DETAILED ACTION
The amendment filed on 08/10/2026 has been entered and fully considered. Claims 1-20 are pending, of which claim 1, 11 and 13 are amended.
Response to Amendment
In response to amendment, the examiner modifies rejection over the prior art established in the previous Office action.
Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Claim Rejections - 35 USC § 103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claim(s) 1-7, 9-11 and 13-20 is/are rejected under 35 U.S.C. 103 as being unpatentable over Koichumanova et al. (Catalysis Today, 2017) (Koichumanova) in view of Ebbesen et al. (Journal of Catalysis, 2007) (Ebbesen) and Specac (Golden Gate Single Reflection Diamond ATR System, 2016).
Regarding claim 1, Koichumanova teaches “A device for in-situ time-dependent attenuated total reflectance (ATR) infrared spectroscopy for monitoring reactions between solid or liquid specimens … configured to be attached to an infrared spectrometer” (p. 187, “The goal of the current paper is to present a detailed description of the procedures used for studying materials and reactions under high-temperature and high-pressure conditions. Description includes details on design and methods enabling not only operation of the cell as a reactor under these conditions, but also acquisition of IR spectroscopic data on both dissolved and adsorbed species.”; p. 187, “The ATR-IR cell was installed in the chamber of an FTIR spectrometer (Bruker, Tensor 27) with a mercury-cadmium-telluride detector (MCT D316/6-L).”). Thus, Koichumanova's ATR-IR cell is a physical reactor cell installed in an FTIR spectrometer and used to acquire infrared spectroscopic information from a specimen while reactions are performed in the cell.
Koichumanova does not expressly teach that the flowing medium is “gaseous.” Ebbesen teaches the missing gas-phase ATR-IR operation (p. 68, “After assembling the ATR-IR cell and reducing the catalyst layer (see Section 2), dry gas-phase CO was introduced into the cell. Fig. 2 shows the ATR-IR spectra obtained during CO flow over Pt/Al2O3.”; Fig. 2, p. 68, “ATR-IR spectra as a function of time (time interval: 1.5 min) showing the region of CO adsorption on Pt/Al2O3 while dry CO was flown (1% CO/Ar).”). Ebbesen therefore expressly teaches introducing a gaseous flowing medium into an ATR-IR cell, flowing the gas over the solid Pt/Al2O3 specimen, and obtaining time-dependent ATR-IR spectra during that gas flow.
It would have been obvious to one of ordinary skill in the art before the effective filing date to modify the ATR-IR flow cell of Koichumanova to operate with a gaseous flowing medium as taught by Ebbesen in order to extend the ATR-IR cell to gas-phase reaction studies and permit comparison of the behavior of a specimen in gas and aqueous environments. Ebbesen expressly teaches the benefit of such operation (p. 72, “This study convincingly shows the benefit of ATR-IR spectroscopy for comparing properties of adsorbed molecules on supported noble metal catalysts in gas phase and aqueous phase, because the same catalyst can be used for both types of experiments.”). Thus, the modification would provide the concrete improvement of permitting the same ATR-IR technique to investigate and compare specimen behavior under both gaseous and aqueous reaction conditions.
“an enclosure configured to cover a solid or liquid specimen placed on an ATR plate of an infrared spectrometer” (Koichumanova, p. 187, “The cell consists of a stainless steel block with a cylindrical channel for IRE (Fig. 1c, 7), inlet (8) and outlet (10) perpendicular to the main channel … The IRE (ZnSe rod, length of 83 mm, diameter of 6.4 mm, conical angle of 45°) coated with a sample (6) according to home-developed coating method … was placed coaxially inside the channel and held in the proper place using Kalrez Spectrum O-rings …”). The stainless-steel block and its cylindrical channel correspond to the claimed enclosure because the sample-bearing ATR internal reflection element is positioned coaxially within that channel. The enclosure therefore surrounds and covers the specimen positioned at the ATR element during spectroscopic measurement. Koichumanova further teaches that this ATR-IR cell is installed in the chamber of the FTIR spectrometer.
