Method and system for solventless calibration of volatile or semi-volatile compounds

Patent metadata

Field	Value
Publication number	US-12233395-B2
Application number	US-202418615536-A
Country	US
Kind code	B2
Filing date	Mar 25, 2024
Priority date	Feb 23, 2018
Publication date	Feb 25, 2025
Grant date	Feb 25, 2025

Abstract

A system for solventless calibration of volatile or semi-volatile compounds and methods thereof. The system includes a fluid path having a first end configured to be operably coupled to a fluid source and a second end configured to be operably coupled to the analytical instrument. A solid sorbent is disposed along the fluid path and is configured to absorb an analyte. The flow of fluid along the fluid path from the first end to the second end causes absorbed analyte to be desorbed from the solid sorbent at a desired concentration to the instrument.

First claim

What is claimed is:

1. A method for solventless calibration, the method comprising:
positioning a microcalibrator in fluid communication with an analytical instrument, the microcalibrator comprising:
a first solid sorbent along a fluid path and configured to absorb an analyte at a first concentration; and
a second solid sorbent along the fluid path and configured to absorb the analyte at a second concentration;

said first solid sorbent and second solid sorbent being positioned parallel to each other;
initiating a fluid flow through the microcalibrator such that the analyte desorbs from the first solid sorbent, the second solid sorbent, or both to the analytical instrument; and
generating a calibration curve from the measured responses of the analytical instrument relative to the analyte desorbed at the first and second concentrations.

2. The method of claim 1 , wherein the first solid sorbent and the second solid sorbent are separately selected from the group consisting of graphitized carbon black, activated carbon, a porous polymer, or a xerogel.

3. The method of claim 1 , wherein the microcalibrator further comprises:
a valve configured to divert fluid flow between the first solids sorbent and the second solid sorbent.

4. The method of claim 1 , wherein the microcalibrator further comprises:
a controller configured to operate a flow of a fluid through the first solid sorbent, the second solid sorbent, or both.

5. The method of claim 1 , further comprising:
heating the first solid sorbent, the second solid sorbent, or both to facilitate desorption of the analyte.

6. The method of claim 1 , further comprising:
loading the first solid sorbent and the second solid sorbent with the analyte.

7. The method of claim 6 , wherein loading further comprises:
operably coupling an analyte source to the microcalibrator.

8. The method of claim 1 , wherein a rate of the fluid flow ranges from 5 mL/min to 100 mL/min.

9. The method of claim 1 , further comprising:
altering the fluid flow so as to adjust the first concentration, the second concentration, or both.

10. A method for solventless calibration, the method comprising:
positioning a microcalibrator in fluid communication with an analytical instrument, the microcalibrator comprising:
a first solid sorbent along a fluid path and configured to absorb an analyte at a first concentration; and
a second solid sorbent along the fluid path and configured to absorb the analyte at a second concentration;

said first solid sorbent and second solid sorbent being positioned parallel to each other;
initiating a first fluid flow through the microcalibrator such that the analyte desorbs from the first solid sorbent, the second solid sorbent, or both to the analytical instrument at the first and second concentrations, respectively; and
initiating a second fluid flow through the microcalibrator such that the analyte desorbs from the first solid sorbent, the second solid sorbent, or both to the analytical instrument at a third concentration and a fourth concentration, respectively.

11. The method of claim 10 , wherein the first solid sorbent and the second solid sorbent are separately selected from the group consisting of graphitized carbon black, activated carbon, a porous polymer, or a xerogel.

12. The method of claim 10 , wherein the microcalibrator further comprises:
a valve configured to divert fluid flow between the first solids sorbent and the second solid sorbent.

13. The method of claim 10 , wherein the microcalibrator further comprises:
a controller configured to operate a flow of a fluid through the first solid sorbent, the second solid sorbent, or both.

14. The method of claim 10 , further comprising:
heating the first solid sorbent, the second solid sorbent, or both to facilitate desorption of the analyte.

15. The method of claim 10 , further comprising:
loading the first solid sorbent and the second solid sorbent with the analyte.

16. The method of claim 15 , wherein loading further comprises:
operably coupling an analyte source to the microcalibrator.

17. The method of claim 1 , wherein a rate of the first and second fluid flows ranges from 5 mL/min to 100 mL/min.

Assignees

• Us Gov Air Force
• Us Air Force

Inventors

• Rubenstein Mitchell H
• Lewis Patrick

Classifications

• B01J20/285

  based on polymers · CPC title

• B01J20/283

  based on silica · CPC title

• B01J20/282

  Porous sorbents (ion exchange B01J39/00 - B01J41/00) · CPC title

• G01N2030/008

  Thermal desorption · CPC title

• G01N2030/328

  valves, e.g. check valves of pumps · CPC title