DETAILED 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 .
Information Disclosure Statement
The information disclosure statement (IDS) submitted on 5/12/2025 has been considered by the examiner.
Claim Objection
Claims 11 and 18-20 are objected to because of the following informalities:
Claim 11: please amend “a test specimen” in Ln 3 to – [[a]] the test specimen--.
Claim 18: please amend “The method of claim 11” to -- The method of claim 11,--.
Claim 19: please amend “The method of claim 18” to -- The method of claim 18,--.
Claim 20: please amend “a first side” to –[[a]] the first side-- “a second side” to –[[a]] the second side--.
Appropriate correction is required.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 11-20 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as failing to set forth the subject matter which the inventor or a joint inventor, or for applications subject to pre-AIA 35 U.S.C. 112, the applicant regards as the invention.
Regarding claim 11, claim 11 recites “the hydrogen permeation transient”, which lacks antecedent basis. Therefore, the scope of claim 11 is indefinite. Claims 12-20 are further rejected by virtue of their dependence upon and because they fail to cure the deficiencies of indefinite claim 11.
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claims 11-14 and 17 are rejected under 35 U.S.C. 103 as being unpatentable over Ayagou et al. (Corrosion and hydrogen permeation in H2S environments with O2 contamination, 1: tests on pure iron at high H2S concentration, Corrosion, 2018, 74, 1192-1202), and further in view of Chen et al. (CN105300874A, English translation). Chen is provided in IDS filed on 5/12/2025.
Regarding claim 11, Ayagou teaches a method of performing electrochemical and hydrogen permeation measurements using a test specimen (a method of performing both corrosion and hydrogen uptake tests using a classic two-chamber hydrogen permeation cell. At the entry side, EIS is used to evaluate the corrosion behavior of the iron membrane in the H2S medium. At the exit side, hydrogen permeation is measured by anodic extraction [the last paragraph in Introduction and section of Electrochemical Measurements]; the iron membrane is deemed as the test specimen), comprising:
arranging the test specimen between two reservoirs (two cells separated by the iron membrane [the 1st paragraph in Electrochemical Measurements]), a first side of the test specimen being exposed to a first reservoir containing a process fluid including hydrogen sulfide (entry side exposed to the corrosive H2S medium [the 1st paragraph in Electrochemical Measurements]), and a second side of the test specimen being exposed to a second reservoir containing a basic solution (exit side exposed to 0.1 M NaOH [the 1st paragraph in Electrochemical Measurements]);
establishing a voltage potential at the first side of the test specimen (The charging side of the iron membrane was used as a working electrode during EIS measurements, with Ag/AgCl reference electrode and a platinum mesh as auxiliary electrode. A perturbation of [Symbol font/0xB1]10 mV amplitude around the corrosion potential was applied, and each EIS measurement was preceded by an OCP measurement [the 2nd paragraph in Electrochemical Measurements]);
measuring a corrosion rate at the first side of the test specimen (Corrosion rates were evaluated through electrochemical measurements at the entry face of the permeation membrane [the 3rd paragraph in Impact of Oxygen on Corrosion]. For both test solutions, an excellent agreement was found between the average corrosion rate calculated from electrochemical measurements and weight-measurement [the paragraph below equation 8]);
establishing a voltage potential at the second side of the test specimen to generate an atomic hydrogen permeation transient for hydrogen atoms permeating from the first side to the second side of the specimen (the exit surface of the membrane as a working electrode was polarized to +250 mV Hg/HgO reference electrode. With the three-electrode system completed with an immersed platinum mesh, the resulting current at the exit surface provided a direct measurement of the hydrogen flux across the iron membrane [the 2nd paragraph in Electrochemical Measurements]); and
measuring a hydrogen permeation transient (Fig.9 shows the measured hydrogen permeation transients [Impact of O2 on Hydrogen Permeation]).
Ayagou is silent to the following limitation: wherein the test specimen subjects to different forms of tensile stress.
Chen teaches a stress corrosion and hydrogen measuring electrochemical in-situ measurement device as shown in Figs.1-2 [para. 0019] comprising a test specimen 5 disposed between two reservoirs, a first side (right side of the specimen 5 in Fig.2) of the test specimen 5 being exposed to a first reservoir (hydrogen charging tank 32 in Fig.2 [para. 0024]) containing a process fluid including hydrogen sulfide (H2S solution 31 in Fig.2 [para. 0024]), and a second side (left side of the specimen 5 in Fig.2) of the test specimen being exposed to a second reservoir (hydrogen measuring tank 33 in Fig.2 [para. 0024]) containing a basic solution (NaOH solution 28 in Fig.2 [para. 0024]), and the test specimen 5 subjects to different forms of tensile stress (under slow strain rate conditions [para. 0002, 0026]; claim 1; strain tensile machine 25 configured to apply a longitudinal strain on the test specimen as shown the four arrows in Fig.2 [para. 0026]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the apparatus in Ayagou to provide a strain tensile machine coupled to the test specimen and configured to apply longitudinal strain on the test specimen, and further modify the method to perform electrochemical and hydrogen permeation measurements using the test specimen subject to different forms of tensile stress, as taught by Chen, since it would allow electrochemical in-situ measurements of stress corrosion and hydrogen permeation [para. 0016 in Chen].
