Abstract:
A transverse optical transmission probe having a probe body and a probe tip. The probe use optical fibers to both transmit radiation from an instrument to the probe tip and to return the sample affected radiation to the instrument. The fibers are in parallel and contained in the probe body. The probe tip includes two optical elements that protrude into the sample and are configured to define a sample gap so that incident radiation pass through the sample in a direction transverse to the axis to the probe and eventually reaches the receiving fiber. Each of the optical elements may be formed from a single piece of material or may be a composite formed by adhering two or more pieces of material together. One or more lensed surfaces may be used to cause the end of the transmitting fiber to be imaged on the end of the receiving fiber.

Description:
CROSS REFERENCE TO RELATED APPLICATIONS 
       [0001]    This application claims the benefit of U.S. Provisional Patent Application Ser. No. 62/089,525, filed Dec. 9, 2014. 
     
    
     BACKGROUND OF THE INVENTION 
       [0002]    1. Field of the Invention 
         [0003]    The invention relates generally to probes for spectroscopic measuring devices and, more particularly, to a transverse optical transmission probe. 
         [0004]    2. Description of the Related Art 
         [0005]    A variety of sampling devices are currently available for use in optical spectroscopy (primarily near-infrared and UV-visible). These generally use optical fibers to couple to an appropriate instrument. They fall into the following categories and suffer from the noted problems:
       1 Single pass transmission probes. An example is the Axiom Analytical FPT-850. These probes provide high performance but involve numerous manufacturing steps and hence do not meet the low cost requirement of our invention.   2. Double pass transflectance probes. These probes are somewhat less expensive to produce than the single pass probes but have significant performance limitations. In particular, the sample gap needs to be one half of the desired pathlength thereby restricting sample flow.   3. Transmission cells. Commercial transmission cells are generally too costly for our current requirements. One could envision a less expensive cell. But it would be difficult to provide the serviceability required for the envisioned application with a transmission cell form factor.       
 
         [0009]    There remains a need, therefore, for a transverse optical transmission probe that is compatible with water based samples, is capable of being produced at very low cost in substantial volume, has a relatively small sample gap but not so small that it causes sample retention in the sample gap and restricts sample flow; and is suitable for easy service and replacement in the field. 
       BRIEF SUMMARY OF THE INVENTION 
       [0010]    The purpose of the invention is to provide a sample interfacing device for use with optical spectroscopy in the near-infrared, visible, and UV spectral regions, with the following objectives: 
         [0011]    A relatively small sample gap, i.e. less than 10 mm and preferably around 1 mm; 
         [0012]    Optimized flow characteristics so as to minimize sample retention in the sample gap; 
         [0013]    Compatible with water based samples; 
         [0014]    Capable of being produced at very low cost in substantial volume; and 
         [0015]    Suitable for easy service and replacement in the field. 
         [0016]    After considering the requirements for the envisioned application, we determined that a probe form factor was preferred in order to meet the requirement for serviceability. A probe can be inserted through the wall of the sample vessel through an appropriate seal and easily removed as a unit for service or replacement. 
         [0017]    In its most general form, our invention includes the following:
       1. The use of optical fibers to both transmit radiation from an instrument to the probe tip and to return the sample affected radiation to the instrument. Within the probe, these fibers would be parallel and contained in a single (preferably cylindrical) structure.   2. The use of, at most, two integrated optical elements protruding from the tip of the probe into the sample and configured so as to cause the incident radiation to pass through the sample in a direction transverse to the axis to the probe and to eventually reach the receiving fiber. Each of the optical elements may be formed from a single piece of material or may be a composite formed by adhering two or more pieces of material together.   3. The use of one or more lensed surfaces to cause the end of the transmitting fiber to be imaged on the end of the receiving fiber.       
 
         [0021]    In accordance with the present invention, structures are disclosed which overcome the problems in the related art and achieve these objectives. 
         [0022]    In a first aspect, the invention resides in a transverse optical transmission probe for analyzing a sample comprising: a probe body; first and second optical fibers in the probe body, each optical fiber having a distal end; a probe tip connected to the probe body; first and second optical elements in the probe tip that protrude into the sample and define a sample gap therebetween through which the sample passes; and wherein the first optical fiber is configured for transmitting radiation from an instrument to the probe tip and the second optical fiber returning sample affected radiation from the probe tip to the instrument. Said first optical element is configured for receiving the radiation transmitted by the first optical fiber and transmitting the radiation across the sample gap and through the sample to form the sample-affected radiation within the sample gap, said second optical element is configured for receiving the sample-affected radiation from the sample gap and transmitting the sample-affected radiation to the second optical fiber; and at least one lensed surface causes the distal end of the first optical fiber to be imaged onto the distal end of the second optical fiber. 
         [0023]    The invention, now having been briefly summarized, may be better visualized by turning to the following drawings wherein like elements are referenced by like numerals. 
     
