capillary column, and the third primary capillary column in a second direction, the second direction being from the third primary capillary column to the first primary capillary column.

2. The first trap of claim 1 , wherein:

the first, second, and third primary capillary columns are open-tubular capillary columns,

the first sorbent coating the interior surface of the first primary capillary column leaves a first open passageway through the first capillary column,

the second sorbent coating the interior surface of the second primary capillary column leaves a second open passageway through the second capillary column, and

the third sorbent coating the interior surface of the third primary capillary column leaves a third open passageway through the third capillary column.

3. The first trap of claim 1 , further comprising a heater, wherein:

during the desorption process, the heater heats the first trap to a desorption temperature between 100 and 300 degrees Celsius.

4. The first trap of claim 3 , wherein:

the heater is positioned a first distance from the first primary capillary column,

the heater is positioned a second distance less than the first distance from the second primary capillary column,

the heater is positioned a third distance less than the second distance from the third primary capillary column,

at a respective time during the desorption process:

the first primary capillary column has a first temperature,

the second primary capillary column has a second temperature greater than the first temperature, and

the third primary capillary column has a third temperature greater than the second temperature.

5. The first trap of claim 1 , further comprising:

a desorption port between the first primary capillary column and a chemical analysis device; and

an exit port coupled to an exit port end of the third primary capillary column, wherein the second primary capillary column is coupled to an end of the third primary capillary column that is opposite the exit port end of the third primary capillary column, wherein:

during the desorption process, the desorption gas enters the third primary capillary column through the third primary capillary column and flows through the first, second, and third primary capillary columns in the second direction,

the desorption process causes the sample to desorb from the first, second, and third primary capillary columns in the second direction,

during the desorption process, the one or more valves allow the desorbed sample and the desorption gas to flow from the first primary capillary column to the chemical analysis device through the desorption port, and

the chemical analysis device performs the chemical analysis on the desorbed sample.

6. The first trap of claim 1 , further comprising:

during the adsorption process, the one or more valves facilitate the flow of water vapor included in the sample through the first, second, and third primary capillary columns through the exit port, thereby removing the water vapor included in the sample from the first trap, and

during the adsorption process, the first primary capillary column, the second primary capillary column, and the third primary capillary column are at the adsorption temperature between 20 and 50 degrees Celsius.

7. The first trap of claim 1 , further comprising a first desorption port between the first primary capillary column and a second trap wherein:

the desorption process causes the sample to desorb from the first, second, and third primary capillary columns,

during the desorption process, the one or more valves allow the desorbed sample to flow from the first primary capillary column to the second trap through the first desorption port, and

the second trap comprises a first secondary capillary column and a second secondary capillary column connected in series with increasing affinity, wherein:

the first secondary capillary column has an interior surface coated by a fourth sorbent, wherein the first secondary capillary column having the interior surface coated by the fourth sorbent is configured to adsorb one or more compounds while the first secondary capillary column has a temperature between 20 and 50 degrees Celsius, the first secondary capillary column having a first end switchably couplable to the first desorption port,

the second secondary capillary column has an interior surface coated by a fifth sorbent, wherein the second secondary capillary column having the interior surface coated by the fifth sorbent is configured to adsorb one or more compounds while the second secondary capillary column has a temperature between 20 and 50 degrees Celsius, the second secondary capillary column having a first end coupled to the first secondary capillary column, and

the second trap further comprises one or more second valves configured to:

during a second adsorption process, allow the desorbed sample from the first trap to flow through the first secondary capillary column and the second secondary capillary column in a third direction, the third direction being from the first end of the first secondary capillary column to an opposite end of the second secondary capillary column that is opposite from the first end of the second secondary capillary column, and

during a second desorption process, allow a second desorption gas to flow through the first secondary capillary column and second secondary capillary column in a fourth direction, the fourth direction being from the opposite end of the second secondary capillary column to the first end of the first secondary capillary column.

8. The first trap of claim 7 , wherein the second trap includes a same number of capillary columns as the first trap or fewer capillary columns than the first trap.

9. The first trap of claim 7 , wherein the first secondary capillary column of the second trap is shorter than the first, second, and third primary capillary columns of the first trap, and the second secondary capillary column of the second trap is shorter than the first, second, and third primary capillary columns of the first trap.

10. The first trap of claim 7 , wherein:

the second trap further comprises a second desorption port switchably couplable to the first end of the first secondary capillary column,

the second desorption process causes the sample to desorb from the first secondary capillary column and the second secondary capillary column,

during the second desorption process, the one or more second valves allow the desorbed sample from the second secondary capillary column to flow from the second secondary capillary column to the first secondary capillary column and allow the desorbed sample from the first secondary capillary column to flow from the first secondary capillary column to the chemical analysis device through the second desorption port, and

the chemical analysis device performs the chemical analysis on the desorbed sample from the first secondary capillary column and the second secondary capillary column.

11. A method of pre-concentrating a sample before chemical analysis, the method comprising:

during an adsorption process of a first trap, the first trap comprising a first primary capillary column, a second primary capillary column, and a third primary capillary column connected in series with increasing affinity, during which the first primary capillary column of the first trap, the second primary capillary column of the first trap, and the third primary capillary column of the first trap are a at an adsorption temperature between 20 and 50 degrees Celsius:

facilitating, via one or more valves, the sample to flow through the first primary capillary column of the first trap, the second primary capillary column of the first trap, and the third primary capillary column of the first trap in a first direction, the first direction being from the first primary capillary column to the third primary capillary column; and

during a desorption process:

facilitating, via the plurality of valves, a desorption gas to flow through the first primary capillary column, the second primary capillary column, and the third primary capillary column in a second direction, the second direction being from the third primary capillary column to the first primary capillary column,

wherein:

the first primary capillary column has an interior surface coated by a first sorbent, the first primary capillary column with the first sorbent having a first affinity for one or more compounds of the sample, the first primary capillary column having a length between 0.2 and 5 meters,

the first primary capillary column, the second primary capillary column, and the third primary capillary column are coupled in series.