Regarding claim 12, modified Ayagou teaches the method of claim 11, further comprising applying a longitudinal strain to the test specimen (as outlined in the rejection of claim 11 above, modified Ayagou teaches applying a longitudinal strain to the test specimen by the added strain tensile machine to perform electrochemical and hydrogen permeation measurements using the test specimen subject to different forms of tensile stress).
Regarding claims 13-14, modified Ayagou teaches the method of claim 12, and Chen further teaches the stress applying device will apply a tensile force to the tensile sample 5 made of the metal material to be measured with the stretching rate of setting until reaching [para. 0032]. Thus, Chen is silent to: wherein the longitudinal strain is constant in force (of claim 13); and wherein the longitudinal strain is variable in force (of claim 14).
Since there are only two finite number of predictable results: (A) wherein the longitudinal strain is constant in force; and (B) wherein the longitudinal strain is variable in force. Therefore, there is a finite number of identified, predictable solutions with a reasonable expectation of success. It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to try by choosing from the above two finite number of identified solutions, which would lead to choose either (A) wherein the longitudinal strain is constant in force; or (B) wherein the longitudinal strain is variable in force. Choosing from a finite number of identified, predictable solutions, with a reasonable expectation for success, is likely to be obvious to a person if ordinary skill in the art. See KSR International Co. v. Teleflex Inc., 550 U.S. 398, 415-421, USPQ2d 1385, 1395 – 97 (2007) (see MPEP § 2143 (I)(E)).
Regarding claim 17, modified Ayagou teaches the method of claim 11, and Ayagou teaches further comprising controllably maintaining a temperature in the first and second reservoirs at a selected magnitude in a range of 20 °F to an elevated temperature of +194 °F (-29 °C to +90 °C) (the cells jackets permits the circulation of thermostatically controlled water, and thus maintained the solution temperature at 24 [Symbol font/0xB1] 2 oC throughout the testing period [the 1st paragraph of Electrochemical Measurements]).
Claims 15 and 18-19 are rejected under 35 U.S.C. 103 as being unpatentable over Ayagou and Chen, as applied to claim 11 above, and further teaches Lewis et al. (US5405513A). Lewis was provided in IDS filed on 5/12/2025.
Regarding claims 15 and 18, modified Ayagou teaches the method of claim 11,and is silent to: (1) further comprising stirring the process fluid in the first reservoir and the basic solution in the second reservoir (of claim 15); and (2) further comprising stirring the process fluid in the first reservoir to promote saturation with H2S gas at high partial pressures; and stirring the basic solution in the second reservoir to promote replenishment of hydroxide ions in the vicinity of the test specimen (of claim 18).
Lewis teaches method and apparatus for the simultaneous measurement of the general corrosion rate and the atomic hydrogen permeation rate through at least two like specimens in the same test cell, under the same conditions at the same time (abstract). Fig.1 shows the electrochemical test cell wherein a hydroxide reservoir 50 is the hydrogen collection device adapted to receive a permeation counter electrode 137 and permeation reference electrode 138 (Col.6, lines 60-65). Counter electrodes 130 and 131 are positioned in the cell body directly in front of each sample port. The counter electrode located at sample port 2 housing the hydrogen permeation test specimen 10 is referred to as the permeation charging counter electrode 130. Gas inlet 135 and outlet 136 with appropriate values are positioned in the test cell (Col. 7, lines 40-58). A stirrer 141 is disposed in the cell body, and the stirrer 141 is activated and maintained at a stir rate of approximately 300 to 400 rpm. The hydroxide reservoir is filled with 0.1N sodium or potassium hydroxide solution (Col. 9, Lines 15-24). Thus, Lewis teaches a first stirrer 141 positioned in the first reservoir.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the apparatus and method in modified Ayagou by adding a first stirrer positioned in the first reservoir to stir the process fluid in the first reservoir, as taught by Lewis, since it would allow to provide a uniform temperature of the solution in the first reservoir (Col.9 Ln 15-19 in Lewis). Furthermore, the claimed limitations (i.e., a first stirrer positioned in the first reservoir to stir the fluid/solution in the first reservoir) are obvious because all the claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination yielded nothing more than predictable results [MPEP 2143(I)(A)].
