Emission spectroscopy based on plasma sources is a well accepted approach to elemental analysis. It is desired that an electrical plasma suitable as an emission source for atomic spectroscopy of a sample should satisfy a number of criteria. The plasma should produce desolvation, volatilization, atomization and excitation of the sample. However the introduction of the sample to the plasma should not destabilize the plasma or cause it to extinguish.
One known and accepted plasma source for emission spectroscopy is a radio frequency (RF) inductively coupled plasma (ICP) source, typically operating at either 27 MHz or 40 MHz. In general, with an RF ICP source the plasma is confined to a cylindrical region, with a somewhat cooler central core. Such a plasma is referred to as a “toroidal” plasma. To perform spectroscopy of a sample with an RF ICP source, a sample in the form of an aerosol laden gas stream may be directed coaxially into this central core of the toroidal plasma.
Although such plasma sources are known and work well, they generally require the use of argon as the plasma gas. However, argon can be somewhat expensive and is not obtainable easily, or at all, in some countries.
Accordingly, there has been ongoing interest for many years in a plasma source supported by microwave power (for example at 2.45 GHz where inexpensive magnetrons are available) which can use nitrogen, which is cheaper and more widely available than argon, as the plasma gas.
However, emission spectroscopy systems based on microwave plasma sources have generally shown significantly worse detection limits than systems which employ an ICP source, and have often been far more demanding in their sample introduction requirements.
For optimum analytical performance of the emission spectroscopy system, it is thought that the plasma should be confined to a toroidal region, mimicking the plasma generated by an RF ICP source.
It turns out to be much more difficult to produce such a toroidal plasma using microwave excitation than it is in for RF ICP source. With an RF ICP source, a current-carrying coil, wound along the long axis of a plasma torch, is used to power the plasma. The coil produces a magnetic field which is approximately axially oriented with respect to the long axis of the plasma torch, and this, in turn, induces circulating currents in the plasma, and these currents are symmetrical about the long axis of the plasma torch. Thus, the electromagnetic field distribution in the vicinity of the plasma torch has inherent circular symmetry about the long axis of the plasma torch. So it is comparatively easy to produce a toroidal plasma with an RF ICP source.
However, the waveguides used to deliver power to microwave plasmas do not have this type of circular symmetry, and so it is much more difficult to generate toroidal microwave plasmas.
There is therefore a desire to provide an improved microwave plasma source which can offer performance which approaches that of RF ICP, together with characteristics such as small size, simplicity and relatively low operating costs.
The various embodiments are best understood from the following detailed description when read with the accompanying drawing figures. Wherever applicable and practical, like reference numerals refer to like elements.
In the following detailed description, for purposes of explanation and not limitation, illustrative embodiments disclosing specific details are set forth in order to provide a thorough understanding of embodiments according to the present teachings. However, it will be apparent to one having had the benefit of the present disclosure that other embodiments according to the present teachings that depart from the specific details disclosed herein remain within the scope of the appended claims. Moreover, descriptions of well-known devices and methods may be omitted so as not to obscure the description of the example embodiments. Such methods and devices are within the scope of the present teachings.
Generally, it is understood that as used in the specification and appended claims, the terms “a”, “an” and “the” include both singular and plural referents, unless the context clearly dictates otherwise. Thus, for example, “a device” includes one device and plural devices.
The present teachings relate generally to an apparatus including a waveguide in combination with a plasma torch to generate and sustain a plasma useful in spectrochemical analysis. The present inventors have conceived and produced novel iris structures for a waveguide which may cause the electric field in the waveguide to experience a phase shift or change in direction across the iris structure from a first side of the iris structure to a second side of the iris structure opposite the first side. Here, an iris is defined as a region of discontinuity inside the waveguide which presents an impedance mismatch (a perturbation) that blocks or alters the shape of the pattern of an electromagnetic field in the waveguide. In some embodiments, the iris can be produced by a reduction in the height and width of the interior of the waveguide, as is discussed in greater detail below.
In particular, the present inventors have discovered that by employing certain iris structure configurations, the electric field may be caused to experience a phase shift of 180 degrees across the iris structure, producing a reversal in direction of the electric field from the first side of the iris structure to the second side of the iris structure such that the electric field at the second side of the iris structure is in an opposite direction from the electric field at first side of the iris structure. By employing these configurations, a toroidal plasma may be generated. A more detailed explanation will be provided in connection with example embodiments illustrated in the attached drawings.
To facilitate a better understanding of the description below,
Apparatus 100 comprises an electromagnetic waveguide (“waveguide”) 101 which is configured to support a desired propagation mode (“mode”) at a frequency suitable for generating and sustaining a plasma, and an iris 106 where a plasma torch (not shown in
Waveguide 101 is configured to support a desired mode of propagation (e.g., TE10) at a microwave frequency. Although the embodiment of waveguide 101 illustrated in
Iris 106 is provided in waveguide 101 by an iris structure 105 which defines an iris hole 108 with a first iris slot 110 disposed at or along a first side of iris hole 108 and a second iris slot 112 disposed at or along a second side of iris hole 108, wherein the first and second sides are separated and spaced apart from each other in the y-direction. In general, first and second iris slots 110 and 112 may have the same size and shape as each other, or the sizes and/or shapes may be different from each other.