Specac further confirms the conventional placement of a removable specimen directly on an ATR crystal of an ATR top plate (p. 35, “When using the Golden Gate™ Single Reflection ATR accessory the sample is placed onto the crystal area (23) of the top plate.”), and teaches that the ATR accessory itself is mounted in an infrared spectrometer (p. 4, “A complete Golden Gate™ ATR accessory system consists of an ATR crystal top plate assembly fixed over an optical beam condensing unit. This complete accessory is mounted into an infrared spectrometer using a Benchmark™ baseplate.”). Thus, in the modified arrangement, the removable specimen is positioned on the ATR crystal/top plate and is covered by the flow-cell enclosure for measurement.
“a specimen entrance door configured to permit entry and removal of the specimen for placement on the ATR plate” is not expressly taught by Koichumanova or Ebbesen. Specac, however, teaches a hinged, openable and closable clamp bridge that provides access to the ATR crystal for placement and removal of a specimen. Specac teaches (pp. 38–39, “Undo the bridge quick lock T-knob (25) and lift the clamp bridge (19) up past the stay up catch (26).”; “When a background spectrum has been collected, a sample can be placed into position on the ATR crystal to collect a sample spectrum.”). For a flat solid specimen, Specac further teaches (pp. 41–42, “Gently lower the bridge (19) past the stay up catch (26) and lock it closed using the quick lock T-knob (25)”; and, for removal, “Unlock the bridge (19) by pushing down and turning the quick lock T-knob (25) 90° anticlockwise and open the bridge (19) up past the stay up catch (26).” followed by “Remove the flat solid sample carefully away from the ATR crystal.”).
The clamp bridge (19) corresponds to the claimed specimen entrance door because it is a hinged, lockable access member that is opened to expose the ATR crystal so that a removable specimen can be placed at the crystal, closed after placement of the specimen, and reopened to permit removal of the specimen.
It would have been obvious to one of ordinary skill in the art to modify the ATR-IR flow-cell arrangement of Koichumanova and Ebbesen to incorporate Specac's openable clamp bridge and removable-specimen mounting arrangement in order to permit a solid specimen to be readily placed on and removed from the ATR crystal while providing controlled mechanical contact for ATR measurement. Specac expressly teaches the technical benefit of this arrangement (p. 4, “most of the Golden Gate™ ATR top plate options available have a special bridge and clamping mechanism that provides for excellent and reproducible contact between a solid sample and the single reflection ATR crystal. The different top plate options that have a bridge and clamping mechanism can utilise a choice of different compression anvil types to provide the best possible contact and sample containment over the ATR crystal for an extremely diverse range of solid sample forms.”). Thus, the modification would provide removable-specimen access while improving the reproducibility and quality of specimen-to-ATR-crystal contact.
“a gas flow inlet configured to provide a supply of the gaseous flowing medium to the enclosure and to contact the specimen” (Koichumanova, p. 187, “The cell consists of a stainless steel block with a cylindrical channel for IRE (Fig. 1c, 7), inlet (8) and outlet (10) perpendicular to the main channel”; “The inlet and outlet of the reactor have Swagelok fittings, which allow connection with 1/16 inch SS tubing.”). Koichumanova therefore provides a physical inlet opening into the same channel containing the sample-bearing IRE. As modified according to Ebbesen, that inlet supplies the gaseous flowing medium because Ebbesen expressly teaches that “dry gas-phase CO was introduced into the cell” and that ATR-IR spectra were obtained “during CO flow over Pt/Al2O3.” The combined structure therefore directs gas through the inlet into the enclosure and over the specimen positioned at the ATR crystal.
“an anvil configured to press the specimen firmly against an ATR crystal of the ATR plate to make tight contact for spectroscopic measurement” is taught by Specac. Specac teaches (p. 35, “The contact between a solid sample and crystal is improved using the clamp bridge (19) and an appropriate compression head anvil (18).”). Specac further teaches the actual operation of that structure for a flat solid specimen (pp. 41–42, “Take the flat solid sample and place it very carefully for the surface to be measured to be in contact with ATR crystal such that it covers the entire surface of the diamond ATR crystal (23).”; “Begin turning the torque screw knob (22) clockwise to lower the anvil (18) towards the sample surface. Continue rotation until the central Torx screw (24) stops rotating, but the outer black knob continues to turn. At this point the maximum load achievable from the torque limiter screws (22) own torque mechanism will be applied to the flat solid sample forcing it against the ATR crystal.”).