Similar to the first stirrer positioned in the first reservoir for mixing/stirring the solution therein to have a uniform temperature, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the apparatus and method in modified Ayagou by adding a second stirrer positioned in the second reservoir for mixing the basic solution in the second reservoir. To incorporate the second stirrer positioned in the second reservoir would constitute a mere duplication of parts that would yield the predictable result of mixing/stirring the basic solution in the second reservoir to provide a uniform temperature of the solution on the second side of the test specimen. It has been held that mere duplication of parts has no patentable significance unless a new and unexpected result is produced. See MPEP § 2144.04(VI)(B). Furthermore, the use of a known technique (i.e., having a stirrer in a cell for mixing the solution within the cell) to improve similar devices in the same way is likely to be obvious. See KSR International Co. v. Teleflex Inc., 550 U.S. 398, 415-421, USPQ2d 1385, 1395 – 97 (2007) (see MPEP § 2143(I)(C)).
With the above modification, modified Ayagou teaches: (1) further comprising stirring the process fluid in the first reservoir and the basic solution in the second reservoir (of claim 15); and (2) further comprising stirring the process fluid in the first reservoir; and stirring the basic solution in the second reservoir (of claim 18).
The limitations “to promote saturation with H2S gas at high partial pressures” and “to promote replenishment of hydroxide ions in the vicinity of the test specimen” in instant claim 18 are intended results of a positively recited step. The court noted that a "‘whereby clause in a method claim is not given weight when it simply expresses the intended result of a process step positively recited.’" Id. (quoting Minton v. Nat’l Ass’n of Securities Dealers, Inc., 336 F.3d 1373, 1381, 67 USPQ2d 1614, 1620 (Fed. Cir. 2003)). MPEP 2111.04(I).
Regarding claim 19, modified Ayagou teaches the method of claim 18, and Ayagou teaches further comprising:
positioning a first reference electrode and a first counter electrode in the first reservoir, forming a charging cell (the charging side of the iron membrane was used as a working electrode with Ag/AgCl reference electrode and a platinum mesh as auxiliary electrode [the 2nd paragraph in Electrochemical Measurements]); and
positioning a second reference electrode and a second counter electrode in the second reservoir, forming a permeation cell (the exist surface of the membrane held in 0.1 M NaOH solution as a working electrode, was polarized to +250 mVHg/HgO [1 M KOH] reference electrode. With the three-electrode system completed with an immersed platinum mesh [the 2nd paragraph in Electrochemical Measurements]).
Claim 16 are rejected under 35 U.S.C. 103 as being unpatentable over Ayagou and Chen, as applied to claim 11 above, and further teaches Zhou et al. (The effect of the partial pressure of H2S on the permeation of hydrogen in low carbon pipeline steel, Corrosion Science, 2013, 67, 184-192)
Regarding claim 16, modified Ayagou teaches the method of claim 11, and is silent to further comprising controllably maintaining a pressure in the first and second reservoirs at a selected magnitude in a range of 1 MPa to an elevated pressure of 14 MPa.
Zhou teaches the effect of different partial pressure of H2S on the hydrogen permeation of API-X52 pipeline carbon steel in a high-temperature and high-pressure hydrogen permeation device (abstract), and Fig. 2 show the test specimen disposed between two reservoirs (a hydrogen-generating cell [input side] and a hydrogen-oxidising cell [detection side]). In this device, the material was sealed along with the hydrogen-generating cell with some insulating materials to allow them to remain sealed under more than 2 MPa of pressure. In the cathodic side, the cell is filled with test solutions, including a certain pressure of H2S. The detection side is filled with a 0.2 N NaOH solution. The thickness of the specimens is 3 mm to ensure that the specimens can withstand the 2 MPa of pressure (section 2.3). Fig.3 shows the hydrogen permeation transient measured for 3 mm steel membranes exposed to test solution at 5% NaCl and 1 MPa H2S or 5% NaCl and 0.1 MPa H2S. Thus, Zhou teaches an apparatus similar to that of Ayagou, but the test specimen and the first reservoir (the hydrogen-generating cell) can withstand 2 MPa of pressure, and further teaches controllably maintaining a pressure in the first reservoir at 1 MPa (see Fig.3).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the apparatus in modified Ayagou such that the first reservoir and test specimen of the modified apparatus can withstand 2 MPa, and further modify the method to perform the hydrogen permeation tests by controllably maintaining a pressure in the first reservoir at 1 MPa, as taught by Zhou, since it would allow to investigate the hydrogen permeation behavior of the test specimen in a high-pressure condition (abstract in Zhou).
