The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Claims 1-4, 7 and 10-15 are rejected under 35 U.S.C. 112(b) as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor, regards as the invention. In claim 1 it is not clear if the complexing agent is added to complex the boric acid or something else in the processing solution. For example the previously cited Belcher paper (Analytica Chimica Acta 1970) teaches that mannitol and other polyols are complexing agents that form complexes with boric acid for its titration. For examination purposes, the complexing agent will be treated as a complexing agent directed toward some component of the processing solution: boric acid, a metal or come other component of the processing solution. In claim 3, it is not clear if the plating metals being claims or further components of the processing solution in addition to the iron required by claim 1 or if applicant is attempting to claim the plating metal instead of the iron required by claim 1. For examination purposes claim 3 will be treated by examiner as requiring the presence of both iron and one or more of the plating metals required by claim 3. Claim 4 will be treated as requiring the plating metal to comprise nickel. With respect to claim 12, “the first equilibrium” does not have antecedent basis in claim 1, but would if dependent from claim 10. For examination purposes, claim 12 will be treated as dependent from claim 10. With respect to claim 14, “the first equilibrium” and “the second equilibrium” do not have antecedent basis in claim 1, but would if dependent from claim 12. For examination purposes, claim 14 will be treated as dependent from claim 12. With respect to claim 15, it is not clear if something is required between the first and second inflection points such as the addition of mannitol or if the titration curve has two inflection points without doing anything after the first inflection point is reached.
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 1-7 and 10-14 are rejected under 35 U.S.C. 103 as being unpatentable over Verma in view of Bush (Transactions of the IMF 1959, newly cited and applied and hereinafter called Bush ‘59 and Bush (Analyst 1951, newly cited and applied and hereinafter called Buch ’51). In the paragraph bridging the columns on page 255 of the Verma paper, a method for the estimation of boric acid in a nickel-plating bath. To a properly buffered solution consisting of nickel salts and boric acid is added an excess of potassium oxalate followed by mannitol, when boric acid becomes available for direct titration and no correction factors have to be used. Reference to analytical methods in electroplating practice will indicate that methods advocated for estimation of boric acid invariably requires a separation of nickel prior to estimation of boric acid. This method based on the complexing of nickel ions with the oxalate places in the hands of electroplating laboratories a rapid method for the estimation of boric acid. Verma does not teach whether the titration is potentiometric or what it means for boric acid to become available for direct titration. Verma does not teach what type of titration of the plating solution was performed, that the plating solution comprised iron or other metals or other specifics titration process.
In the paper Bush ‘59 teaches the analysis of nickel sulphamate plating solutions for total nitrogen, free ammonia, nickel, boric acid and I : 3:6 trisulphonic acid. The third and fourth paragraphs of the left column on page 43 teaches that the nickel sulphamate bath usually consists of nickel sulphamate, free sulphamic acid, boric acid and naphthalene 1 : 3 : 6 trisulphonic acid, but due to the hydrolysis of the sulphamic acid, ammonium salts are usually present, together with equivalent amounts of sulphate ions. In the absence of added ammonium salts, the amount of ammonium ion present in the bath is a basis on which the sulphate content may be calculated, thus avoiding the separate determination of this ion, an operation which presents considerable difficulty. Some baths contain nickel chloride, while cobalt often occurs with nickel in these solutions in the ratio of about 0·1-1·0 parts cobalt to 100 parts of nickel. Traces of copper and iron are always present. Pages 44-45 discuss the analysis of boric acid through titration with sodium hydroxide using mannitol. This titration cannot be carried out in the presence of metallic ions, which precipitate as the borate or hydroxide within the pH range of the titration. In their method nickel must be removed from the solution before carrying out the determination of the boric acid content. A separation can be effected by distillation as methyl borate, by mercury cathode electrolysis or by passing through a cation exchange column. The latter procedure has the advantage of speed and simplicity and was used by Bush '59. The paragraph bridging pages 44-45 teaches that the potentiometric determination of the mannitol-boric acid complex is a satisfactory finish to the determination, but the use of the conventional two-indicator method is quite satisfactory in the present case, and determinations using both methods showed very close agreement. The reference cited for the potentiometric determination is Buch '51. In the published procedure, 5 ml of accurately measured sample was passed through the exchange column with water and collected until the eluant was found to be free from acid. 2 drops of p-nitro-phenol indicator (0.2% w/v) were added to the collected eluent, sodium hydroxide solution (20% w/v) was added until the yellow color of the indicator to neutralize the acid. The solution was reacidified with dilute sulphuric acid (2% v/v) until the solution was colorless followed by adding 3 drops in excess. The solution was refluxed under a water-cooled condenser to expel carbon-dioxide and cooled to room temperature. The condenser was washed down into the flask and sodium hydroxide (0·1 N; carbonate free) was added to the solution until one drop produced a faint yellow coloration First titration). 5 g of mannitol and 6 drops of phenolphthalein indicator (1% w/v in 50% ethanol) were added and the resulting solution was titrated with sodium hydroxide until the first appearance of a pink tinge. The paper teaches a conversion of 1 ml sodium hydroxide (0·1 N) = 0·006184 g boric acid.