The compression anvil (18), torque screw knob (22), and clamp bridge (19) collectively provide the claimed pressing structure: rotation of the torque screw lowers the anvil toward the removable solid specimen and applies a load that expressly forces the specimen against the ATR crystal, thereby establishing the tight specimen-to-crystal contact used for ATR spectroscopic measurement. Specac expressly states that this contact is “improved” by the compression anvil and that its bridge-and-clamping arrangement provides “excellent and reproducible contact” between the solid specimen and ATR crystal.
Accordingly, it would have been obvious to one of ordinary skill in the art to modify the ATR-IR flow-cell system of Koichumanova, as modified by Ebbesen for gaseous-flow operation, to incorporate Specac's openable clamp bridge and compression anvil so that discrete solid specimens could be inserted and removed and pressed into excellent and reproducible contact with the ATR crystal for spectroscopic measurement.
Regarding claim 2, Koichumanova teaches
“The cell consists of a stainless steel block with a cylindrical channel for IRE … inlet (8) and outlet (10) perpendicular to the main channel …” (page 187, par 1).
This expressly identifies an outlet (10) in the same enclosed ATR cell that contains the sample-coated IRE. Because the inlet and outlet are both connected to the same cylindrical channel holding the IRE and sample, the structure necessarily exhausts the flowing medium after that medium has traversed the enclosure and contacted the specimen.
Ebbesen shows gas is flowed through the ATR cell:
“dry gas-phase CO was introduced into the cell … during CO flow over Pt/Al2O3.” (page 68, par 3).
The combined system therefore uses Koichumanova’s outlet structure to exhaust the gas-phase medium after contact with the specimen.
Regarding claim 3, Koichumanova teaches an ATR-IR cell installed in an FTIR spectrometer and expressly discusses ATR crystal configurations:
“The ATR-IR cell was installed in the chamber of an FTIR spectrometer (Bruker, Tensor 27) …” (page 187, par 3).
“A number of commercial and home-built ATR-IR cell designs are available such as flow cell with trapezoidal Internal Reflection Element (IRE), circular flow cell with cylindrical IRE …” (page 186, par 1).
“Because the IR light reflects internally in the order of 10 times in a typical multiple reflection ATR crystal …” (page 186, par 0).
These quotes teach an ATR accessory/cell used with an infrared spectrometer and expressly teach a multiple reflection ATR crystal. The reference also identifies alternative IRE geometries, including trapezoidal and cylindrical IREs. The concrete interaction is that the ATR cell is mounted in the FTIR spectrometer, and the IR beam is focused onto the IRE inside the cell to obtain ATR spectra from the specimen on the IRE.
What is not expressly shown
The exact phrase “single-bounce type” is not expressly present in the excerpts presently available, although Koichumanova does teach different IRE designs and expressly teaches multiple reflection ATR crystal. On the current record, the multiple-bounce portion is well supported; the single-bounce alternative is not expressly shown by the cited quotes.
Claim 4-5, Neither Koichumanova nor Ebbesen, on the current record, teaches this claimed numerical internal volume. Koichumanova discusses channel geometry and flow behavior, but no quoted disclosure here teaches an enclosure volume less than 5 cubic micrometers or between 5 cubic millimeters and 5 cubic micrometers. However, it would have been obvious to one of ordinary skill I the art to optimize the internal volume of the enclosure, by routine experimentation.
Regarding claim 6, Koichumanova teaches “The cell consists of a stainless steel block …” (page 187, par 1)
A stainless steel block is a concrete enclosure material and is a heat-conducting material. The quote identifies the specific physical structure that forms the enclosure and provides the claimed material characteristic.
Regarding claim 7, Koichumanova teaches
“A commercial ATR-Tunnel cell with a heating possibility (temperatures up to 300 ◦C and pressures up to 80 bar) … The cell consists of a stainless steel block …” (page 187, par 1).
“The liquid flow was preheated in a coil-shaped preheater (1/16 inch tubing wrapped around an aluminium cylinder with a heating cartridge) … The flow leaving the cell was cooled in a counter-flow heat exchanger with water as the cooling agent.” (page 187, par 3).
These quotes teach exactly the claimed type of enclosure material and operating capability. The enclosure is a stainless steel block, and the system is used with heating hardware to high temperatures and with cooling hardware. The references therefore disclose materials of the claimed type, including stainless steel and aluminum-associated heating/cooling hardware.
Regarding claim 9, Koichumanova teaches “The cell consists of a stainless steel block with a cylindrical channel for IRE … inlet (8) and outlet (10) … and a thermocouple (9) installed in a pocket hole at the middle point of the reactor.” (page 187, par 1).