Similar to the first reservoir to withstand 2 MPa pressure and maintain the pressure in the first reservoir at 1 MPa, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to further modify the apparatus and method in modified Ayagou by having the second reservoir also withstands 2 MPa of pressure, and controllably maintaining a pressure of the second reservoir at 1 MPa. To incorporate the second reservoir withstanding 2 MPa pressure would constitute a mere duplication of parts that would yield the predictable result of the second reservoir to withstand a high pressure of 2 MPa such that the apparatus would be used to investigate hydrogen permeation behaviors of the test specimen under high-pressure environment. It has been held that mere duplication of parts has no patentable significance unless a new and unexpected result is produced. See MPEP § 2144.04(VI)(B).
Claim 20 is rejected under 35 U.S.C. 103 as being unpatentable over Ayagou, Chen and Lewis, as applied to claim 19 above, and further teaches Nakamaru et al. (JP2016061652A, English translation) and Cao et al. (CN207036626U, English translation). Nakamaru and Cao were provided in IDS filed on 2/15/2025.
Regarding claim 20, modified Ayagou teaches the method of claim 19, and Ayagou is silent to further comprising extending the first reference electrode toward a first side of the test specimen using a first salt bridge; and extending the second reference electrode toward a second side of the test specimen using a second salt bridge.
Nakamaru teaches a hydrogen permeation test apparatus as shown in Fig.1, wherein each cell housing/reservoir includes a counter electrode 4a/4b and a reference electrode 3a/3b, wherein the test sample 2, counter electrode 4a and reference electrode 3a are coupled to a first potentiostat (the left potentiostat in Fig.1), and the test sample 2, counter electrode 4b and reference electrode 3b are coupled to a second potentiostat (the right potentiostat in Fig.1), and wherein the first reference electrode 3a is extending toward a first side of the test specimen, and the second reference electrode 3b is extending toward a second side of the test specimen (see Fig.1) [paras. 0032-0034].
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the first and second reference electrodes in modified Ayagou such that the first reference electrode is extending to the first side of the test specimen, and the second reference electrode is extending toward the second side of the test specimen, as taught by Nakamaru, since Nakamaru teaches the suitable alternative configuration for hydrogen permeation test (see Fig.1). Furthermore, the use of a known technique (i.e., having each reference electrode extending toward the corresponding side of the test specimen in each reservoir as taught by Nakamaru) to improve similar devices (a system for hydrogen permeation measurements in modified Ayagou) in the same way is likely to be obvious. See KSR International Co. v. Teleflex Inc., 550 U.S. 398, 415-421, USPQ2d 1385, 1395 – 97 (2007) [see MPEP § 2143 (I)(C)].
Modified Ayagou is silent to wherein each reference electrode comprising a salt bridge.
Cao teaches a device for hydrogen permeation test under a constant stress loading state (Fig.1 and claim 1), wherein the device comprises a reference electrode including a salt bridge 8 (para. 0023; Fig.1; claim 1).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the first reference electrode and the second reference electrode in modified Ayagou such that each of the first and second reference electrodes includes a salt bridge, as taught by Cao, since Cao teaches that it would be suitable to use a reference electrode including a salt bridge for the hydrogen permeation test under tensile stress (claim 1 and [para. 0023]). To incorporate a 2nd salt bridge into the second reference electrode would constitute a mere duplication of parts of the first reference electrode including the first salt bridge that would yield the predictable result of providing each of the first and second reference electrodes including its respective salt bridge disposed into the respect first and second cell housings. It has been held that mere duplication of parts has no patentable significance unless a new and unexpected result is produced. See MPEP § 2144.04(VI)(B).
Conclusion
The prior arts made of record and not relied upon are considered pertinent to applicant's disclosure: Haugstveit (Hydrogen diffusion and H2S corrosion in steel, Master thesis of Norwegian University of Technology and Science, 2001) teaches a double cells for hydrogen permeation test (section 3 on pages 25-32). Shirband (Shirband Z., Understanding the effects of hydrogen, hydrostatic testing and mill-scale on SCC of pipelines in near-neutral pH environments, PhD thesis, University of Alberta, 2016) teaches a double cell for hydrogen permeation test (Fig.3.1 and section 3.2). Yamamoto et al. (US4294667A) teaches a corrosion evaluation method comprising a test specimen disposed between two reservoirs (see Figs. 1-2).
Any inquiry concerning this communication or earlier communications from the examiner should be directed to SHIZHI QIAN whose telephone number is (571)272-3487. The examiner can normally be reached Monday-Thursday 8:00 am-5:00 pm.
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/SHIZHI QIAN/Examiner, Art Unit 1795
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