In the paper Bush ’51 teaches the measurement of boron in boronized metals. The boron after conversion to mannitoboric acid is finally determined by potentiometric titration with sodium hydroxide, which obviates the difficulties inherent in the use of color-change indicators. The last full paragraph on page 684 teaches that early titrations were carried out with p-nitrophenol as the indicator for the first stage of the titration and phenolphthalein as end-point indicator for the alkali titration of the monohydric acid formed by the addition of mannitol. The titration of boric acid with these indicators presented difficulty. The color change was not always sharp and this could lead to appreciable personal error. The operation could be carried out with greater ease and accuracy by titrating the boric acid solution by means of a calomel - glass electrode system and a Cambridge pH meter. the paragraph bridging pages 684-685 teaches that a boron solution was prepared by dissolving pure recrystallized borax in distilled water, free from carbon dioxide, and diluting to 1 liter in a calibrated flask to make a solution containing 0-001082 g of boron per ml. Portions of this solution were aliquoted and titrated with 0.10 N sulphuric acid by means of a calomel - glass electrode system and a Cambridge pH meter. Readings of pH against acid additions were recorded throughout the titration and the end-point was determined by plotting the differential and obtaining the point of inflection of the curve. This titration was used to standardize the sulphuric acid. The pH value of the solution was then adjusted to that of the end-point, 5g of mannitol were added and the solution titrated with 0.1 N sodium hydroxide, free from carbon dioxide, and readings of pH against alkali additions were recorded as before. The end-point was determined by noting the point of inflection of the curve. The amount of sodium hydroxide used is that required to neutralize the mannito-boric acid. A curve obtained for the end-point of this titration is shown in Figure 2. The first two full paragraphs on page 685 after figure 3 teaches that to apply the principle to the titration of the boric acid in the solution after removal of the associated metals by electrolysis, the pH at the beginning of the titration should be that at which the free mineral acid has been neutralized, which is determined by adjusting the solution to about pH 4.0, then titrating with sodium hydroxide and recording pH values against alkali additions. The point at which the free mineral acid is neutralized is obtained by noting the point of inflection of the curve. It is unnecessary to adjust the pH of the solution to that of the end-point before adding mannitol and continuing the titration as described earlier. The standard sodium hydroxide corresponding to the boron present is that required to titrate the solution between the points of inflection of the two curves. A typical titration is shown in Figure 3. The curve shown in figure 3 has several points marked with letters that are explained in the figure legend as follows: A, the point at which free mineral acid is neutralized; B-C, depression of pH caused by addition of mannitol; D, end-point of boric acid titration. The specific method is found on page 687 of which the final three paragraphs are directed to the actual titration. Relevant to the instant claims is the following. Transfer the liquid after carbon dioxide expulsion to a 600-ml squat-form beaker marked at a volume of 400 ml, adjust the volume up to the mark with distilled water, free from carbon dioxide, and measure the pH of the solution. Adjust the acidity to about pH 4.0 and then titrate with 0.1 N sodium hydroxide solution, recording the pH value against the titre throughout. Determine the point of neutralization of the free mineral acid by plotting the differential and noting the point of inflection of the curve. Add 5 g of mannitol and continue the titration, recording pH against sodium hydroxide addition as previously. The end-point is at the point of inflection of the curve. The amount of 0.1 N sodium hydroxide solution required to titrate the test solution between the point of inflection of the two curves is equivalent to the amount of boron present.