This quote expressly teaches instrumentation associated with the enclosure for temperature measurement, namely “a thermocouple (9)” positioned at the middle point of the reactor. That is a concrete measuring structure linked to the enclosure/reactor volume.
Koichumanova also teaches pressure control:
“Pressure in the system was kept at the required level by a back-pressure regulator.” (page 187, par 3).
Thus, the overall reactor setup teaches measurement/control instrumentation for at least temperature and pressure. The current quotes do not expressly teach flow-rate or chemical-composition instrumentation located within the enclosure itself, but temperature instrumentation is clearly taught.
Regarding claim 10, Koichumanova teaches “A commercial ATR-Tunnel cell with a heating possibility (temperatures up to 300 ◦C and pressures up to 80 bar) …” (page 187, par 1).
“The cell was heated using a rod-shaped heating cartridge (100W) …” (page 187, par 1).
These quotes identify the specific heating structure used with the enclosure. The heating cartridge raises the temperature of the cell region that surrounds the specimen-coated IRE, thereby raising the specimen temperature during ATR monitoring.
Regarding claim 11, Koichumanova teaches “A method for in-situ time-dependent attenuated total reflectance (ATR) infrared spectroscopy for monitoring reactions between a solid or liquid specimen …” (Koichumanova, p. 187, “The goal of the current paper is to present a detailed description of the procedures used for studying materials and reactions under high-temperature and high-pressure conditions. Description includes details on design and methods enabling not only operation of the cell as a reactor under these conditions, but also acquisition of IR spectroscopic data on both dissolved and adsorbed species.”). Koichumanova therefore uses the ATR-IR cell as a reactor while acquiring spectroscopic information from species associated with the specimen during the reaction.
Koichumanova does not expressly teach that the flowing medium is “gaseous.” Ebbesen teaches the missing gas-phase operation (Ebbesen, p. 68, “After assembling the ATR-IR cell and reducing the catalyst layer (see Section 2), dry gas-phase CO was introduced into the cell. Fig. 2 shows the ATR-IR spectra obtained during CO flow over Pt/Al2O3.”). Ebbesen therefore establishes that an ATR-IR reaction cell can be operated with a gaseous flowing medium contacting a solid specimen.
It would have been obvious to one of ordinary skill in the art to modify the ATR-IR flow cell of Koichumanova to operate with a gaseous flowing medium as taught by Ebbesen in order to permit ATR-IR investigation of gas-phase reactions. Ebbesen expressly teaches the resulting technical benefit (Ebbesen, p. 72, “This study convincingly shows the benefit of ATR-IR spectroscopy for comparing properties of adsorbed molecules on supported noble metal catalysts in gas phase and aqueous phase, because the same catalyst can be used for both types of experiments.”).
“attaching a flow chamber to an infrared spectrometer, the flow chamber comprising an enclosure, a gas inlet and a specimen door,” Koichumanova teaches attaching an ATR-IR flow chamber having an enclosure and inlet to an infrared spectrometer (Koichumanova, p. 187, “The cell consists of a stainless steel block with a cylindrical channel for IRE (Fig. 1c, 7), inlet (8) and outlet (10) perpendicular to the main channel”; p. 187, “The ATR-IR cell was installed in the chamber of an FTIR spectrometer (Bruker, Tensor 27) with a mercury-cadmium-telluride detector (MCT D316/6-L).” ). The stainless-steel block and cylindrical channel constitute the enclosure, inlet (8) supplies flowing medium to that enclosure, and the ATR-IR cell is installed in the FTIR spectrometer.
Koichumanova does not expressly teach the claimed specimen door. Specac teaches an openable and closable clamp bridge providing access to the ATR crystal (Specac, pp. 38–39, “Undo the bridge quick lock T-knob (25) and lift the clamp bridge (19) up past the stay up catch (26).”; “When a background spectrum has been collected, a sample can be placed into position on the ATR crystal to collect a sample spectrum.” ). Specac further teaches that the bridge has a locking mechanism and is closed during solid-sample measurement (Specac, p. 37, “The clamp bridge (19) has a quick lock and release mechanism (25). When pressure needs to be applied to a solid sample via an appropriate fitted anvil (18), the bridge must be closed”; “The quick lock and release T-knob handle (25) is pushed down and turned 90° clockwise to lock the bridge (19) closed.”).
