WO1988001053A1 - Supersonic nozzle for use in an infrared spectrometer - Google Patents

Supersonic nozzle for use in an infrared spectrometer Download PDF

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Publication number
WO1988001053A1
WO1988001053A1 PCT/US1987/001855 US8701855W WO8801053A1 WO 1988001053 A1 WO1988001053 A1 WO 1988001053A1 US 8701855 W US8701855 W US 8701855W WO 8801053 A1 WO8801053 A1 WO 8801053A1
Authority
WO
WIPO (PCT)
Prior art keywords
nozzle
windows
slit
aperture
exit
Prior art date
Application number
PCT/US1987/001855
Other languages
French (fr)
Original Assignee
Whisenhunt, Fred, S.
Gough, Terrance, E.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Whisenhunt, Fred, S., Gough, Terrance, E. filed Critical Whisenhunt, Fred, S.
Publication of WO1988001053A1 publication Critical patent/WO1988001053A1/en

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/85—Investigating moving fluids or granular solids
    • G01N2021/8557—Special shaping of flow, e.g. using a by-pass line, jet flow, curtain flow

Definitions

  • This invention relates to a supersonic nozzle for injecting a gas into an infrared spectrometer and, in particular, to a supersonic nozzle having an aperture that produces a one-dimensional expansion of said gas.
  • a supersonic nozzle for dispersing a gas in an infrared spectrometer having a pumping system for pumping said gas through said spectrometer, has an entrance and exit for said gas. There are means at said entrance and exit for connecting said nozzle into said spectrometer so that the gas to be analyzed will flow through said nozzle from said entrance to said exit using the pumping system of said spectrometer.
  • a narrow passageway extends from said entrance to a wall containing an aperture. Two windows extend from either side of said aperture towards said exit, each window being normal to a plane formed by said aperture and parallel to the other window. Each window has an interior surface that is set back slightly from said aperture.
  • the windows together define a region for one-dimensional expansion of said gas, said windows being of an appropriate material to pass infrared rays.
  • An expansion chamber is located between said windows and said exit, said •5 chamber being substantially larger than said one- dimensional expansion region.
  • the nozzle is a narrow slit having two ends and the windows extend from either end of said slit towards said exit, each window being 0 normal to an imaginary straight line extending between the ends of said slit.
  • Figure 1 is a perspective view of one embodiment of a supersonic nozzle
  • Figure 2 is a sectional side view of part of .the nozzle of Figure 1;
  • Figure 3 is a sectional top view of part of the nozzle of Figure 1;
  • Figure 4 is an end view of an aperture in the form of a narrow slit
  • Figure 5 is an end view of an aperture in the form of a circle;
  • Figure 6 is a partially cut-away side view of a further embodiment of a supersonic nozzle;
  • Figure 7 is a partially cut-away top view of the nozzle of Figure 6;
  • Figure 8 is an enlarged partial top view of a window assembly in the nozzle of Figure 6;
  • Figure 9 is an enlarged view of a tip of the nozzle containing an aperture.
  • a supersonic nozzle 2 for injecting a gas in an infrared spectrometer (not shown), has an entrance 4 and an exit 6.
  • a pumping system (not shown) pumps said gas through said spectrometer.
  • the swagelok fitting 8 has a threaded portion 10 and a base 12.
  • the base 12 is in turn affixed to two windows 14 (only one of which is shown in Figure 1).
  • the windows 14 are parallel to one another and together with a top and bottom 16 enclose a one-dimensional expansion region.
  • the bottom 16 is a mirror image of the top 16. Between the windows 14 and the exit 6 is an expansion chamber 18, said chamber being substantially larger than said one-dimensional expansion region.
  • the swagelok fitting 8 has a narrow passageway 20 centrally located therein. As can best be seen from Figures 4 and 5, a rectangular housing 21 extends from the base 12 to a wall 22 containing an aperture 24.
  • the narrow passageway 20 extends from the threaded portion 10 of the swagelok fitting 8, through the base 12 and rectangular housing 21 to the aperture 24 in the wall 22.
  • Windows 14 extend from either side of said aperture 24 and actually commence between the aperture 24 and the base 12. Each window 14 is parallel to a plane formed by said aperture and parallel to the other window 14.
  • Each window 14 has an interior surface 30 that is set back slightly from said aperture 24.
  • the windows 14 together define a one- dimensional expansion region 32 for expansion of the gas being analyzed after it passes through the aperture 24.
  • the top and bottom 16 combine with the windows 14 to. completely enclose the region 32.
