# US 11,828,739 B2 · Large volume gas chromatography injection port

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- Number: US 11,828,739 B2
- Document ID: US11828739B2
- Status: Granted
- Kind: B2
- Application number: 17/457,120
- Filed: 2021-12-01
- Published: 2022-03-17
- Granted: 2023-11-28
- Earliest claimed: 2017-08-29
- Assignees: Mls Acq, Inc.
- Applicants: MLS ACQ, Inc.
- Inventors: Kelly Renee McPartland; Martin L. Spartz
- Web page: https://patentgrep.com/patent/US11828739B2

## CPC

- G01N 30/74: Optical detectors {(measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J)}
- G01J 3/18: using diffraction elements, e.g. grating (gratings per se G02B)
- G01J 3/42: Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry (beam switching arrangements G01J3/08)
- G01N 21/3504: for analysing gases, e.g. multi-gas analysis
- G01N 30/12: by evaporation
- G01N 30/16: Injection (G01N30/24 takes precedence)
- G01N 30/20: using a sampling valve
- G01N 30/30: of temperature
- G01N 30/32: of pressure or speed (G01N30/36 takes precedence)
- G01N 30/40: using back flushing
- 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)}
- G01N 2021/3595: {using FTIR}
- G01N 2030/008: {Thermal desorption}
- G01N 2030/025: {Gas chromatography}
- G01N 2030/121: {cooling; cold traps}
- G01N 2030/128: {Thermal desorption analysis}
- G01N 2030/328: {valves, e.g. check valves of pumps}
- G01N 2030/402: {purging a device}
- G01N 2030/743: {FTIR}
- 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)
- G01J: MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY (light sources F21, H01J, H01K, H05B; investigating properties of materials by optical means G01N)

## Abstract

A method and system for sample analysis involve a temporally-resolving separation of sample components. In the method, solvent vapors are condensed prior to entering a temporally-resolving separator, a GC column, for example, and solvent-depleted vapors are directed to the separator where constituents are resolved in time. A system for analyzing a sample comprises an injection port, a temporally-resolving separator (e.g., a GC column) and a conduit connecting the two. The injection port is at a temperature sufficiently high to vaporize the solvent and analytes present in a sample. The conduit is configured and/or operated to condense the solvent, while maintaining the analytes in the vapor phase.

## Claims

### Claim 1

A sample analysis method, comprising:
vaporizing a solvent and analytes present in a sample;
condensing solvent vapors upstream of a temporally-resolving separator to produce a solvent-depleted vapor component;
passing the solvent-depleted vapor component through the temporally-resolving separator, thereby resolving in time analytes present in the solvent-depleted vapor component; and
analyzing the time-resolved analytes with a Fourier transform infrared spectrometer.

### Claim 2 (depends on 1)

The sample analysis method of claim 1, further comprising evacuating the condensed solvent vapors.

### Claim 3 (depends on 1)

The sample method of claim 1, wherein the solvent is water and is present in the sample in an amount of at least 99 volume percent.

### Claim 4 (depends on 1)

The sample analysis method of claim 1, wherein the sample is provided by direct injection and without sample splitting.

### Claim 5 (depends on 1)

The sample analysis method of claim 1, wherein the solvent vapor is condensed in a transfer line upstream of the temporally-resolving separator.

### Claim 6 (depends on 1)

The sample analysis method of claim 1, wherein the temporally-resolving separator is a GC column.

### Claim 7 (depends on 1)

The sample analysis method of claim 1, wherein at least a portion of solvent vapors condenses on inner surfaces of a transfer line.

### Claim 8

A sample analysis method, comprising:
vaporizing a sample containing a solvent and analytes from a thermal desorption tube or a cryo-trap;
condensing solvent vapors upstream of a temporally-resolving separator to produce a solvent-depleted vapor component; and
passing the solvent-depleted vapor component through the temporally-resolving separator, thereby resolving in time analytes present in the solvent-depleted vapor component.

### Claim 9 (depends on 8)

The sample analysis method of claim 8, wherein the method does not employ a secondary thermal desorption tube.

### Claim 10 (depends on 8)

The sample analysis method of claim 8, further comprising a mass spectrometry or an optical spectrometry analyzer.

### Claim 11 (depends on 8)

The sample analysis method of claim 8, wherein solvent vapors are condensed downstream of the thermal desorption tube or the cryo-trap.

### Claim 12

A sample analysis system, comprising:
an injection port;
a temporally-resolving separator;
a conduit connecting the injection port and the temporally-resolving separator; and
a Fourier transform infrared spectrometer for analyzing time-resolved analytes from the temporally-resolving separator,
wherein,
the injection port is at a temperature sufficiently high to vaporize a solvent and analytes present in a sample; and
the conduit is configured to condense the solvent and maintain the analytes in the vapor phase.

### Claim 13 (depends on 12)

The sample analysis system of claim 12, wherein the temporally-resolving separator is a GC column.

### Claim 14 (depends on 12)

The sample analysis system of claim 12, further comprising an arrangement for cooling or heating or both cooling and heating the conduit and/or heating the injection port.

### Claim 15 (depends on 12)

The sample analysis system of claim 12, further comprising an arrangement for removing the condensed solvent from an interior of the conduit.

### Claim 16 (depends on 12)

The sample analysis system of claim 12, wherein the conduit includes one or more changes in cross section.

### Claim 17 (depends on 12)

The sample analysis system of claim 12, further comprising a controller.

### Claim 18 (depends on 12)

The sample analysis system of claim 12, further comprising an arrangement for detecting a temperature of the conduit or for detecting a temperature of the injection port or for detecting a temperature of both the conduit and the injection port.

### Claim 19 (depends on 12)

The sample analysis system of claim 12, wherein the conduit is configured to condense solvent vapors on inner conduit surfaces.

### Claim 20

A sample analysis system, comprising:
a thermal desorption tube or a cryo-trap;
a conduit for passing vapors from the thermal desorption tube or the cryotrap to a temporally-resolving separator,
wherein,
the conduit is configured to condense the solvent and maintain the analytes in the vapor phase.

### Claim 21 (depends on 20)

The sample analysis system of claim 20, wherein the system does not employ a secondary thermal desorption tube.

### Claim 22 (depends on 20)

The sample analysis system of claim 20, further comprising a mass spectrometry or an optical spectrometry analyzer.

### Claim 23 (depends on 8)

The sample analysis method of claim 8, wherein the sample is not introduced via an injection port.

### Claim 24 (depends on 20)

The sample analysis system of claim 20, wherein the system does not include an injection port.