Liquid chromatography/Fourier transform IR spectrometry interface flow cell

• US 4,618,769 A
• Filed: 01/04/1985
• Issued: 10/21/1986
• Est. Priority Date: 01/04/1985
• Status: Expired due to Fees

• Current Assignee: US Government Represented By The United States Department of Veterans Affairs
• Original Assignee: United States Department of Energy
• Inventors: Taylor, Larry T., Johnson, Charles C.
• Primary Examiner(s): Howell, Janice A.
• Application Number:
  US06/689,104
• Time in Patent Office: 655 Days
• Field of Search: 250/338 R, 250/339, 250/341, 356/440, 356/246
• US Class Current: 250/338.1
• CPC Class Codes: G01N 2021/0346 Capillary cells; Microcells
• CPC Class Codes: G01N 21/05 Flow-through cuvettes G01N21/09 takes precedence; handling fluid samples G01N1/10
• 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

A zero dead volume (ZDV) microbore high performance liquid chromatography (μHPLC)/Fourier transform infrared (FTIR) interface flow cell includes an IR transparent crystal having a small diameter bore therein through which a sample liquid is passed. The interface flow cell further includes a metal holder in combination with a pair of inner, compressible seals for directly coupling the thus configured spectrometric flow cell to the outlet of a μHPLC column end fitting to minimize the transfer volume of the effluents exiting the μHPLC column which exhibit excellent flow characteristics due to the essentially unencumbered, open-flow design. The IR beam passes transverse to the sample flow through the circular bore within the IR transparent crystal, which is preferably comprised of potassium bromide (KBr) or calcium fluoride (CaF₂), so as to minimize interference patterns and vignetting encountered in conventional parallel-plate IR cells. The long IR beam pathlength and lensing effect of the circular cross-section of the sample volume in combination with the refractive index differences between the solvent and the transparent crystal serve to focus the IR beam in enhancing sample detection sensitivity by an order of magnitude.

Claims

1. In a Fourier transform infrared spectrometer wherein a sample material is isolated by liquid chromatography and directed through an elongated tube of small inner diameter for irradiation by an infrared beam in obtaining an infrared spectrum of the sample material representing the composition thereof, a sample flow cell comprising:

a generally cylindrical crystal having a longitudinal axis and a generally circular cross-section, wherein said crystal is transparent to infrared radiation and is positioned in line with the infrared beam with its longitudinal axis aligned generally perpendicular to the infrared beam, whereby said infrared beam is incident upon said crystal and is focused generally on the crystal'"'"'s longitudinal axis and is transmitted therethrough so as to exit therefrom; and

a small diameter, linear bore having a circular cross-section positioned within said crystal along the longitudinal axis and extending the length thereof and oriented generally perpendicular to the direction of propagation of the infrared beam therein, said bore coupled to the elongated tube for receiving and directing the sample material in the path of the infrared beam wherein the exiting infrared beam includes the infrared spectrum of the sample material.

2. An infrared spectrometer sample flow cell as in claim 1 further comprising gasket means positioned between a lateral surface of said crystal through which said bore extends and the elongated tube for coupling the elongated tube and said bore in a leak-proof manner.

3. An infrared spectrometer sample flow cell as in claim 2 wherein said gasket means is comprised of a hard plastic.

4. An infrared spectrometer sample flow cell as in claim 1 further including an IR beam source and a spectrometer positioned on respective sides of said crystal for respectively generating and receiving the IR beam.

5. An infrared spectrometer sample flow cell as in claim 4 further including means positioned on the side of said crystal adjacent to said spectrometer for directing the IR beam thereto.

6. An infrared spectrometer sample flow cell as in claim 5 wherein said means for directing the IR beam to said spectrometer includes an opqaue sheet having an aperture positioned adjacent to said spectrometer and through which the IR beam passes to said spectrometer.

7. An infrared spectrometer sample flow cell as in claim 1 wherein said crystal is comprised of KBr.

8. An infrared spectrometer sample flow cell as in claim 1 wherein said crystal is comprised of CaF₂.

9. An infrared spectrometer sample flow cell as in claim 1 further including cell holder means for coupling said crystal to the elongated tube, said cell holder means including coupling means for connecting said bore to the elongated tube in a linear arrangement.

10. An infrared spectrometer sample flow cell as in claim 9 further including first and second gasket means positioned between respective facing surfaces of said crystal and said cell holder means for forming a seal therebetween.

11. An infrared spectrometer sample flow cell as in claim 10 wherein said cell holder means includes first and second apertures in respective facing surfaces thereof through which the sample material enters and exits said crystal and which define respective ends of said bore.

12. An infrared spectrometer sample flow cell as in claim 1 wherein the IR beam and said bore have substantially equal width dimensions.