IP Library Granted Patent US 11,300,503
Granted Patent B2
US 11,300,503 · App. 16/113,856 · Granted Apr 12, 2022

Carbon ladder calibration

Inventors: Eddie Dean Wyatt (Havertown, PA); Martin L. Spartz (Ellington, CT)
Assignee: MLS Acq, Inc.
G01N21/3504G01N30/02G01N30/8668G01N30/8672G01N30/7206G01N33/0047G01N2021/3595G01N2030/025G01N2030/042
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Quick Facts
Patent No.
US 11,300,503
App. No.
16/113,856
Granted
Apr 12, 2022
Kind
B2
Abstract

A GC sample carbon ladder is generated with the help of one or more of the following techniques: correction of solvent effects; fit analysis of the spectrum obtained for a target member of the carbon ladder and a reference spectrum; fit analysis of a sample carbon ladder in comparison with reference spectral features; constraints for proper order of elution; and/or inclusion of all members in a selected carbon ladder set.

Claims (22)

1. A process for generating a carbon ladder calibration chromatogram, the process comprising:

generating an initial chromatogram of a sample eluting through a gas chromatography (GC) column, wherein the sample comprises carbon ladder compounds;

comparing a spectrum of one or more observed peaks in the initial chromatogram with reference spectra of the compounds;

assigning the one or more observed peaks by determining a best match between the spectrum of the one or more observed peak and the reference spectra to obtain a candidate calibration chromatograph; and

shifting the candidate calibration chromatogram by one or more carbon numbers to determine an overall best match, thereby generating the carbon ladder calibration chromatogram; and

wherein solvent effects are reduced by:

obtaining a regression of the reference spectrum for a solvent against a sample spectrum in a selected spectral region, to determine a solvent concentration; and

subtracting from the sample spectrum the product obtained by multiplying a solvent spectrum by a regression scaling factor.

2. The calibration process of claim 1 , wherein the observed peaks are detected by optical spectroscopy.

3. The calibration process of claim 1 , wherein the observed peaks are detected by Fourier transform infrared (FTIR) spectrometry.

4. The calibration process of claim 1 , wherein the initial chromatogram is corrected by removing solvent effects.

5. The process of claim 1 , wherein the selected spectral region is a region devoid of features characterizing the carbon ladder compounds.

6. The process of claim 1 , wherein the process is conducted under a no gap constraint.

7. The process of claim 1 , wherein the process is conducted by following a normal elution order of the carbon ladder compounds.

8. The process of claim 1 , wherein the process allows for a gap in the carbon ladder.

9. The process of claim 1 , wherein the candidate calibration chromatograph is shifted by one or more carbon numbers forward and/or backwards across the peaks, moving the entire ladder one peak at a time.

10. The process of claim 1 , wherein the carbon ladder compounds include hydrocarbons.

11. The process of claim 1 , wherein retention indices of the carbon ladder compounds are Kovats indices.

12. The process of claim 1 , wherein retention indices of the carbon ladder compounds used are Lee indices.

13. The process of claim 1 , wherein the best match or the overall best match is expressed by a best fit, least error, least average error or least total error.

14. The process of claim 1 , wherein the sample eluted from the GC column is temporally resolved into components that are directed to a sample cell and detected by Fourier transform infrared (FTIR) spectrometry.

15. The process of claim 14 , wherein the sample cell is a multiple path cell.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 6, 2018
From: WYATT, EDDIE DEAN; SPARTZ, MARTIN L.
To: MLS ACQ, INC. D/B/A MAX ANALYTICAL TECHNOLOGIES
Reel/Frame 047026/0605 →
Continuity (3)
Provisional Application 62551936 · Aug 30, 2017
Provisional Application 62551933 · Aug 30, 2017
Related Publication 20190064131A1 · Feb 28, 2019