In operation, an electromagnetic wave may propagate from first end 102 of waveguide 101, pass through first iris slot 110, iris hole 108, and second iris slot 112, and reach second end 104 of waveguide 101.
In the embodiment illustrated in
In some embodiments, the center of the iris 106 (e.g. at principal axis 116) is disposed at a distance (represented as a first length L1 in
In some embodiments, iris structure 105 which defines iris 106 may be a metal section having a thickness dimension along the length (y-direction) of waveguide 101, with a through-hole extending in the x-direction through the width of the metal section to define iris hole 108 which is configured to accommodate therein a plasma torch (see
As will be described in greater detail below, in some embodiments iris hole 108 may include disposed therein a dielectric material, for example a cylindrical dielectric tube or sleeve 111 as illustrated in the example embodiment apparatus 100 in
As noted above, iris hole 108 may be configured to accommodate therein a plasma torch. A plasma torch is a device with a conduit or channel for delivering a plasma gas, which, upon contacting the electromagnetic waves, produces a plasma. The plasma torch may also comprise a conduit or channel for delivering a sample in the form of an aerosol or gas to a location where plasma forms. Plasma torches are known in the art.
In operation, when plasma torch 400 is inserted into iris hole 108, a carrier gas with an entrained sample to be spectroscopically analyzed normally flows through innermost tube 402, an intermediate gas flow is provided in intermediate cylinder 403, and a plasma-sustaining and torch-cooling gas flow is provided in outermost tube 404. In some embodiments, the plasma-sustaining and torch-cooling gas may be nitrogen. For example, the plasma-sustaining and torch-cooling gas may be nitrogen, and arrangements are provided for producing a flow of this gas conducive to form a stable plasma having a substantially hollow core, and to prevent plasma torch 400 from becoming overheated. For example, in some embodiments the plasma-sustaining gas may be injected radially off-axis so that the flow spirals. This gas flow sustains the plasma and the analytical sample carried in the inner gas flow is heated by radiation and conduction from the plasma. In some embodiments, for the purpose of initially igniting the plasma, the plasma-sustaining and torch-cooling gas flow may temporarily and briefly be changed: for example, from nitrogen to argon.
A more detailed description of an example embodiment of a plasma torch is described in detail in commonly owned U.S. Pat. No. 7,030,979 to Hammer. The disclosure of U.S. Pat. No. 7,030,979 is specifically incorporated herein by reference. It will be understood that other configurations of a plasma torch, and other suitable means of injecting the sample to be analyzed and the plasma gas into iris 106, are contemplated.
As indicated above, a selected mode is supported in waveguide 101 when not perturbed. However, the iris 106 presents a perturbation that alters the wavelength and shape of the mode in the waveguide 101. By virtue of the structure of waveguide 101 and iris 106, a plasma may be generated and sustained in a desired shape.
In some embodiments, waveguide 101 may be configured to support a TE10 propagation mode having a frequency in the microwave portion of the electromagnetic spectrum. For example, in some embodiments the selected mode may have a characteristic frequency of approximately 2.45 GHz. Notably, however, the embodiments described herein are not limited to operation at 2.45 GHz, and in general not limited to operation in the microwave spectrum. In particular, because the operational frequency range which is selected dictates the wavelength of the selected mode(s) of operation, and the operational wavelengths are primarily limited by the geometric sizes of plasma torch 400 and waveguide 101, the operational frequency is also limited by the geometric size of plasma torch 400 and waveguide 101. Illustratively, the present teachings can be readily implemented to include operational frequencies both higher and lower that 2.45 GHz. Furthermore, the desired mode is not limited to the illustrative TE10 mode, and the waveguide 101 (or first and/or second portions 117, 118 depicted in
The present inventors have discovered that by disposing a dielectric material inside of iris hole 108, and outside of plasma torch, in particular between plasma torch 400 and an inner wall or surface in the iris structure which defines iris hole 108, the electric field may be caused to experience a phase shift or change in direction from first iris slot 110 to second iris slot 112. In particular, the present inventors have discovered that in some embodiments the electric field may be caused to experience a phase shift of 180 degrees, that is a reversal in direction from first iris slot 110 to second iris slot 112, such that the electric field at second iris slot 112 is in an opposite direction from the electric field at first iris slot 110.