    
     
       DESCRIPTION OF THE DRAWINGS 
         [0024]    The presently preferred embodiments of the just summarized invention can be best understood in connection with a detailed description of the following figures. 
           [0025]      FIG. 1  shows a first preferred probe  100  comprised of a probe body  110  and a probe tip  120  having a sample gap  121 ; 
           [0026]      FIG. 2  shows a process line or vessel having a wall  50  with an aperture  51 ; 
           [0027]      FIG. 3  shows the probe  100  mounted in the wall  50  of the process line or vessel of  FIG. 2  with a hex nut  115  used to compress an O-ring  114  against the wall  50 ; 
           [0028]      FIG. 4  shows a distal portion of the first preferred probe  100  of  FIG. 1 , focusing in on the first preferred probe tip  110 ; 
           [0029]      FIG. 5  is similar to  FIG. 4  but includes some typical dimensions and the refractive index values used for components of the first preferred probe tip  120 ; 
           [0030]      FIG. 6  shows how a flat plate is temporarily clamped against the end of the probe ferrules  7 ,  8  while the optical fibers  6 ,  7  are epoxied in place in order to assure that the ends of the optical fibers  6 ,  7  are in the same plane; 
           [0031]      FIG. 7  shows a first version of a positioning mask  10  having precise rectangular cutouts  11 ,  12  that closely conform to the cross-sectional dimensions of the optical prisms  1 , 3 ; 
           [0032]      FIG. 8  shows a second version of a positioning mask  10 ′ having rectangular cutouts  11 ′,  12 ′ that provide some additional space relative to the cross-sectional dimensions of the optical prisms  1 , 3 . 
           [0033]      FIG. 9  shows a simplified portion of a second alternative probe  200  having an an alternative probe tip  220  where elements  15  and  16  incorporate both the lensed surfaces and the diagonal reflecting surfaces and elements  17  and  18  are simple rectangular blocks of optical material; 
           [0034]      FIG. 10  shows a distal portion of a third alternative probe  300  having an alternative probe tip  320 ; and 
           [0035]      FIG. 11  shows a distal portion of a fourth alternative probe  400  having an alternative probe tip  420 . 
       
    
    
     DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS 
       [0036]    The primary impetus for development of our invention has been a particular set of applications utilizing near-infrared vibrational spectroscopy. However, it can also be applied to other fields of optical spectroscopy. 
       (1) First Preferred Embodiment 
       [0037]      FIG. 1  shows a first preferred probe  100  that is comprised of a probe body  110  and a probe tip  120  having a sample gap  121 . The preferred probe body  110  has a shoulder  111  with an annular groove on its underside, and threads  113  along its length. The preferred probe tip  120  has a sample gap  121 . 
         [0038]      FIG. 2  shows a process line or vessel having a wall  50  with an aperture  51  for receiving the probe  100 . 
         [0039]      FIG. 3  provides additional details showing how the probe  100  could be mounted through the wall  50  of the sample vessel. As shown in  FIG. 3 , the preferred probe  100  is secured to the sample vessel&#39;s wall  50  with an O-ring  114  (e.g. a size 020 O-ring) compressed against the vessel&#39;s wall  50  between the probe body&#39;s shoulder  111  and a hex nut  115 . This is just one example of many possible mechanisms for mounting the probe  100  with its probe tip  120  and related sample gap  121  exposed to the fluid to be analyzed. 
         [0040]      FIG. 4  is a close-up view of a distal portion of the first preferred probe  100  of  FIG. 1 , focusing on the structure and operation of first preferred probe tip  120 . In this particular embodiment, the inventors have chosen optical components  1 ,  2 ,  3 ,  4  so as to minimize cost and complexity. Since the anticipated samples will be water based and not strongly caustic, it is advantageously possible to adhere the various components together by using optical quality epoxy, thereby eliminating the need for any air gaps in the optical system. Note that the presence of air gaps would necessitate that these be sealed and hence would require a more complex (and expensive) mechanical structure. 
         [0041]      FIG. 4  shows the optical components of the first preferred embodiment, namely items  1 ,  2 ,  3 , and  4 . We anticipate that, in large scale production, each of the pairs ( 1  and  2 ) and ( 3  and  4 ) could be molded as a single component. For prototyping and early stage production, each pair was comprised of a rectangular cross section prism ( 1  and  3 ) and a plano-convex lens ( 2  and  4 ). These shapes are desirable because they can easily be produced by typical optical polishing vendors. For reasons that will become apparent below, these optical components will be fabricated from materials having relatively high refractive indices. Examples might be sapphire and a high index glass such as SF11. In some embodiments, the index of refraction is greater than about 1.65, and in other embodiments the index of refraction is greater than about 1.5. In a presently preferred embodiment, the index of refraction is greater than 1.7 and less than about 1.8. In a presently preferred embodiment, the index of refraction is greater is about 1.75. 
         [0042]    Optical radiation is introduced into the probe tip by means of one of a pair of optical fibers  5  and  6  which are contained in ferrules  7  and  8 . For sake of this discussion, we will let  5  be the input fiber. A typical fiber will have a numeric aperture of 0.22. For this value, the light emerging from a distal end of the fiber will diverge with a half angle of about 12.7 degrees in air. Once the light enters the high index optical medium of item  1 , the divergence angle will be reduced substantially (7.22 degrees for n=1.75), as shown in the Figure. The diverging light is reflected by a mirrored coating on the diagonal surface of prism  1  and is then directed to the convex surface of lens  2  where it is formed into a nominally collimated beam. After traversing the sample gap, the light is collected by the second lens  4 , reflected by the second diagonal surface, and focused on a distal end of the receiving fiber,  6 . As we have seen, the use of high refractive index optical materials minimizes the divergence angle thereby minimizes the required diameter of the lenses. It is also dictated by the fact that the lensed surfaces are in contact with the sample, which will typically have a refractive index around n=1.33. 
         [0043]      FIG. 5  is similar to  FIG. 4  but includes some typical dimensions and the refractive index values used for our illustration. For the initial prototypes, we plan to use sapphire for the prisms in order to maximize the transmission for the longer wavelength end of the near-IR region. Sapphire has a refractive index of refraction in the near-IR of about n=1.75. We also plan to use commercially available SF11 glass lenses which have a refractive index in the near-IR of about n=1.785. We have selected an available lens design that allows us to conveniently image the end of the input fiber on the end of the receiving fiber. Each fiber is assumed to have a core diameter of 0.3 mm. In other embodiments, the fibers may have a different core diameter, e.g. 0.2 mm. 
         [0044]    In  FIG. 5 , the minimum sample gap  121  has been chosen to be 1 mm. Since the curved surfaces of the two lenses  2 ,  4  are in contract with the sample, the actual sample gap will vary across the surface. However, the data nonlinearity introduce by this variation can easily be dealt with by performing separate analyses for regions of high and low water absorption. The chosen dimensions provide for free liquid flow around the lenses  2 ,  4  so as to discourage sample retention and enhance cleaning. For example, if the gap between the cylindrical surfaces of the lenses and the positioning mask were 1 mm or less—rather than the 2 mm shown in the figures—there would be a tendency for viscous samples to collect in this region. 
       (2) Practical Mechanical Considerations 
       [0045]    So far we have described an idealized optical design for our invention. However, there are additional practical considerations. In particular, the optical elements  1 , 2  and  3 , 4  need to be aligned so as to accurately image the end of the input fiber  5  on that of the receiving fiber  6 . As presently preferred, the mounting hardware (and assembly jigs) are designed to passively align the optics as closely as possible. However, we presently believe that it will necessary to allow for some additional final active alignment while the optical elements are being epoxied together. The mechanical discussion below includes a couple of ways that this can be accomplished. 
