Gas-liquid contact extraction method and apparatus

Patent metadata

Field	Value
Publication number	US-9347919-B2
Application number	US-201214358744-A
Country	US
Kind code	B2
Filing date	Nov 16, 2012
Priority date	Nov 17, 2011
Publication date	May 24, 2016
Grant date	May 24, 2016

Abstract

The present invention provides a method and apparatus for rapidly extracting the analyte existing in the liquid phase in analyzing an analyte “having a large partition coefficient in gas-liquid equilibrium”, “having a high water solubility”, or “having a low olfactory threshold” by a gas-liquid contact extraction method, and further provides, a method and apparatus for unmanned continuous sample introduction of the analyte to a GC or the like for a long time. In the present invention, using a gas-liquid contact extractor to which a sample liquid is continuously introduced from above and a purge gas from beneath, the analyte in the sample liquid is extracted by gas-liquid contact between the sample liquid and the purge gas. A discharge pipe is connected to the bottom of the gas-liquid contact extractor, the pipe having a liquid sump through which the sample liquid is discharged, while blocking the outflow of the purge gas from the liquid sump.

First claim

We claim:

1. A gas-liquid contact extraction method using a gas-liquid contact extractor to which a sample liquid is continuously introduced from above and a purge gas from beneath, for extracting an analyte in the sample liquid by gas-liquid contact between the sample liquid and the purge gas, the method comprising discharging the sample liquid through a liquid sump provided to a discharge pipe connected to a bottom of the gas-liquid contact extractor, while blocking outflow of the purge gas from the liquid sump, wherein the sample liquid is preheated to an extraction temperature in the gas-liquid contact extractor prior to supplying the sample liquid to the gas-liquid contact extractor.

2. The gas-liquid contact extraction method according to claim 1 , wherein a water-soluble component having a partition coefficient K larger than 1 or an analyte having an olfactory threshold lower than 10 ppt (pg/ml) existing in the sample liquid is gas-liquid contact extracted.

3. The gas-liquid contact extraction method according to claim 2 , wherein the gas-liquid contact extractor is provided in a temperature-controlled oven, and a temperature of a flow channel to a collection tube for condensing the gas-liquid contact extracted analyte is set to a temperature equal to or higher than an oven temperature (gas-liquid extraction temperature), so that the gas-liquid extracted analyte is condensed in the collection tube.

4. The gas-liquid contact extraction method according to claim 1 , wherein the gas-liquid contact extractor is provided in a temperature-controlled oven, and a temperature of a flow channel to a collection tube for condensing the gas-liquid contact extracted analyte is set to a temperature equal to or higher than an oven temperature (gas-liquid extraction temperature), so that the gas-liquid extracted analyte is condensed in the collection tube.

5. A gas-liquid contact extraction apparatus comprising a gas-liquid contact extractor to be supplied with a liquid sample from above and a purge gas from beneath, a discharge pipe connected to the bottom of the gas-liquid contact extractor, a liquid sump provided to the discharge pipe for discharging the sample liquid and blocking the discharge of the purge gas, and a collection tube for condensing the gas-liquid contact extracted analyte, wherein the gas-liquid contact extractor is provided in a temperature-controlled oven and is adapted to provide a temperature of a flow channel to the collection tube for condensing the gas-liquid contact extracted analyte set to a temperature equal to or higher than an oven temperature.

6. The gas-liquid contact extraction apparatus according to claim 5 , wherein the contact surface of the gas-liquid contact extractor with a sample liquid is surface treated to achieve a spread wetting state.

7. An automatic liquid sample supply apparatus comprising a liquid sample supply part connected to the gas-liquid contact extraction apparatus according to claim 6 through a syringe pump and a selector valve for switching a flow channel, allowing an analyte gas-liquid contact extracted by the gas-liquid contact extraction apparatus to be sent to a collection tube.

8. The gas-liquid contact extraction apparatus according to claim 6 , wherein the surface treatment is any one of a hydrophilic treatment and a water repellent treatment.

9. An automatic liquid sample supply apparatus comprising a liquid sample supply part connected to the gas-liquid contact extraction apparatus according to claim 8 through a syringe pump and a selector valve for switching a flow channel, allowing an analyte gas-liquid contact extracted by the gas-liquid contact extraction apparatus to be sent to a collection tube.

10. An automatic liquid sample supply apparatus comprising a liquid sample supply part connected to the gas-liquid contact extraction apparatus according to claim 5 through a syringe pump and a selector valve for switching a flow channel, allowing an analyte gas-liquid contact extracted by the gas-liquid contact extraction apparatus to be sent to a collection tube.

11. A gas-liquid contact extraction method using a gas-liquid contact extractor to which a sample liquid is continuously introduced from above and a purge gas from beneath, for extracting an analyte in the sample liquid by gas-liquid contact between the sample liquid and the purge gas, the method comprising discharging the sample liquid through a liquid sump provided to a discharge pipe connected to a bottom of the gas-liquid contact extractor, while blocking outflow of the purge gas from the liquid sump, wherein the gas-liquid contact extractor is provided in a temperature-controlled oven, and a temperature of a flow channel to a collection tube for condensing the gas-liquid contact extracted analyte is set to a temperature equal to or higher than an oven temperature (gas-liquid extraction temperature), so that the gas-liquid extracted analyte is condensed in the collection tube.

12. The gas-liquid contact extraction method according to claim 11 , wherein a water-soluble component having a partition coefficient K larger than 1 or an analyte having an olfactory threshold lower than 10 ppt (pg/ml) existing in the sample liquid is gas-liquid contact extracted.

Assignees

• Shimadzu Corp
• Gl Sciences Inc
• Gl Sciences Inc

Inventors

• Fukumoto Shinji
• Yamauchi Hiroshi
• Aono Akira
• Shimomura Manabu
• Takei Yoshiyuki
• Mimura Tadashi
• Suzuki Akira
• Furuno Masahiro

Classifications

• B01D3/346

  the gas being used for removing vapours, e.g. transport gas · CPC title

• G01N2001/4066

  using difference of solubility between liquid and gas, e.g. bubbling, scrubbing or sparging · CPC title

• G01N30/7206

  interfaced to gas chromatograph (interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04) · CPC title

• G01N1/24

  Suction devices {(G01N1/22 - G01N1/2294 take precedence)} · CPC title

• G01N30/06 Primary

  Preparation · CPC title