12. The method of claim 11 , further comprising:

during the desorption process, heating the first trap to a desorption temperature with a heater of the first trap, the desorption temperature between 100 and 300 degrees Celsius.

13. The method of claim 11 , further comprising:

during the desorption process:

causing the desorption gas to enter the third primary capillary column through an exit port of the first trap, the exit port coupled to an exit port end of the third primary capillary column, wherein the second primary capillary column is coupled to an end of the third primary capillary column that is opposite the exit port end of the third primary capillary column,

causing the sample to desorb from the first, second, and third primary capillary columns in the second direction; and

allowing, via the one or more valves, the desorbed sample and the desorption gas to flow from the first primary capillary column to a chemical analysis device through a desorption port between the first primary capillary column and the chemical analysis device; and

performing the chemical analysis on the desorbed sample with the chemical analysis device.

14. The method of claim 11 , further comprising:

during the adsorption process, facilitating, via the one or more valves, water vapor included in the sample to flow through the first, second, and third primary capillary columns through an exit port of the first trap, thereby removing the water vapor included in the sample from the first trap

wherein:

the exit port of the first trap is coupled to an exit port end of the third primary capillary column, and

the second primary capillary column is coupled to an end of the third primary capillary column that is opposite the exit port end of the third primary capillary column.

15. The method of claim 13 , wherein the desorption process causes the sample to desorb from the first, second, and third primary capillary columns, and during the desorption process, the one or more valves allow the desorbed sample to flow from the first primary capillary column to a second trap through a first desorption port of the first trap, the method further comprising:

during a second adsorption process, allowing, via one or more second valves of the second trap, the desorbed sample to flow through a secondary capillary column of the second trap in a third direction, the third direction being from a first end of the secondary capillary column to an opposite end of the secondary capillary column, and

during a second desorption process, allowing, via the one or more second valves, a second desorption gas to flow through the secondary capillary column in a fourth direction, the fourth direction being from the opposite end of secondary capillary column to the first end of the secondary capillary column.

16. The method of claim 15 , further comprising:

during the second desorption process:

desorbing the sample from the secondary capillary column; and

allowing, via the one or more second valves, the desorbed sample from the secondary capillary column to flow from the secondary capillary column into a chemical analysis device through a second desorption port of the second trap; and

performing, with the chemical analysis device, the chemical analysis on the desorbed sample from the secondary capillary column.

17. A system comprising:

a sample container containing a sample;

a first trap, the first trap comprising a first primary capillary column, a second primary capillary column, and a third primary capillary column connected in series with increasing affinity, wherein:

a chemical analysis device, the chemical analysis device comprising a detector configured to detect one or more compounds of the sample; and

one or more valves fluidly coupling the first trap to the sample container, the one or more valves configured to:

during an adsorption process during which the first primary capillary column, the second primary capillary column, and the third primary capillary column are at an adsorption temperature between 20 and 50 degrees Celsius, facilitate the sample to flow from the sample container through the first primary capillary column, the second primary capillary column, and the third primary capillary column in a first direction, the first direction being from the first primary capillary column to the third primary capillary column, and

18. The system of claim 17 , wherein the first trap further comprises a desorption port between the first primary capillary column and the chemical analysis device, wherein:

the desorption process causes the sample to desorb from the first, second, and third primary capillary columns,

during the desorption process, the one or more valves allow the desorbed sample to flow from the first primary capillary column to the chemical analysis device through the desorption port, and

the chemical analysis device performs the chemical analysis on the desorbed sample.

19. The system of claim 17 , further comprising:

a second trap fluidly coupled to a desorption port of the first trap and to the chemical analysis device by way of the one or more valves, the second trap comprising a first secondary capillary column and a second secondary capillary column connected in series with increasing affinity, wherein:

the desorption process is a first desorption process, and

the one or more valves are further configured to:

during the first desorption process, allow the sample to desorb from the first, second, and third primary capillary columns and flow from the first primary capillary column to the second trap through the desorption port of the first trap;

during a second adsorption process, allow the desorbed sample from the first trap to flow through the first secondary capillary column and the second secondary capillary column in a third direction, the third direction being from a first end of the first secondary capillary column to an opposite end of the second secondary capillary column that is opposite from the first end of the second secondary capillary column; and

during a second desorption process, allow a second desorption gas to flow through the first secondary capillary column and the second secondary capillary column in a fourth direction, the fourth direction being from the opposite end of the second secondary capillary column to the first end of the first secondary capillary column and into the chemical analysis device through a second desorption port of the second trap.

20. The first trap of claim 1 , wherein:

the first primary capillary column has a first inner diameter less than 0.021 inches,

the second primary capillary column has a second inner diameter less than 0.021 inches, and

the third primary capillary column has a third inner diameter less than 0.021 inches.

21. The first trap of claim 7 , wherein:

the sample has a first volume when exiting the first trap, and

the sample has a second volume less than the first volume when exiting the second trap.

Assignments (1)

ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 26, 2017

From: CARDIN, DANIEL B.

To: ENTECH INSTRUMENTS INC.

Reel/Frame 042154/0920 →

Continuity (2)

Provisional Application 62318061 · Apr 4, 2016

Related Publication 20170284978A1 · Oct 5, 2017