Document e5LrQ8xm7B0DN1ZKnrdn1j4a9

Wil u a n H. Da v is ARBA S Ma r V7N - WCTIACO De a n S. Ed mo n d s Fr a n k E. Ba r r o w s W. Br o w n Mo r t o n Me r t o n W. Sa q e Wil l is H.Ta y l o r .Jr . Er n e s t H. Me r c h a n t Ge o r o e E.Mid o l e t o n Mo r r is D Ja c k s o n R Mo r t o n Ad a ms Ra y mo n d F. Ad a ms Le s l ie B. Yo c n o Da n ie l V. Ma h o n e y D4947 Co u n s e l l o r s a t La w 165 Br o a d w a y Ne w Yo r k . Wa s h in g t o n Ornccs Na t io n a l Pr e s s Bu il d e n o ' December 27, As s o c ia t e s Ra y mo n d B Ca n f ie l d Ba l d w in Gu il d Amb r o s e A. Ar n o l d S. Ho w r v l Br o w n . Jr . Lo u is D. Fo r w a r d H. St a n l e y Ma n s f ie l d Ge o r o e E. Fa it h t t il l Do n a l F. M^Ca mt h t Ha l E. Se a o r a w r s Jo h n Bo x ie Jo h n T Ta b l e t Cu r t Vo n Bo e t t ic h k r . Jr . Ja me s B. Cb r is t is Ja me s W La is t Cy r u s S Ha p o o o d Roots T. Mc Le a n ff A BOLD A. TAV** Ke n h c t u U. Ml iik a t Ba r r y E. Do w n e r _ _ _ Ca r l - Rin o 1939 Mr. Frederick Laist, Vice-President International Smelting & Refining Co. 25 Broadway, (Hoom 1720) New York, N. Y. Dear Sir: Re: Johnson et al. Application, Ser. No. 178,352, Filed December 6, 1937, For: Method of Producing White Lead Enclosed herewith are two copies of a supplemental amendment and affidavit of Jilliam J. Knox, Jr. which was forwarded to the Patent Office today for filing in the above- mentioned application. Very truly yours. Encs. 3 copy sent to Mr. Case - AS Dec. 1939 r PNYC00008448 PENN1E, DAVIS, MARVIN AND EDMONDS COPY D4947 70:AJ Deoember 27, 1939 William J, Knox, Jr., Superintendent White Lead Plant International Smelting & Refining Co, East Chicago, Indiana Dear Ur, Knox: Re; Johnson et al. Application, Ser. No, 178,352, Piled Deoember 6, 1937, For; Method of Producing White Lead Thank you very much for your letter of December 22, 1939 with which you returned the exeouted affidavit in connection with the above-mentioned application. The affidavit seemed to be entirely satisfactory, and in faot, I was quite impressed with the showing whioh you made. I have preparod a supplemental amendment and have forwarded it with the affidavit for filing in the Patent Office. A oopy of the supplemental amendment and affidavit should come to you in the regular course. Permit me to thank you for your excellent coopera tion in this matter. Very truly yours, C.C. Mr. Lalst C.C. Ur. Case Lo. PN*cooooa449 N11446.01 IN THE UNITED STATEN PATENT OFFICE In re application of ) GUNNARD E. JOHNSON and ) REGINALD G. BOWMAN and ) WILLIAM J. KNOX., JR, ) Dlv. 56 - Room 4725 i) } METHOD OF PRODUCING SHITE LEAD New York, N. Y,, Deoember 27, 1930 SUPPLEMENTAL AMENDMENT Sir: Supplemental to the amendment filed in tha aboveidentified application on Ootober 14, 1939, an affidavit of William J. Knox, Jr., one of the above-named applicants, la being filed herewith. The principal basis on whloh the claims were rejeoted in the Offioe eotion of April 22, 1939, was lack of invention over the disclosures made in the Johnson et al. patent Ho. 1,845,713. The Examiner stated that this refer ence dearly teaahes the advantages of controlling bicarbo nate ion oonoontration in the analyte, and that in view of thia disclosure there is no Invention in the particular method of controlling bicarbonate ion concentration by the stepB of exceso oarbonation of the catholyte and adding hydroxyl ions to the anolyto in sufficient amount to establish therein a desired bicarbonate ion concentration. Actually the process of the present invention is not suggested by the disclosures of the reference. The accompanying affidavit shows that the oontrol method of the present invontion is greatly superior to the oontrol method PNYC00008A50 N11446.02 of tho Johnson at al. patent, and that it leads to extremely beneficial rosulta which oould not bo predietod on the basis of the disclosures of the references. In the affidavit it ia shown, for example, that tho chemical composition of white lead must be uniform in order to obtain a pigment having uniform oil-absorption or oil-taking properties, and that prior to the present invention tho chemical composition of white lead pigment produced eleotrolytionlly, aa indicated by Its GOg content, varied materially (on tho average from 11.403 to 12.103 COg, a range of 0.703 COg). The method of the present invention made it possible to control tho chemical composition of the pigment much more olosely (from 11.72'3 to 11.763 GOg, a normal range of only 0.04p). This product, being much more uniform than the product previously made, is a markedly superior product. The fact that this superior product nan made poBsibla by tho oontrol method of the invention is Bhown by the fact that tho process by which tho improved product is made differs from the prooeaa by whi^h the former product was made only by the substitution of the control method of the invention for tho oontrol methods formerly usod, among whieh was tho oontrol method described In tho Johnson at al. patent. A further remarkable and unpredictable advantage of the mothod of the invention is the speed with which It permits the composition of the white load product to be adjusted during commercial operation of the process. By following oontrol