It would have been obvious to one of ordinary skill in the art to use a potentiometric titration for the Verma method as taught by Bush ’51 because one of ordinary skill in the art would have recognized that the oxalate functions to complex the metals so that the boric acid can be measured/titrated with mannitol as taught by Verma, nickel plating solution also comprise iron, cobalt and copper as taught by Bush ’59, boric acid in nickel plating solutions can be measured by titration using colorimetric indicators or by potentiometric titration as taught by Bush ‘ 51and the potentiometric method is carried out with greater ease and accuracy than one using colorimetric indicators as taught by Bush ’51. It additionally would have been obvious to one of ordinary skill in the art at the time the application was filed to carry out titration steps that can be performed separately on the solution to measure other components or prepare the test solution for measurement of the boric acid and add the mannitol to the solution at an appropriate time as shown by Bush ‘59 because of the ability to measure multiple components of a nickel plating solution as shown by Bush ‘59. With respect to the specific metals of claims 1-4 and 7 Bush ’59 clearly teaches that a nickel plating solution such as one that would be measured by the process of Verma would comprise iron in addition to nickel, cobalt and copper. With respect to claims 10-15, Bush ’51 teaches that the potentiometric titration would include titration with sodium hydroxide to a first equilibrium defined by a first inflection point, addition of the polyol mannitol used by Verma, titration with sodium hydroxide to a second equilibrium defined by a second inflection point and determining the concentration of boric acid based on a difference in the amount of sodium hydroxide used to reach the first equilibrium and the second equilibrium so that modification of Verma by the teachings of Bush’ 59 and Bush ’51 shows the obviousness of these claims for the reasons given for the obviousness of claim 1.
Claims 7-8 are rejected under 35 U.S.C. 103 as being unpatentable over Verma in view of Bush ’59 and Bush ‘51 as applied to claim 1 above, and further in view of Weber (US 5,183,544) or Takahashi (Bunseki Kagaku 1976, newly cited and applied). Verma does not teach other possible complexing agents.
In example 3 of the patent Weber teaches titration methods for measuring nickel and boric acid (see column 8, lines 30-42). Of importance in the nickel measurement method is the use of 0.05 molar ethylene diamine tetraacetic acid (EDTA) as the titration agent. Those of skill in the art would have recognized that EDTA is acting as a nickel complexing agent during the titration.
The abstract of Takahashi teaches that based on the investigation of chemical reactivities of metal borides and of the metal chelate effects on the alkalimetric titration of boron, a method of successive determinations of metals and boron of Mn-, Fe-, Cu- and Al-borides has been developed. The procedure is as follows: 1) Mn-, Fe- and Cu-borides: dissolve 10 to 30 mg of a sample in a mixture of 3 ml of 3N HNO3, 3 ml of 3N H2SO4 and 0.3 ml of 10% H2O2 by heating in a quartz flask equipped with a reflux condenser. Cool the solution obtained, add 0.02M CyDTA solution in excess and neutralize to pH 3 with 2N NaOH solution. Boil the solution for several minutes to ensure the formation of the metal chelate. After cooling, adjust the pH exactly to 6.7 with 0.5M NaHCO3 solution, and then determine the metal concentration by back-titrating the excess CyDTA with 0.01M ZnSO4 solution using MTB as an indicator. After the titration is over, make the solution to pH 3 with 2N H2SO4 and boil for several minutes to expel CO2. Cool the solution, adjust the pH exactly to 7.0 with 0.1N CO2-free NaOH solution and add 5g of mannite (mannitol) and ten drops of 0.1% phenolphthalein solution. Finally, titrate the mannite-boric acid complex with 0.05N NaOH solution until the pink tinge is observed (pH 8.2). 2) Al-boride: fuse 10 to 30 mg of a sample with a mixture of 1.5 g of Na2CO3 and 0.3 g of KNO3 in a nickel crucible. Digest the melt with water and filter off the residue (nickel oxide). Add 0.01 M EDTA solution in excess to the filtrate and make it to pH 3 with 2N H2SO4. Determine Al and boron by the same method as described in 1).
It would have been obvious to one of ordinary skill in the art at the time the application was filed to replace the oxalate complexing agent of Verma with a known nickel/metal complexing agent such as the EDTA taught by Weber or Takahashi because of its known/recognized metal complexing ability in titration methods as taught by at least Takahashi.
