Photometric flow apparatus for small sample volumes and method of making same

• US 5,917,606 A
• Filed: 09/06/1996
• Issued: 06/29/1999
• Est. Priority Date: 09/06/1995
• Status: Expired due to Term

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Hewlett-Packard Company (HP Inc.)
• Inventors: Kaltenbach, Patrick
• Primary Examiner(s): Kim, Robert
• Assistant Examiner(s): MERLINO, AMANDA H
• Application Number:
  US08/709,017
• Time in Patent Office: 1,026 Days
• Field of Search: 356/410, 356/440, 356/246
• US Class Current: 356/440
• CPC Class Codes: G01N 2021/0346 Capillary cells; Microcells
• CPC Class Codes: G01N 2030/746 detecting along the line of flow, e.g. axial
• CPC Class Codes: G01N 21/05 Flow-through cuvettes G01N21/09 takes precedence; handling fluid samples G01N1/10
• CPC Class Codes: G01N 2201/0642 Light traps; baffles
• CPC Class Codes: G01N 27/44721 by optical means
• 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 photometric apparatus (100) for small sample volumes comprises a cell body (102), a light input means (104) arranged adjacent to a first surface of the cell body (102), a light source (105) emitting light of predetermined wavelength or wavelength range through the light input means (104), a light output means (106) arranged adjacent to a second surface of the cell body (102) opposite to the first surface, a light detector (107) arranged adjacent to the light out put means (104), and a flow channel (108) formed in the cell body (102), wherein surfaces of the walls of the channel (108) have a roughness smaller than the predetermined wavelength.

Claims

1. Photometric apparatus for small sample volumes comprising:

a cell body;

a light input means arranged adjacent a first surface of the cell body;

a light source for emitting light of predetermined wavelength or wavelength range through the light input means;

a light output means arranged adjacent a second surface of the cell body opposite to the first surface;

a light detector arranged adjacent the light output means; and

a flow channel formed in the cell body;

wherein surfaces of the walls of the channel have a roughness smaller than the predetermined wavelength or all wavelengths of the wavelength range of the source.

2. Apparatus according to claim 1, wherein the light input means comprises an optical input waveguide;

and wherein the light output means comprises an optical output waveguide.

3. Apparatus according to claim 1, wherein the light input means comprises a first transparent window;

and wherein the light output means comprises a second transparent window.

4. Apparatus according to claim 1, wherein the cell body is formed of non-transparent material.

5. Apparatus according to claim 3, wherein the flow channel comprises:

a first portion formed adjacent to the first transparent window and extending substantially parallel to the first surface of the cell body;

a second portion extending from the first surface to the second surface of the cell body; and

a third portion formed adjacent to the second transparent window and extending substantially parallel to the second surface of the cell body.

6. Apparatus according to claim 1, comprising an inlet capillary and an outlet capillary in fluid connection with the flow channel.

7. Apparatus according to claim 1, wherein at least one of an inlet capillary and an output capillary has an expanded inner diameter at the capillary/flow channel junction.

8. Apparatus according to claim 6, comprising capillary support structure attached to the cell body for supporting the inlet and the outlet capillary.

9. Apparatus according to claim 8, wherein the inlet capillary and the outlet capillary are secured to the capillary support structure by glue or plastic fittings.

10. Apparatus according to claim 1, wherein the cell body comprises a first and a second portion, a first and a second flow channel forming part arranged between the first portion and the second portion of the cell body, wherein the cell body is formed by directly fusing together the first portion of the cell body, the first and second flow channels respectively forming parts, and the second portion.

11. Apparatus according to claim 4, wherein the flow channel includes junction portions connecting the flow channel portions under an angle of 45°

.

12. Apparatus according to claim 1, wherein the flow channel has a rectangular cross-section of less than 150×

150 μ

m and a channel length of less than 1.5 mm.

13. Apparatus according to claim 1, wherein the flow channel has a rectangular cross-section of less than 150×

150 μ

m, a channel length of less than 1.5 mm and a total volume of less than 10 nl.

14. Apparatus according to claim 3, wherein the transparent windows are made of fused silica.

15. The photometric apparatus of claim 1 wherein the channel includes separate individual parts that are polished before being assembled to achieve the stated roughness.

16. A method of making a flow cell for use in liquid chromatography, the cell in use being responsive to optical energy having a predetermined wavelength or wavelength range, comprising determining the wavelength or wavelength range, forming in the cell an elongated flow channel for the liquid, the flow channel being arranged so in use of the cell the optical energy propagates and the liquid flows along the flow channel longitudinal axis, and machining and polishing the channel wall so the wall surface roughness has a value less than the determined wavelength or all wavelengths of the wavelength range of the source.

17. The method of claim 16, further including forming the channel from separate individual parts that are polished to achieve the stated channel wall surface roughness, the individual parts being polished to achieve the stated roughness prior to being assembled to form the channel.

18. Apparatus for use in spectroscopy analysis of small samples in liquid solution comprising

a source of optical radiation having a predetermined wavelength or range of wavelengths, radiation from the source being directed in a predetermined direction,

an optical detector for radiation from the source,

a photometric flow cell including first and second members forming a cell body, the cell body including a flow channel for the liquid, the flow channel including a first component extending in the predetermined direction, the first component of the flow channel being defined by a slit between opposed edges of first and second plates bonded to the cell body and opposed faces of the first and second members, the edges of the plates and the opposed faces defining the first component of the flow channel having a roughness smaller than the predetermined wavelength or all wavelengths of the wavelength range of the source,

first and second windows transparent to optical radiation from the source bonded to the cell body so that optical radiation from the source propagates through the first window, thence through the slit, thence through the second window and thence to the optical detector,

the channel including second and third components connected to opposite sides of the slit for respectively supplying the liquid solution to the slit and removing the liquid solution from the slit.

19. Apparatus according to claim 18, wherein the second channel component includes a first passage between the first plate and the first window and the third channel component includes a second passage between the second plate and the second window.

20. Apparatus according to claim 18, wherein the slit has only planar faces.

21. Apparatus according to claim 18, wherein the slit has a cross-sectional area no greater than 0.25 square millimeters.

22. Apparatus according to claim 18, wherein the cell body and the plates are opaque to optical radiation of the source.

23. A method of making a photometric flow cell for use in spectroscopy analysis of small samples in liquid solution, the spectroscopy analysis being performed with an optical radiation source having a predetermined wavelength or range of wavelengths, the cell including first and second members having planar faces and a slit forming a component of a flow channel for the liquid sample, the method comprising polishing first and second edges of first and second plates so the edges have a roughness less than the predetermined wavelength or all wavelengths of the wavelength range of the source, then bonding faces of the plates to planar faces of the first and second members to form the slit of the flow channel for the liquid solution, then bonding windows transparent to the optical radiation to opposite faces of the members substantially at right angles to the flow direction of the liquid solution through the slit.

24. A method according to claim 23, wherein the plates are bonded to the members so there is (a) a first set back of another edge of the first plate from a face of the first window and a second set back of a further edge of the second plate from a face of the second window, and (b) the another and further edges are substantially transverse to the flow direction of the liquid solution through the slit, and (c) a first passage in the flow channel is formed between the another edge and the first window and a second passage in the flow channel is formed between the further edge and the second window.