  • the top and bottom 16 each have an interior surface 34, that tapers toward either side of said slit at an angle of approximately 45o relative to the wall 22 to approximate anticipated stream lines of the expanding gas.
  • the tapered portion of the interior surface 34 of said top and bottom 16 on either side of said slit 24 has a semi-circular- cross-section as shown in Figure 2.
  • the windows 14 of Figures 2 and 3 are rectangular in shape and extend to the relatively large expansion chamber 18 (not shown in Figures 2 and 3) between the windows 14 and the exit 6.
  • the aperture 24 in the wall 22 is in the form of a narrow slit.
  • the windows extend from either end of said slit towards said exit, each window being normal to an imaginary straight line extending between the ends of said slit.
  • the slit and nozzle are oriented so that the direction of the spectrometer's radiation beam is parallel to said slit.
  • the aperture 24 is in the form of a circle. Both apertures 24 are centrally located between the windows 14, which are set back slightly from the apertures. The distance of setback shown in Figures 4 and 5 is exaggerated for ease of illustration.
  • the windows 14 can be suspended on either side of said aperture 24.
  • the same reference numerals as those used for the nozzle 2 are used in Figures 6 to 9 for those components that are the same or similar.
  • the nozzle 36 has a tube 38 with a threaded entrance 40.
  • the tube 38 extends into one end 42 of a housing 44.
  • the other end 46 of the housing 44 is an exit similar to the exit 6 of the nozzle 2.
  • the tube 38 extends partially into the housing 44 and terminates at an end 54.
  • a removable tip 55 which is described in more detail below.
  • the tip 55 contains an aperture, which is preferably in the form of a slit or circle similar to the apertures shown in Figures 4 and 5.
  • windows 14 are suspended on either side of the tip 55 and extend towards the exit 46.
  • the windows have a round shape and are preferably made from zinc selenide or any other suitable material that will pass infrared rays.
  • the windows 14 are parallel to one another and normal to an end wall 56 of the tip 55. From either side of the windows 14, support panels 58 are affixed. '
  • the support panels 58 have the shape of a truncated cone and extend from the windows 14 to the outer wall 60 of the housing 44 where they are sealed to said outer wall.
  • the tip 55 is described in more detail in Figure 9.
  • the tip 55 can be slidably inserted into the tube 38.
  • the tip 55 has a T-shaped cross-section with a base 62 and a projection 64.
  • the projection 64 has an end wall 56 which contains an aperture 24.
  • the aperture 24 is connected by a centrally located passageway 66 to an interior 68 of the tube 38.
  • the advantage of using a nozzle having a tip 55 is that various tips can be designed, each having an aperture of a different size and shape. Depending on the particular type of aperture desired by an operator of the mass spectrometer, the appropriate tip can be inserted into the tube 38. When a different tip is desired, it is a relatively simple matter to remove one tip and replace it with another tip.
  • the tube 38 could have an end wall which contained an aperture of a fixed size and shape.
  • Examples of some of the sizes that have actually been used successfully with a nozzle similar to that shown in Figures 6, 7, 8, 9 are as follows: Diameter of circular aperture - 100 ⁇ m; Slit aperture - 40 ⁇ m x 750 ⁇ m; Diameter of end wall containing aperture - .25 mm; Thickness of end wall containing aperture - 200 ⁇ m;
  • FTIR spectroscopy has well known advantages over laser systems: firstly, the spectral coverage available with FTIR is vastly superior; secondly, the ability to record- all transitions in the spectrum at the same time is particularly important for the richer spectra of larger van der Waal's di ers. With the nozzle of the present invention FTIR spectroscopy compares favourably with laser systems. It can be extremely important to produce clusters in a nozzle expansion of a gas. However, up to the time of the present invention, clusters were not able to be produced using supersonic nozzles, in amounts sufficient for detection by FTIR spectroscopy.

Abstract

Supersonic nozzle (2) for injecting a gas into an infrared spectrometer, said nozzle having an aperture (24) that produces a one-dimensional expansion of said gas. The nozzle has an entrance (4) and exit (6) and between the aperture (24) and the exit (6) is a region for one-dimensional expansion of the gas. The region has two windows (14) that extend on either side of said aperture (24) towards said exit, said windows having an interior surface (30) that is set back slightly from said aperture (24). The windows (14) are made of an appropriate material such as zinc selenide to pass infrared rays and allow the gas to expand in one dimension only.