In the modified Koichumanova flow chamber, Specac's openable and closable clamp bridge corresponds to the claimed specimen door because the bridge provides an access opening to the specimen/ATR-crystal region, is opened to permit placement or removal of the specimen, and is thereafter closed and locked during spectroscopic measurement.
It would have been obvious to incorporate Specac's openable bridge and clamping arrangement into the Koichumanova/Ebbesen ATR flow chamber to permit placement and removal of discrete solid specimens while providing reproducible specimen contact. Specac expressly teaches that its “special bridge and clamping mechanism” provides “excellent and reproducible contact between a solid sample and the single reflection ATR crystal” and that compression anvils provide “the best possible contact and sample containment over the ATR crystal.” (Specac, p. 4).
“inserting the specimen inside the enclosure through the specimen door and placing the specimen on top of an ATR crystal of the infrared spectrometer,” Specac teaches opening the bridge and then positioning the specimen directly on the ATR crystal (Specac, pp. 38–39, “Undo the bridge quick lock T-knob (25) and lift the clamp bridge (19) up past the stay up catch (26).”; “When a background spectrum has been collected, a sample can be placed into position on the ATR crystal to collect a sample spectrum.” ; Specac, p. 41, “Take the flat solid sample and place it very carefully for the surface to be measured to be in contact with ATR crystal such that it covers the entire surface of the diamond ATR crystal (23).” ). In the modified Koichumanova enclosure, opening the Specac bridge provides access through the specimen-door opening to the ATR crystal, and the specimen is placed through that opening onto the ATR crystal inside the flow chamber.
“pressing the specimen firmly against the ATR crystal with an anvil to make tight contact for spectroscopic measurement, closing the specimen door,” Specac teaches (Specac, p. 35, “The contact between a solid sample and crystal is improved using the clamp bridge (19) and an appropriate compression head anvil (18).”). Specac further teaches the particular sequence (Specac, pp. 41–42, “Gently lower the bridge (19) past the stay up catch (26) and lock it closed using the quick lock T-knob (25)”; “Begin turning the torque screw knob (22) clockwise to lower the anvil (18) towards the sample surface. Continue rotation until the central Torx screw (24) stops rotating, but the outer black knob continues to turn. At this point the maximum load achievable from the torque limiter screws (22) own torque mechanism will be applied to the flat solid sample forcing it against the ATR crystal.” ). Thus, the bridge is closed and locked and the anvil is lowered to apply mechanical load that expressly forces the specimen against the ATR crystal for ATR spectral measurement.
“directing the gaseous flowing medium from the inlet port through the flow chamber so that solid or liquid specimen reacts with one or more components of the gaseous flowing medium,” Koichumanova teaches an inlet and outlet connected to the flow-cell channel containing the specimen-bearing IRE (Koichumanova, p. 187, “The inlet and outlet of the reactor have Swagelok fittings, which allow connection with 1/16 inch SS tubing.” ), while Ebbesen teaches directing gaseous reactants through an ATR-IR cell containing the specimen (Ebbesen, p. 68, “dry gas-phase CO was introduced into the cell. Fig. 2 shows the ATR-IR spectra obtained during CO flow over Pt/Al2O3.”).
Ebbesen further expressly teaches reaction with a component of the gaseous flowing medium (Ebbesen, p. 69, “After CO adsorption on the Pt/Al2O3 layer, the adsorbed CO was oxidized by oxygen (in either dry gas phase or aqueous phase), during which ATR-IR spectra were recorded.”). Accordingly, in the combined system, gaseous reactant supplied through the inlet passes through the flow chamber and contacts the specimen, where oxygen reacts with adsorbed CO on the Pt/Al2O3 specimen.
“recording the infrared spectra of the solid or liquid sample as function of time by the infrared spectrometer, the infrared spectra changing as a result of reactions between the specimen and components of the gaseous flowing medium,” Ebbesen expressly teaches that, during oxidation of the adsorbed CO by oxygen, “ATR-IR spectra were recorded” and that “[t]he normalized integrated peak area of linearly adsorbed CO during oxidation is shown in Fig. 5 as a function of time for both the gas and aqueous phase.” Ebbesen further states, “In both experiments, an immediate decrease in the peak intensity of linear and bridging CO was observed during oxidation of preadsorbed CO.” (Ebbesen, p. 69). Thus, the infrared spectra are recorded as a function of time and the measured spectral intensity changes as the adsorbed CO is oxidized by oxygen in the flowing gaseous medium.