Although
In should be understood that
In some embodiments, the dielectric material (e.g., cylindrical dielectric sleeve 111) which is disposed in iris hole 108 may be disposed on an inner wall or surface of the iris structure—in particular an inner wall which defines iris hole 108. In some embodiments, the dielectric material may be disposed directly on an inner wall of the iris structure which defines iris hole 108, while in other embodiments there may be a space or gap between the dielectric material and the inner wall of the structure which defines iris hole 108. In general, the dielectric material has a dielectric constant which is greater than that or air. In some embodiments, the dielectric material may have a dielectric constant of at least 2, and more preferably a dielectric constant of at least 7. In some embodiments, the dielectric material may comprise ceramic or alumina. In other embodiments, the dielectric material may comprise one or more of the following materials: silicon nitride, aluminum nitride, sapphire, silicon. The thickness of the dielectric material may be selected depending on the dielectric constant of the material. In general, a thinner material may be employed when the dielectric constant is greater, and a thicker material may be selected when the dielectric constant is less. In some embodiments, the ratio of the thickness of cylindrical dielectric sleeve 111 to the radius of iris hole 108 may be from 10% to 30%.
In some embodiments, the total phase shift in iris hole 108 may be around φ0=90°˜180° to provide a sufficient amount of variation for the electric field. For iris hole 108 having a given size, the phase shift may be increased by the presence of the dielectric material within iris hole 108. With the addition of dielectric material, we find that βglg+β0l0=φ0, where βg and β0 are the propagation constants inside the dielectric material and in air, respectively (βg=2π/λg and β0=2π/λ0 where λg and λ0 are wavelengths inside the dielectric material and in air, respectively). Accordingly, we find that 2π×(lg/λg+l0/λ0)=φ0. This equation indicates that the shorter the wavelength in a given material, the smaller the distance which is required to produce a given phase shift. So to achieve a desired phase shift through a dielectric material such as ceramic or alumina, for example, the path length is less than that for air. Of course as a practical matter, in general iris hole 108 will not be filled entirely with a dielectric material, as space is required for the plasma torch. The equation above also indicates that if a material with a higher dielectric constant is employed (which means lower λg at a given frequency) then the distance required for the phase shift can be reduced, meaning that a shorter length of dielectric material can be used and the diameter required for iris hole 108 can be reduced.
Iris structure 705 defines iris hole 108 with a first iris slot 710 disposed along a first side of iris hole 108 and a second iris slot 712 (see
The present inventors have discovered that by making one or both of first and second iris slots 710 and 712 to have a greater height at the ends thereof than in the middle, the electric field can be caused to experience a phase shift or change in direction from first iris slot 710 to second iris slot 712. In particular, the present inventors have discovered that the electric field may be caused to experience a phase shift of 180 degrees, that is a reversal in direction from first iris slot 710 to second iris slot 712 such that the electric field at second iris slot 712 is in an opposite direction from the electric field at first iris slot 710.
Toward this end, in iris 706 the height (i.e., the size in the z-direction) of at least one of first and second iris slots 710 and 712 is greater at the ends of the iris slot than in the middle of the iris slot. In some embodiments, the height (i.e., the size in the z-direction) of both of first and second iris slots 710 and 712 is greater at the ends of the iris slot than in the middle of the iris slot.
In the particular examples illustrated in
The shape of first and second iris slot(s) 710 and/or 712 may cause the electric field to have opposite directions at opposite sides of iris 706, which generates an axial magnetic field inside iris hole 108. In some embodiments, the electric field distribution inside the plasma generated by plasma torch when disposed in it is hole 108 of iris 706 is circumferential, which is similar to that of an RF ICP source and the first embodiment described above with respect to
The electric field distribution illustrated in
In the particular example embodiment illustrated in
Many variations of the example embodiments described above are possible. Furthermore, features of the example embodiments may be combined to produce other embodiments. In some embodiments a dielectric material may be provided inside the iris hole of an iris structure, and one or both of the iris slots of the iris structure may have a shape where the height of the iris slot is greater at the ends thereof than in the middle. In such embodiments, an axial magnetic field and an electric field having opposite directions on opposite sides of the iris may be more readily achieved for producing a desired plasma shape (e.g., toroidal). For example, by employing a bowtie-shaped iris slot in a device which includes a dielectric material in the iris hole, it may be possible to employ a thinner dielectric material and/or a dielectric material which has a lower dielectric constant. Similarly, when a dielectric material (e.g., a cylindrical dielectric sleeve) is provided in a device having a bowtie-shaped iris slot, it may be possible to reduce the difference in the height of the iris slot between the ends of the iris slot and the middle of the iris slot.
Embodiments of a waveguide-based apparatus for exciting and sustaining a plasma as described above may be employed in various systems and for various applications, including but not limited to an atomic emission spectrometer (AES) for performing atomic emission spectroscopy or a mass spectrometer for performing mass spectrometry. In some embodiments, a spectrograph (e.g., an Echelle spectrograph) may be employed to separate atomized radiation emitted by the plasma into spectral emission wavelengths that are imaged onto a camera to produce spectral data, and a processor or computer may be employed to process and display and/or store the spectral data captured by the camera
In addition to the embodiments described elsewhere in this disclosure, exemplary embodiments of the present invention include, without being limited to, the following:
A number of embodiments of the invention have been described. Nevertheless, one of ordinary skill in the art appreciates that many variations and modifications are possible without departing from the spirit and scope of the present invention and which remain within the scope of the appended claims. The invention therefore is not to be restricted in any way other than by the scope of the claims.
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20140265850 A1 | Sep 2014 | US |