Description

SUPERSONIC NOZZLE FOR USE IN AN INFRARED SPECTROMETER
BACKGROUND OF THE INVENTION FIELD OF THE INVENTION
This invention relates to a supersonic nozzle for injecting a gas into an infrared spectrometer and, in particular, to a supersonic nozzle having an aperture that produces a one-dimensional expansion of said gas.
DESCRIPTION OF THE PRIOR ART It is known to use laser technology to record spectra of gases in jets. In fact, because of the success of laser technology in this area, the use of conventional spectrometers has been almost totally neglected. While nozzles have been used during experimentation in FTIR spectroscopy, the results previously obtainable are much inferior to the resolution and sensitivity of laser techniques. .Further, previous nozzles could not be used to produce clusters. * SUMMARY OF THE INVENTION
In accordance with the present invention, a supersonic nozzle, for dispersing a gas in an infrared spectrometer having a pumping system for pumping said gas through said spectrometer, has an entrance and exit for said gas. There are means at said entrance and exit for connecting said nozzle into said spectrometer so that the gas to be analyzed will flow through said nozzle from said entrance to said exit using the pumping system of said spectrometer. A narrow passageway extends from said entrance to a wall containing an aperture. Two windows extend from either side of said aperture towards said exit, each window being normal to a plane formed by said aperture and parallel to the other window. Each window has an interior surface that is set back slightly from said aperture. The windows together define a region for one-dimensional expansion of said gas, said windows being of an appropriate material to pass infrared rays. There are means in said spectrometer to pass infrared rays through said panels. An expansion chamber is located between said windows and said exit, said •5 chamber being substantially larger than said one- dimensional expansion region.
Preferably, the nozzle is a narrow slit having two ends and the windows extend from either end of said slit towards said exit, each window being 0 normal to an imaginary straight line extending between the ends of said slit.
BRIEF DESCRIPTION OF THE DRAWINGS In drawings which illustrate a preferred embodiment of the invention: Figure 1 is a perspective view of one embodiment of a supersonic nozzle;
Figure 2 is a sectional side view of part of .the nozzle of Figure 1;
Figure 3 is a sectional top view of part of the nozzle of Figure 1;
Figure 4 is an end view of an aperture in the form of a narrow slit;
Figure 5 is an end view of an aperture in the form of a circle; Figure 6 is a partially cut-away side view of a further embodiment of a supersonic nozzle;
Figure 7 is a partially cut-away top view of the nozzle of Figure 6;
Figure 8 is an enlarged partial top view of a window assembly in the nozzle of Figure 6; and
Figure 9 is an enlarged view of a tip of the nozzle containing an aperture.
DESCRIPTION OF A PREFERRED EMBODIMENT Referring to the drawings in greater detail, in Figure 1, a supersonic nozzle 2 for injecting a gas in an infrared spectrometer (not shown), has an entrance 4 and an exit 6. A pumping system (not shown) pumps said gas through said spectrometer. There are means at said entrance 4, being a swagelok fitting 8 for connecting said nozzle 2 into said spectrometer. The swagelok fitting 8 has a threaded portion 10 and a base 12. The base 12 is in turn affixed to two windows 14 (only one of which is shown in Figure 1). The windows 14 are parallel to one another and together with a top and bottom 16 enclose a one-dimensional expansion region. The bottom 16 is a mirror image of the top 16. Between the windows 14 and the exit 6 is an expansion chamber 18, said chamber being substantially larger than said one-dimensional expansion region. The swagelok fitting 8 has a narrow passageway 20 centrally located therein. As can best be seen from Figures 4 and 5, a rectangular housing 21 extends from the base 12 to a wall 22 containing an aperture 24. The narrow passageway 20 extends from the threaded portion 10 of the swagelok fitting 8, through the base 12 and rectangular housing 21 to the aperture 24 in the wall 22. Windows 14 extend from either side of said aperture 24 and actually commence between the aperture 24 and the base 12. Each window 14 is parallel to a plane formed by said aperture and parallel to the other window 14. Each window 14 has an interior surface 30 that is set back slightly from said aperture 24. The windows 14 together define a one- dimensional expansion region 32 for expansion of the gas being analyzed after it passes through the aperture 24.