“allowing the gaseous flowing medium to escape the enclosure.” Koichumanova expressly provides both “inlet (8) and outlet (10) perpendicular to the main channel” and states that “[t]he inlet and outlet of the reactor have Swagelok fittings, which allow connection with 1/16 inch SS tubing.” (Koichumanova, p. 187). When operated with the gaseous flowing medium taught by Ebbesen, inlet (8) admits the gas to the enclosure and outlet (10) provides the flow path by which the gaseous medium exits the enclosure after passing the specimen.
Regarding claim 13, “A method for in-situ time-dependent attenuated total reflectance (ATR) infrared spectroscopy for monitoring reactions between a solid or liquid specimen and a gaseous flowing medium,” is taught by Koichumanova in view of Ebbesen for the reasons set forth above regarding claim 11. Ebbesen expressly teaches gas-phase ATR-IR reaction monitoring, including that “dry gas-phase CO was introduced into the cell” and that ATR-IR spectra were obtained “during CO flow over Pt/Al2O3.” (Ebbesen, p. 68).
“placing the specimen on top of an ATR crystal of an infrared spectrometer and pressing it firmly to the ATR crystal with an anvil to make tight contact for spectroscopic measurement,” Specac teaches that the Golden Gate ATR accessory is mounted into an infrared spectrometer and provides a specimen-contacting ATR crystal (Specac, p. 4, “A complete Golden Gate™ ATR accessory system consists of an ATR crystal top plate assembly fixed over an optical beam condensing unit. This complete accessory is mounted into an infrared spectrometer using a Benchmark™ baseplate.”). Specac further teaches (Specac, p. 41, “Take the flat solid sample and place it very carefully for the surface to be measured to be in contact with ATR crystal such that it covers the entire surface of the diamond ATR crystal (23).” ) and (Specac, pp. 41–42, “Begin turning the torque screw knob (22) clockwise to lower the anvil (18) towards the sample surface… the maximum load achievable from the torque limiter screws (22) own torque mechanism will be applied to the flat solid sample forcing it against the ATR crystal.” ). Thus, Specac's anvil is a concrete mechanical structure that applies load to the specimen and forces the specimen into contact with the ATR crystal for collection of an ATR spectrum.
“attaching to the infrared spectrometer a flow chamber, so that the specimen on the ATR crystal is inside the flow chamber, the flow chamber comprising an enclosure, a gas inlet, and a specimen entrance door,” Koichumanova teaches an ATR-IR flow chamber attached to an FTIR spectrometer and containing the sample-bearing IRE (Koichumanova, p. 187, “The cell consists of a stainless steel block with a cylindrical channel for IRE (Fig. 1c, 7), inlet (8) and outlet (10) perpendicular to the main channel”; “The IRE … coated with a sample (6) … was placed coaxially inside the channel”; and “The ATR-IR cell was installed in the chamber of an FTIR spectrometer.” ). The stainless-steel block/channel is the enclosure, the specimen-bearing ATR element is positioned inside that enclosure, and inlet (8) supplies flowing medium to the enclosure.
Koichumanova does not expressly teach the specimen entrance door. Specac teaches the missing openable access structure (Specac, pp. 38–39, “Undo the bridge quick lock T-knob (25) and lift the clamp bridge (19) up past the stay up catch (26).”; “When a background spectrum has been collected, a sample can be placed into position on the ATR crystal to collect a sample spectrum.”). Specac further teaches reopening the same bridge to remove the specimen (Specac, p. 42, “Unlock the bridge (19) by pushing down and turning the quick lock T-knob (25) 90° anticlockwise and open the bridge (19) up past the stay up catch (26).”; “Remove the flat solid sample carefully away from the ATR crystal.”). In the modified flow chamber, bridge (19) therefore corresponds to the specimen entrance door because it is the openable and closable access structure through which the ATR-crystal specimen region is accessed for placement and removal of the specimen.
