Retention time chromatograph employing an IR absorption spectrographic detector

• US 4,044,257 A
• Filed: 02/20/1975
• Issued: 08/23/1977
• Est. Priority Date: 02/20/1975
• Status: Expired due to Term

• Current Assignee: Barry Block, Harry E. Aine
• Original Assignee: DIAX Corporation
• Inventors: Kreuzer, Lloyd B.
• Primary Examiner(s): Smith, Alfred S.
• Assistant Examiner(s): Anderson, B. C.
• Application Number:
  US05/551,379
• Time in Patent Office: 915 Days
• Field of Search: 250/343, 250/344, 73/23.1, 55/197, 356/97
• US Class Current: 250/344
• CPC Class Codes: G01J 3/427 Dual wavelengths spectrometry
• CPC Class Codes: G01N 30/74 Optical detectors measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J

Abstract

Sample material of retention time peaks of a chromatograph are exposed to infrared radiation at first and second wavelengths and the absorption of the infrared energy by the sample peak is measured. The measured infrared absorption at the first and second wavelengths is correlated with the retention time of the sample peak as an identification of the sample material. In addition, overlapping retention time peaks are resolved by detecting the change in the ratio of the infrared absorption at the first and second wavelengths as a function of retention time for a given peak.

Claims

1. In a method of identifying the sample material of a retention peak of a retention time chromatograph, the steps of:

determining the retention time of a retention peak of a sample constituent in the effluent of a retention time chromatograph;

detecting the absorption of infrared energy by the sample material of the retention peak from a laser beam at first and second infrared wavelengths of the laser beam;

controlling the pressure of the sample constituent material to a predetermined value in a region wherein the absorption of the infrared energy from the laser beam is detected; and

correlating the retention time of the sample peak with the detected absorption of the sample peak at said first and second infrared wavelengths to identify the sample constituent of the retention peak and deriving the ratio of the infrared absorption of the sample material of said retention peak at said first and second wavelengths; and

wherein the step of correlating the retention time of the sample peak with the absorption of the sample at said first and second wavelengths comprises correlating said ratio with the retention time to identify the sample constituent.

2. The method of claim 1 including the step of, detecting time dependent changes in the correlation of the detected absorption of the sample peak at said first and second wavelengths as a function of retention time within a given peak to resolve overlapping retention peaks.

3. The method of claim 1 including the step of detecting changes in said ratio as a function of retention time within a given peak to resolve overlapping retention peaks.

4. The method for resolving constituents of a fluid sample including the steps of:

deriving a pair of sample absorption signals which are a function of the absorption of infrared energy by constituents of the sample material from a laser beam of infrared radiation at first and second wavelengths λ

₁ and λ

₂, respectively;

controlling the pressure of the fluid sample to a predetermined value in the region where the absorption signals are derived; and

deriving an output proportional to the ratio of the two sample absorption signals at λ

₁ and λ

₂ said output being characteristic of the constituents in the fluid sample under analysis.

5. The method of claim 4 including the step of displaying at least one of the absorption signal outputs at λ

₁ and λ

₂.

6. The method of claim 4 including the step of deriving the ratio of the sample absorption signals as a function of time to detect time dependent changes in said ratio, such changes being indicative of changes in constituents of the sample under analysis.

7. The method of claim 6 wherein the fluid sample to be analyzed is the effluent stream of a retention time chromatograph and including the step of, correlating the derived ratio as a function of time with retention peaks of the retention time chromatograph for resolving overlapping chromatograph signal peaks.

8. Apparatus for identifying sample constituents of a retention peak of a retention time chromatograph including:

means for determining the retention time of retention peak of a sample constituent in the effluent of a retention time chromatograph;

means for detecting the infrared absorption of the sample material of the retention peak at first and second infrared wavelengths of coherent radiation;

means for controlling the pressure of the sample material to a predetermined value in the infrared detection region where the absorption is detected; and

means for correlating the retention time of the sample peak with the detected absorption of the sample peak at said first and second infrared wavelengths to identify the sample constituent and means for deriving the ratio of the absorption of the sample material of said retention peak at said first and second wavelengths; and

wherein said means for correlating the retention time of the sample peak with the absorption of the sample at said first and second wavelengths comprises means for correlating said ratio with the retention time to identify the sample constituent

9. The apparatus of claim 8 including, means for detecting time dependent changes in the correlation of the detected absorption of the sample peak at said first and second infrared wavelengths as a function of retention time within a given retention time peak to resolve overlapping retention peaks.

10. The apparatus of claim 8 including means for detecting changes in said ratio as a function of retention time within a given peak to resolve overlappig retention peaks.

11. In an apparatus for detecting constituents of a fluid sample employing the principle of absorption of infrared energy by the constituents in the fluid sample from an incident beam of infrared radiation:

means for deriving a pair of sample absorption signals which are a function of the absorption of infrared energy by constituents of the sample from an infrared laser beam of energy at first and second wavelengths λ

₁ and λ

₂, respectively;

means for controlling the pressure of the sample to a predetermined value in the region where the absorption of infrared energy by the sample is obtained; and

means for deriving an output proportional to the ratio of the two sample absorption signals at λ

₁ and λ

₂ said output being characteristic of the constituents in the fluid sample under analysis.

12. The apparatus of claim 11 including means for displaying said ratio signal.

13. The apparatus of claim 11 including means for deriving said output proportional to the ratio of the sample absorption signals as a function of time to detect time dependent changes in said ratio which are indicative of changes in the constituents of the sample under analysis.

14. The apparatus of claim 13 including retention time chromatograph means having an effluent stream to be analyzed;

detector means for detecting the sample constituents as a function of retention time; and

wherein said means for deriving the pair of sample absorption signals derives said signals from the effluent stream of the retention time chromatograph.