         [0046]    The first mechanical requirement for assembly of the probe  100  is to assure that the ends of the optical fibers  5 ,  6  are in the same plane.  FIG. 6  illustrates a presently preferred method of how this can be accomplished. The fibers  5 ,  6  are terminated in cylindrical ferrules  7 ,  8 . These will be free to slide through corresponding and parallel bores  127 ,  128  in the probe body  110 . To mount the fibers  5 ,  6  in the probe body  110 , we will clamp a flat plate  9  against the end of the probe body  110 . The fiber containing ferrules  7 ,  8  are slid into the bores  127 ,  128  of the probe body  110  until they contact the plate  9  and then epoxied in place. The plate  9  is then removed. 
         [0047]    The next step is to assemble the probe tip  120  by mounting and properly aligning the optical elements  1 ,  2  and  3 ,  4  on the end of the probe body  110 . We presently foresee at least two possible approaches to doing this. Both of these would employ a positioning mask  10  on the end of the probe.  FIGS. 7 and 8  show two presently preferred positioning masks  10  and  10 ′. 
         [0048]    In  FIG. 7 , the first positioning mask  10  has precise rectangular cutouts  11 ,  12  matched as closely as possible to the cross-sectional dimensions of the optical prisms  1 ,  3 . The prisms  1 , 3  are simply inserted through these cutouts  11 ,  12  and adhered to a distal end of the probe body  110 , in contact with the ends of the two fibers  5 ,  6 , using an optically transparent epoxy. The other two holes,  13  and  14 , are used to accommodate pins  115  that are positioned in the probe body  110  (see  FIG. 1 ) for accurately locating the mask  10  in a desired registration with the distal end of the probe body  110 . 
         [0049]    The positioning mask  10  provides passive mechanical alignment, but it may not achieve the desired optical alignment and some form of active alignment may be needed. One way to accomplish this is to leave at least one of the lenses  2 ,  4  to be mounted and actively positioned after the mounting of the prisms  1  and  3 . We can then connect the fibers  5 ,  6  to an instrument and monitor the signal level as the lens(es) is/are positioned. The lens(es)  2 ,  4  would then be adhered in place by using UV curing epoxy. 
         [0050]      FIG. 8  shows a second version of a positioning mask  10 ′ that is suitable for dynamic alignment. The second positioning mask  10 ′ features rectangular cutouts  11 ′,  12 ′ that provide additional space relative to the cross-sectional dimensions of the optical prisms  1 ,  3 . The additional space is used to move the optical prisms  1 ,  3  before adhering them in their final position with the UV curing epoxy. 
         [0051]    In  FIG. 8 , the illustrated cutouts  11 ,  12  are slightly elongated in transverse axes, but other arrangements may be possible. Using the second version of the positioning mask  10 ′, we would mount the lenses  2 ,  4  on the prisms  1 ,  3  before mounting the prisms  1 ,  3  to the probe body  110 . The prisms  1 ,  3  would then be positioned so as to maximize the signal. To facilitate this dynamic mounting, the cutouts  13 ′,  14 ′ are elongated in transverse directions so that one prism  1  could slide in the X direction and the other prism  2  in the Y direction. 
       (3) Other Possible Embodiments 
       [0052]      FIG. 9  shows a second alternative probe  200 , in greatly simplified presentation, that is based on a second alternative probe tip  220  have a simple modification relative to the first preferred probe tip  120  (other elements have been omitted for simplicity of presentation). The probe tip  220  provides sample gap  321 . In this design, elements  15  and  16  incorporate both the lensed surfaces and the diagonal reflecting surfaces. Elements  17  and  18  are simple rectangular blocks of optical material. The function of this design would be the same as that of  FIG. 1 . However, it would be more expensive to fabricate in small quantities since it would not use a commercially available lens. 
         [0053]      FIG. 10  shows a third alternative probe  300  that has lenses  19 ,  22  mounted below the prisms  1 ,  3 , within the probe body  110 , to eliminate the need for lensed surfaces in contact with the sample. Here, lens  19  collects the light diverging from the input fiber  5  and forms it into a collimated beam (dashed lines). Prisms  1  and  3  are the same as in  FIGS. 1 to 5 . Elements  20  and  21 , however, have parallel optical faces and cross sections which can be either circular or rectangular. Lens  22  focuses the collimated light onto the receiving fiber  6 . 
         [0054]    This third design  300  has the advantage of eliminating the pathlength variation across the sample gap  321 . However, it has the disadvantage of requiring a more complicated mechanical structure. In addition, it introduces the possibility of sample leakage into the necessary air gaps associated with the lenses  21 ,  22  located within the probe body  310 . 
         [0055]      FIG. 11  illustrates a fourth alternative  400  having a probe tip  410  with a sample gap  421  according to a further alternative design. In this design, the probe tip  410  comprises a sample contacting optical element,  23 , that is fabricated as a single component having a circular cross section in the region of contact with the probe body  410 . In principle, this design could use an O-ring  414  or similar seal to interface an annular shoulder of the probe tip  420  to the probe body  410  with a suitable compression collar  430 , thereby eliminating the need for epoxy in contact with the sample. This design would be quite difficult to fabricate using conventional polishing methods but might be amenable to molding with appropriate tooling. 
         [0056]    Many alterations and modifications may be made by those having ordinary skill in the art without departing from the spirit and scope of the invention. Therefore, it must be understood that the illustrated embodiments have been set forth only for the purposes of example and that it should not be taken as limiting the invention as defined by the following claims. The claims are thus to be understood to include the specifically illustrated and described embodiments, structures based on equivalents concepts, and substitutions that incorporate the invention.