With respect to the recited sequence of placing and pressing the specimen before attaching the flow chamber, Specac additionally teaches that the specimen/ATR top-plate assembly can be prepared before its installation into the spectrometer arrangement. In particular, Specac teaches a reactive-sample anvil for which, “[w]hen clamped in position an air tight seal is formed around the sample being held in contact against the ATR crystal. Air sensitive samples can be positioned on a top plate in a controlled environment (for example a glove box or fume cupboard). The top plate and anvil can then be taken from the controlled area and placed on the Golden Gate™ optical unit in the spectrometer.” (Specac, pp. 31–32). Thus, Specac expressly contemplates placing the specimen on the ATR crystal and clamping it with the anvil before completing assembly of the specimen-bearing ATR structure with the spectrometer apparatus.
It would have been obvious to one of ordinary skill in the art to employ this known specimen-first assembly sequence when incorporating Specac's removable-specimen/anvil arrangement into the Koichumanova/Ebbesen flow chamber because Specac expressly teaches that the arrangement permits the specimen to be positioned and clamped before the ATR assembly is installed in the spectrometer. This would facilitate handling of removable or air-sensitive specimens while maintaining the specimen in contact with the ATR crystal during subsequent assembly.
“directing the gaseous flowing medium from the gas inlet into the flow chamber so that specimen reacts with the gaseous flowing medium,” is taught by Koichumanova's flow-cell inlet in view of Ebbesen's gas-phase operation. Ebbesen teaches that “dry gas-phase CO was introduced into the cell” and ATR-IR spectra were obtained “during CO flow over Pt/Al2O3.” (Ebbesen, p. 68). Ebbesen further teaches that “the adsorbed CO was oxidized by oxygen (in either dry gas phase or aqueous phase), during which ATR-IR spectra were recorded.” (Ebbesen, p. 69). Thus, gaseous medium is directed into the ATR flow cell and a component of that gaseous medium reacts with material at the specimen.
“recording the infrared spectra of the sample as function of time by the infrared spectrometer, the infrared spectra changing as a result of reactions between the specimen and components of the gaseous flowing medium,” Ebbesen teaches recording ATR-IR spectra during gas-phase oxidation and expressly reports the spectral response as a function of time: “The normalized integrated peak area of linearly adsorbed CO during oxidation is shown in Fig. 5 as a function of time for both the gas and aqueous phase”; and “[i]n both experiments, an immediate decrease in the peak intensity of linear and bridging CO was observed during oxidation of preadsorbed CO.” (Ebbesen, p. 69). The declining CO peak intensity is therefore a time-dependent change in the infrared spectrum resulting from oxidation by a component of the gaseous flowing medium.
“allowing the gaseous flowing medium to escape the enclosure,” Koichumanova teaches that the flow-cell enclosure includes both “inlet (8) and outlet (10)” and that “[t]he inlet and outlet of the reactor have Swagelok fittings, which allow connection with 1/16 inch SS tubing.” (Koichumanova, p. 187). When modified for the gaseous flow taught by Ebbesen, the gaseous medium enters through inlet (8), passes through the specimen-containing flow chamber, and exits through outlet (10).
Regarding claim 14, Koichumanova teaches
“The IRE (ZnSe rod …)”
“Common materials used for IREs include germanium, silicon, zinc sulfide and zinc selenide … ZnSe has been used in our study as the most suitable material, due to its high refractive index, wide spectral range …” (page 186, par 3).
These quotes teach an ATR crystal/IRE made of ZnSe and expressly explain its suitability based on optical properties in the IR range. That supports the limitation that the crystal material is transparent in the infrared spectral range. The exact HATR terminology is not presently quoted, but ATR crystal and IR-transparent material are taught.
Regarding claim 15, Ebbesen teaches changing gas composition during operation:
“After a flow of dry CO, the cell was flushed with dry argon for 15 min, after which a dry oxygen-rich stream (10% O2/Ar) was introduced to oxidize the adsorbed CO.” (page 68, par 4).
This exact sequence teaches a non-constant gas composition. The flowing medium changes from dry CO to dry argon to oxygen-rich gas. That is sufficient for the alternative limitation that the gaseous flowing medium composition is not constant.
Regarding claim 16, the limitation “composition is not known” does not impose any structural or functional limitation on the method steps, as the method operates the same regardless of whether the operator knows the composition. Therefore, the limitation is not entitled to patentable weight.
Regarding claim 17, Ebbesen teaches
“dry oxygen-rich stream (10% O2/Ar)” (page 68, par 4).
This quote expressly teaches a gaseous flowing medium containing more than one chemical compound, namely oxygen and argon.