Applicant's arguments filed March 26, 2026 have been fully considered but they are not persuasive. In response to the changes and arguments the rejection under 35 U.S.C. 112(b) has been maintained and modified to account for new issues and things that examiner missed before and the obvious rejection has been substantially modified with mostly new secondary references.
With respect to the rejection under 35 U.S.C. 112(b), the previously cited Belcher reference has been cited to show that a compound such as the added mannitol has been considered to be a complexing agent for the boric acid. Applicant’s modification of claim 1 by adding the “comprising iron” language only defined that the processing liquid must contain iron in addition to the boric acid being measured. It did not limit what else might be present in the processing fluid or define the target of the complexing agent. Thus, there is still a valid question of what constitutes the target for the complexing agent: boric acid, one or more metals present in the processing solution or some other component of the processing solution. For that reason, applicant’s argument is not persuasive with respect to the previously outlined clarity issue. The additionally outlined items are relevant to problems that examiner missed in the previous action (i.e., the antecedent basis issues) or were created by the changes applicant made to the claims. Thus applicant’s arguments are moot with respect to these issues.
With respect to the obviousness rejection and applicant’s argument that Verma and the previously applied secondary references failed to teach a processing solution comprising iron, the Ertl (Ertl is the first listed inventor on the actual patent) and Azevedo references are no longer being applied against the instant claims. Thus arguments directed to those particular references and their combination with Verma are moot. With respect to this specific argument the newly applied Bush ’59 paper clearly teaches that a nickel plating solution would contain iron, cobalt and copper in addition to the nickel and boric acid. Thus Bush shows that the nickel plating solution of Verma would have been expected to “comprise iron” so that the argument is not persuasive with respect to the instant reference combination. Because Bush ’59 has this teaching, the additionally applied secondary references do not need to have this teaching.
With respect to the problems caused by metals in boric acid titrations referred to by applicant, Verma acknowledges that there are problems that the invariably required the separation of nickel prior to estimation of boric acid. That acknowledgement was immediately followed by the teaching that the method based on the complexing of nickel ions with the oxalate places in the hands of electroplating laboratories a rapid method for the estimation of boric acid. In other words Verma teaches that the use of complexing agents of the metal eliminates the need to separate the metal(s) prior to determining boric acid. This would have been expected to apply to similar plating bath titrations by those of ordinary skill in the art. Moreover, the newly cited and applied Takahashi paper shows the use of the complexing agents CyDTA (1,2-Cyclohexylenedinitrilotetraacetic acid) and EDTA in titrations to determine boron (boric acid) using mannite (mannitol) and sodium hydroxide (NaOH) for several metal borides. This clearly provides further evidence that one of ordinary skill in the art would have expected known metal complexing agents to allow the measurement of boric acid in the presence of metal ions that would be expected in a metal plating solution. Thus the argument is not persuasive relative to the current set of references.
With respect to previous claims 10-14 and new claim 15 in particular, the Bush ’59 paper clearly teaches that the solutions were measured by both a previously developed potentiometric method and the two-indicator method that was described on pages 44-45 (see the paragraph bridging pages 44-45. The referenced paper for the previously described potentiometric method was the Bush ’51 paper. Thus Bush ’59 teaches measurement of boric acid in a nickel plating solution by a potentiometric titration method and points one to the Bush ’51 paper for the description of that method. From figure 3 of the Bush ’51 paper and its associated description/discussion as noted in the description of that reference above, it is clear that a potentiometric titration would have met the requirements set forth in claims 10-15 including a sequential titration process with two inflection points reflecting the peaks in the titration curves for a quantitative determination of the boric acid present in the sample solution. Thus the argument directed at the limitations of new claim 15 is also not persuasive with respect to the current reference combination.
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure. The additionally cited art relates to titration methods in general and/or boron/boric acid analysis titration methods. Of note is the Tereshko paper also teaching the use of complexing agents, Tiron and EDTA, as masking agent to eliminate the metal interference of titanium, zirconium, iron, aluminum and manganese in the titration process for the determination of boron in metal borides, boron nitride boronated graphite rods.
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/ARLEN SODERQUIST/Primary Examiner, Art Unit 1797
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