The top and bottom 16 combine with the windows 14 to. completely enclose the region 32. The top and bottom 16 each have an interior surface 34, that tapers toward either side of said slit at an angle of approximately 45o relative to the wall 22 to approximate anticipated stream lines of the expanding gas. Preferably, the tapered portion of the interior surface 34 of said top and bottom 16 on either side of said slit 24 has a semi-circular- cross-section as shown in Figure 2. The windows 14 of Figures 2 and 3 are rectangular in shape and extend to the relatively large expansion chamber 18 (not shown in Figures 2 and 3) between the windows 14 and the exit 6.
As shown in Figure 4, the aperture 24 in the wall 22 is in the form of a narrow slit. The windows extend from either end of said slit towards said exit, each window being normal to an imaginary straight line extending between the ends of said slit. The slit and nozzle are oriented so that the direction of the spectrometer's radiation beam is parallel to said slit. In Figure 5, the aperture 24 is in the form of a circle. Both apertures 24 are centrally located between the windows 14, which are set back slightly from the apertures. The distance of setback shown in Figures 4 and 5 is exaggerated for ease of illustration.
In a further embodiment of the invention, as shown in Figures 6, 7, 8 and 9, the windows 14 can be suspended on either side of said aperture 24. The same reference numerals as those used for the nozzle 2 are used in Figures 6 to 9 for those components that are the same or similar. The nozzle 36 has a tube 38 with a threaded entrance 40. The tube 38 extends into one end 42 of a housing 44. The other end 46 of the housing 44 is an exit similar to the exit 6 of the nozzle 2.
The tube 38 extends partially into the housing 44 and terminates at an end 54. In the end 54 is slidably inserted a removable tip 55 which is described in more detail below. While it is not shown in Figures 5 to 9, the tip 55 contains an aperture, which is preferably in the form of a slit or circle similar to the apertures shown in Figures 4 and 5. As can best be seen from Figure 8, windows 14 are suspended on either side of the tip 55 and extend towards the exit 46. The windows have a round shape and are preferably made from zinc selenide or any other suitable material that will pass infrared rays. The windows 14 are parallel to one another and normal to an end wall 56 of the tip 55. From either side of the windows 14, support panels 58 are affixed.' The support panels 58 have the shape of a truncated cone and extend from the windows 14 to the outer wall 60 of the housing 44 where they are sealed to said outer wall.
The tip 55 is described in more detail in Figure 9. The tip 55 can be slidably inserted into the tube 38. The tip 55 has a T-shaped cross-section with a base 62 and a projection 64. The projection 64 has an end wall 56 which contains an aperture 24. The aperture 24 is connected by a centrally located passageway 66 to an interior 68 of the tube 38. The advantage of using a nozzle having a tip 55 is that various tips can be designed, each having an aperture of a different size and shape. Depending on the particular type of aperture desired by an operator of the mass spectrometer, the appropriate tip can be inserted into the tube 38. When a different tip is desired, it is a relatively simple matter to remove one tip and replace it with another tip. As an alternative, the tube 38 could have an end wall which contained an aperture of a fixed size and shape. Examples of some of the sizes that have actually been used successfully with a nozzle similar to that shown in Figures 6, 7, 8, 9 are as follows: Diameter of circular aperture - 100 μm; Slit aperture - 40 μm x 750 μm; Diameter of end wall containing aperture - .25 mm; Thickness of end wall containing aperture - 200 μm;
Distance between zinc selenide windows - 2 mm; Outside diameter of brass tube, being narrow portion of housing - 25 mm; Clear opening provided by windows - 5 mm diameter;
Using the narrow slit nozzle of the present invention, cold gas and clusters were observed up to approximately 2 cm from the nozzle. Therefore, it can be concluded that the nozzle is able to produce an extended "zone of silence". Clusters are formed of matter intermediate between infinite solid and monomeric gas. FTIR spectroscopy has well known advantages over laser systems: firstly, the spectral coverage available with FTIR is vastly superior; secondly, the ability to record- all transitions in the spectrum at the same time is particularly important for the richer spectra of larger van der Waal's di ers. With the nozzle of the present invention FTIR spectroscopy compares favourably with laser systems. It can be extremely important to produce clusters in a nozzle expansion of a gas. However, up to the time of the present invention, clusters were not able to be produced using supersonic nozzles, in amounts sufficient for detection by FTIR spectroscopy.