Regarding claim 18, Ebbesen teaches
“dry oxygen-rich stream (10% O2/Ar) was introduced to oxidize the adsorbed CO.” (page 68, par 4).
This teaches a two-component gas stream in which O2 is the reactive component that oxidizes the adsorbed CO. Ar is the inert diluent component and, on the face of the disclosure, is not the component causing oxidation. Thus, the quote supports the claimed arrangement of one nonreactive component and one reactive component in the gaseous flowing medium.
Regarding claim 19, Ebbesen teaches
“No gaseous CO was detected during CO flow, whereas linearly adsorbed CO on platinum was initially detected …” (page 68, par 4).
This quote directly teaches adsorption of a chemical component of the gaseous flowing medium onto the specimen. CO is present in the gas-phase stream and becomes adsorbed CO on platinum. That satisfies the adsorption branch of the claim. The desorption branch is not needed because the claim is written in the alternative.
Regarding claim 20, Koichumanova teaches a catalyst specimen on the ATR element:
“APR of hydroxyacetone over supported Pt catalyst is used as a model reaction … to demonstrate the ability to observe adsorbates on the catalyst surface.” (page 187, par 0)
“In flow cells, the catalyst is deposited on top of the IRE …” (page 186, par 1).
Ebbesen teaches that the gas-phase medium reacts on the catalyst-bearing ATR element:
“The adsorption and oxidation of carbon monoxide over a Pt/Al2O3 catalyst layer deposited on a ZnSe internal reflection element was investigated both in gas phase and water …” (abstract).
“dry gas-phase CO was introduced into the cell … during CO flow over Pt/Al2O3.” (page 68, par 3).
These disclosures, read together, provide the full cause-and-effect chain. Koichumanova supplies the catalyst-on-IRE ATR flow-cell structure. Ebbesen supplies the gas-phase catalytic reaction mode, specifically oxidation of CO over the catalyst layer in the ATR cell. Thus, the specimen is a catalyst, and one or more components of the gaseous flowing medium participate in the catalyzed reaction.
Claim(s) 8 is/are rejected under 35 U.S.C. 103 as being unpatentable over Koichumanova in view of Ebbesen and Specac as applied to claims 1-7, 9-11 and 13-20 above, and further in view of Ryczkowski (Catalysis Today, 2001).
Regarding claim 8, Koichumanova does not specifically disclose that the device further comprising a vacuum pump in communication with an interior of the enclosure and configured to create negative pressure within the enclosure.
However, Ryczkowski discloses a vacuum pump in communication with an interior of the enclosure and configured to create negative pressure within the enclosure:
“The internal volume of the IR cell is ca. 25 ml. The gas inlet and outlet of the IR cell were connected to gas line and vacuum system (0.13 Pa), respectively, through a three-way valve and a two-way valve. By proper switching of these valves, the catalyst sample in the IR cell can be evacuated or introduced to different gas atmospheres.” (Fig. 1, page 270, par 3).
It would have been obvious to one of ordinary skill in the art to include a vacuum pump in communication with an interior of the enclosure and configured to create negative pressure within the enclosure, in order to introduce different gas atmospheres into the enclosure.
Claim(s) 12 is/are rejected under 35 U.S.C. 103 as being unpatentable over Koichumanova in view of Ebbesen and Specac as applied to claims 1-7, 9-11 and 13-20 above, and further in view of Watschinger et al. (Rev. Sci. Instrum., 2021) (Waschinger).
Regarding claim 12, Koichumanova does not specifically teach directing the gaseous flowing medium from the inlet port through the flow chamber so that it is filled with the gaseous flowing medium before the specimen is placed in the enclosure.
Watschinger teaches directing the gaseous flowing medium from the inlet port through the flow chamber so that it is filled with the gaseous flowing medium before the specimen is placed in the enclosure.
“N2-purged spectrometer with a high-temperature operando transmission FTIR reaction cell (D),” (Fig. 1).
It would have been obvious to one of ordinary skill in the art to direct the gaseous flowing medium (N2) from the inlet port through the flow chamber so that it is filled with the gaseous flowing medium before the specimen is placed in the enclosure, in order to N2-purge the FTIR reaction cell.
Response to Arguments
Applicant’s arguments with respect to claim(s) 1 have been considered but are moot in view of new ground of rejection
Conclusion
Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
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/XIAOYUN R XU, Ph.D./ Primary Examiner, Art Unit 1797
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