Focusing agents and methods of using same

Patent metadata

Field	Value
Publication number	US-11215596-B2
Application number	US-201916415118-A
Country	US
Kind code	B2
Filing date	May 17, 2019
Priority date	Mar 8, 2016
Publication date	Jan 4, 2022
Grant date	Jan 4, 2022

Abstract

A method for reducing the variability, as measured by relative standard deviation (RSD), of an analytical testing technique is provided. This improvement in RSD improves the confidence in the values obtained during field testing. The method includes incorporating a focusing agent into the sampling media, which permits providing sampling media such as thermal desorption tubes preloaded with the focusing agent.

First claim

What is claimed is:

1. A method for reducing a relative standard deviation (RSD) in an analytical chromatographical testing procedure for quantifying a chemical agent, comprising:
obtaining an analysis sample with an analytical sampling device, the analytical sampling device having an adsorbent material therein onto which the analysis sample is adsorbed, the adsorbent material having a focusing agent adsorbed therein, wherein the focusing agent including a plurality of isotope analogs of the chemical agent with each isotope analog of the plurality being at a concentration that is different from concentrations of other isotope analogs of the plurality;
desorbing the focusing agent and the analysis sample from the analytical sampling device to form a desorbed mixture and transferring the desorbed mixture a chromatographical system;
observing a first signal relating to the focusing agent and a second signal relating to the chemical agent; and
correcting the second signal with the first signal wherein an RSD of the corrected second signal is reduced compared to an RSD resulting from a use of an internal standard or an existing calibration curve.

2. The method of claim 1 , wherein desorbing the focusing agent and the chemical agent from the analytical sampling device further comprises:
adsorbing the desorbed mixture onto a second pre-concentrator operably connected to the chromatographic system; and
performing a second desorption process from the second pre-concentrator prior to transferring the desorbed mixture into the chromatographic system.

3. The method of claim 1 , wherein the focusing agent comprises a semi-volatile compound.

4. The method of claim 3 , wherein the semi-volatile compound is selected from the group consisting of bromopentafluorobenzene, diisopropyl fluoro phosphate, a dialkyl malonate, or a combination thereof.

5. The method of claim 3 , wherein the semi-volatile compound is a dialkyl malonate selected from dimethyl malonate, diethyl malonate, dipropyl malonate, diisopropyl malonate, dibutyl malonate, dipentyl malonate, or a combination thereof.

6. The method of claim 5 , wherein dialkyl malonate comprises diethyl malonate, and optionally comprises an isotopic derivative selected from diethyl malonate-2- 13 C, diethyl malonate-1,2- 13 C, or diethyl malonate-1,2,3- 13 C.

7. The method of claim 1 , wherein the adsorbent material comprises alumina, silica, carbon-containing adsorbents, a zeolite, a porous glass, a clay, a porous polymer based on 2,6-diphenyl-p-phenylene oxide, a hydrophobic copolymer of styrene-divinylbenzene resin, a polyurethane, or a combination thereof.

8. The method of claim 1 , wherein a relative concentration of the isotope analogs of the plurality is 1:2:3.

9. The method of claim 1 , wherein the isotope analogs of the plurality are 13C isotope analogs of diethyl malonate.

Assignees

• Us Gov Air Force
• Us Air Force

Inventors

• Rubenstein H Mitchell

Classifications

• G01N30/8668 Primary

  using retention times · CPC title

• G01N2030/0095

  Separation specially adapted for use outside laboratory, e.g. field sampling, portable equipments · CPC title

• G01N33/0057 Primary

  Warfare agents or explosives · CPC title

• G01N30/8672

  not depending on an individual instrument, e.g. retention time indexes or calibration transfer · CPC title

• G01N30/08

  using an enricher · CPC title