Claims

I CLAIM:
1. A supersonic nozzle (2) for injecting a gas in an infrared spectrometer using a pumping system for pumping said gas through said spectrometer, said nozzle comprising:
(a) An entrance (4) and an exit (6) for said gas with means at said entrance and at said exit for connecting said nozzle into said spectrometer so that gas to be analyzed will flow through said nozzle from said entrance to said exit using the pumping system;
(b) A narrow passageway (20) extending from said entrance to a wall (22) containing an aperture (24);
(c) Two windows (14) extending from either side of said aperture towards said exit, each window being normal to a plane formed by said aperture and parallel to the other window, each window having an interior surface (30) that is set back slightly from said aperture, said windows together defining a region (32) for one-dimensional expansion of said gas said windows being of an appropriate material to pass infrared rays;
(d) Means in said spectrometer to pass infrared rays through said windows; and
(e) An expansion chamber (18) located between said windows and said exit, said chamber being substantially larger than said one- dimensional space.
2. A nozzle as claimed in Claim 1 wherein the aperture (24) is a circular opening.
3. A nozzle as claimed in Claim 1 wherein the aperture (24) is a narrow slit having two ends and the windows extend from either end of said slit towards said exit, each window being normal to an imaginary straight line extending between the ends of said slit.
4. A nozzle as claimed in Claim 3 wherein the direction of the spectrometer's radiation beam is parallel to said slit.
5. A nozzle as claimed in Claim 4 wherein the windows form two sides of a region (32) for one- dimensional expansion of said gas, said region also having a closed top and bottom, said top and bottom being mirror images of one another, said slit (24) having two sides, said top (16) and bottom (16) each having an interior surface (34) that tapers toward either side of said slit at an angle of approximately 45o relative to said wall to approximate anticipated stream lines of the expand'ing gas.
6. A nozzle as claimed in Claim 5 wherein the tapered portion of the interior surface (34) of said top (16) and bottom (16) on either side of said slit (24) has a semi-circular cross-section.
7. A nozzle as claimed in any one of Claims 1, 3 or 5 wherein the windows (14) are rectangular in shape and extend to a relatively large expansion chamber (18) between the windows and the exit (6) .
8. A nozzle as claimed in any one of Claims 1, 2 or 3 wherein the windows (14) are made from zinc selenide.
9. A nozzle as claimed in Claim 4 wherein the windows (14) are suspended on either side of said slit (24).
10. A nozzle as claimed in Claim 9 wherein the windows (14) are circular in shape.
11. A nozzle as claimed in Claim 1 wherein the expansion chamber (18) extends from said slit (24) to said exit (6) .
12. A nozzle as claimed in Claim 6 wherein the windows (14) are approximately 2 mm apart from one another.
13. A nozzle as claimed in any one of Claims 4, 5 or 6 wherein the slit (24) has a width of approximately 40 μm.
14. A nozzle as claimed in Claim 6 wherein a zone of silence can be observed between said windows (14) approximately 2 cm from said slit.
15. A nozzle as claimed in any one of Claim 1, 2 or 3 wherein the windows (14) are made from potassium bromide.
PCT/US1987/001855 1986-07-31 1987-07-29 Supersonic nozzle for use in an infrared spectrometer WO1988001053A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CA000515050A CA1268348A (en) 1986-07-31 1986-07-31 Supersonic nozzle for use in an infrared spectrometer
CA515,050 1986-07-31

Publications (1)

Publication Number Publication Date
WO1988001053A1 true WO1988001053A1 (en) 1988-02-11

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WO (1) WO1988001053A1 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4861999A (en) * 1987-08-20 1989-08-29 Gough Terrance E Supersonic nozzle for use in an infrared spectrometer

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2731877A (en) * 1956-01-24 clamann
US3901820A (en) * 1974-04-12 1975-08-26 Modern Controls Inc Pressure modulated gas measuring method and apparatus
US4440013A (en) * 1982-03-03 1984-04-03 International Business Machines Corp. Gas chromatograph, Fourier transform, infrared spectroscopy system

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2731877A (en) * 1956-01-24 clamann
US3901820A (en) * 1974-04-12 1975-08-26 Modern Controls Inc Pressure modulated gas measuring method and apparatus
US4440013A (en) * 1982-03-03 1984-04-03 International Business Machines Corp. Gas chromatograph, Fourier transform, infrared spectroscopy system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4861999A (en) * 1987-08-20 1989-08-29 Gough Terrance E Supersonic nozzle for use in an infrared spectrometer

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Publication number Publication date
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