Methods and apparatuses for trace and ultratrace analysis

Patent metadata

Field	Value
Publication number	US-10139317-B2
Application number	US-201514928694-A
Country	US
Kind code	B2
Filing date	Oct 30, 2015
Priority date	Oct 30, 2015
Publication date	Nov 27, 2018
Grant date	Nov 27, 2018

Abstract

Methods of analyzing analytes from a liquid medium are disclosed. A system and apparatus for the analysis of analytes from a liquid medium are further disclosed. In particular, methods and apparatus of analyzing analytes by freezing liquid medium and partitioning the analyte into a sorptive stirrer are disclosed. Further, the methods and apparatus of the present invention can be useful in concentrating and isolating target chemicals of high value.

First claim

What is claimed is:

1. A method of extracting a solute from a liquid medium, comprising:
stirring a liquid medium containing an analyte in a sample container with a sorptive stirrer comprising a sorptive material;
cooling the sample container while the analyte is being stirred so the liquid medium freezes and the analyte is concentrated and absorbed into or adsorbed by the sorptive material, wherein said cooling is done by a cooling source; and
simultaneously extracting the analyte into or by the sorptive material while the analyte is concentrated.

2. The method of claim 1 , wherein said sorptive stirrer is an overhead stirrer or a magnetic sorptive stir bar rotated by a magnetic stir plate, magnetic U-shaped bracket, donut-shaped magnet, or electromagnetic field generator; and wherein said sorptive stirrer optionally comprises a chemically-inert coating, jacket, or layer.

3. The method of claim 2 , wherein said magnetic U-shaped bracket or donut-shaped magnet rotates around said cooling source.

4. The method of claim 1 , wherein said stirring step further comprises incrementally lowering the sample container into the cooling source.

5. The method of claim 1 , further comprising a step of measuring variables of the method, wherein the measuring step measures temperature, speed of the sample container movement, speed of the sorptive stirrer, and combinations thereof.

6. The method of claim 1 , further comprising a step of controlling the method using control software.

7. A method of extracting a solute from water, comprising:
stirring water containing an analyte in a sample container with a sorptive stirrer comprising a sorptive material;
cooling the sample container while the water is being stirred so the water freezes and the analyte is concentrated and absorbed into the sorptive stir bar; and
simultaneously extracting the analyte into or by the sorptive material while the analyte is concentrated.

8. The method of claim 7 further comprising identifying and/or quantifying the analyte with an analytical technique including one or more of the following: gas-chromatography and mass-spectroscopy (GCMS), thermal desorption GCMS, liquid chromatography, fluorometry, or spectroscopy.

9. The method of claim 8 , further comprising quantifying the analyte in an amount of nanograms to femtograms.

10. The method of claim 9 , wherein the cooling is performed by a cooling source, and wherein the sample container is placed in or on said cooling source.

11. The method of claim 10 , wherein the cooling source is a cold bath, a jacketed beaker, a coolant, a cooled air system, a thermoelectric device, helium, or a nitrogen system.

12. The method of claim 11 , wherein sorptive stirrer is a magnetic stir bar or overhead stirrer with a sorptive material; and wherein said sorptive stirrer optionally comprises a chemically-inert coating, jacket, or layer.

13. The method of claim 12 , wherein the stirring is performed by a magnetic stir plate, a rotating magnetic U-shaped bracket, or a rotating magnetic donut-shaped component of an electromagnetic field generator that generates a rotating magnetic field around said sample container.

14. The method of claim 13 , further comprising a step of lowering the sample container into the cooling source to facilitate freezing of the water.

15. The method of claim 14 , wherein the lowering is performed by a stepper motor.

16. The method of claim 14 , further comprising the step of measuring one and or more variables including temperature, speed of the sample container movement, speed of the stir bar, magnetic field strength and/or position, spectroscopic parameters, and/or combinations thereof.

17. The method of claim 16 , further comprising controlling with a control software the temperature, speed of the sample container movement, speed of the stir bar, magnetic field strength and/or position, spectroscopic parameters, and/or combinations thereof.

Assignees

• South Dakota Board Of Regents

Inventors

• Logue Brian

Classifications

• G01N1/42

  Low-temperature sample treatment, e.g. cryofixation · CPC title

• G01N33/18

  Water · CPC title

• B01D15/02

  with moving adsorbents · CPC title

• G01N2001/1068

  Cooling sample below melting point · CPC title

• G01N1/10 Primary

  in the liquid or fluent state {(burettes, pipettes B01L3/02; sampling of ground water E02D1/06; metering by volume of fluids or fluent solid material G01F11/00, G01F13/00)} · CPC title