methods formerly used, a period amounting on the average to about 50 minutes elapsed between the time when it first become apparent that some adjustment should bo mado to oorreot the composition of the oell produot, and the time by which the adjustment actually was reflected in the oompositlon in the produat. In accordance with the oontrol -2- pNVC0000645l method of tho invention, this period amounts on tha avarage only to about S ninutoo. Tha control method of tho invention hao proven muc'i more eoonomioal in oomneroial operation than the oontrol methods formerly known and employed. For example, it is stated in the affidavit that a tank room containing 48 cells required tho attendance of four non for its sucowsful opera tion under the oontrol method described in the Johnoon et al, patent, whereas under the now control mothod the name tank room may be operated by two non. In view of the decided advantages of the oontrol method of the invention, which advantages oould not have beet predicted from tho disclosures of tho references relied upon, it is submitted thnt tho olainod proooso represents a marked advnnoo in the art and constitutes n patentable invention of a high order. It is therefore beliovod that the claims appearing in the case 3hould be allowed. Heopeotfully submitted, Attorneys for Applicants *3* PNYC00008452 IN THE UNITED STATES PATENT OFFICE In ra application of g u n n a r d s. j o iin s o n and REGINALD O. BOWMAN and WILLIAM J. KNOX, JR. Serial No. 178,352 Piled December fi, 1937 Div. 56 - Koom 4725 } ) ) ) ) METHOD OF PRODUCING WHITE LEAD ) ) ) AFFIDAVIT STATS OF INDIANA ) SS t COUNTY OP LAKE ) William J. Knox, Jr., being duly sworn deposoa and says: I am one of the applicants in the above-mentioned application. I am employed by the International Smelting and Refining Co., and I am thoroughly familiar with the white Load Plant of that Company at East Chioago, Indiana, where white lead is produced eleotrolytloally, I am and have been for the past 14 years Superintendent in oharge of this White Lead Plant. Since the invention described and claimed in the above-mentioned application was made, it has been employed in the White Load Plant and has resulted in considerable savings as compared with the processes previously employed there, including the prooess deaoribed in United States patent No. 1,845,713, and in the production of a superior white lead product. Variations in the chemical composition of white lead pigment have a marked effect on the oil-absorption or '>'`l'COOO<)8<53 N11446.03 oil-taking property of auoh pigments. The magnitude of this effeot is shown in the following table, in which is set forth the oil-absorption or oil-taking property of the pigment as determined by the three methods most oomonly used by paint teohnologista in determining the amount of oil required to produce a paint of bruehing eonslstonoy. Produot "A" Produot "B" Product X" Analysis - Percent C02 " Pb003 " Pb{0H)a Primary Oil Absorption (gjae/lOOoo) Consistency (Stromer- Krebbs Units 353 oil) Plow (Gardner flow meter, 35fS oil) 11.15 67.70 33.30 13.5 9.3K 2.2" 11.75 71.20 20.81 11.5 9. H 2.75" 12.40 75.30 24.80 8.5 7.4n 3.6" Up until the time the invention described in the above-mentioned application was made and put into use, the COg content of the white lead product produoed at the Tfhlta Lead Plant varied in normal operation of the plant from 11.4$ to 12.10$. The 00g oontent of the white lead produot made at the flhite Lead Plant alnoe the said Invention was there put into use varies in normal operation of the plant from 11.72 ft to 11.76 ft. This produot is more uniform than and hence superior to the product formerly made. The prooess by whieh the improved produot is made differs from the prooess by which the former produot was made only in that the method described in the above-mentioned application for controlling composition of the white lead produot has been substituted for the methods previously employed, among whieh waa the method of exact neutralization or aocurate deficient oarbonatlon described in United States patent Ho. 1,845,713. Aooordlng to the process of the United States patent Ho. 1,845,713, a considerable period of time was -2- p"rc o'008<, 54 required to effeet adjustment of the composition of the white lead produot. This period, which amounted on an average to about 50 minutes, wan a result of the time required for the following chain of events to take place before actual adjustment of the composition of the product could ooour: (1) Titration of oatholyte at frequent intervals. (8) Adjust ment of oarbonation faa daispor to inorscc; 2? deorodegree of oarbonation of catholyte. (3) Time required to displaoe old oatholyte in storage tanks, piping, and cells by new oatholyte of adjusted oarbonato-to-hydroride ratio. (4) Time of adjustment of ooraposltion of analyte by flow of oatholyte Ions of new ratio from oatholyte to anolyte compartment of oell. In accordance with the method described in the above-mentioned application, steps (2), (3) and (4) set forth above are eliminated, as it is only necessary to change the setting of one valve to vary the volume of alkalins solution flowing into the anolyte and so to adjust the bicarbonate ion concentration of the anolyte, and thereby to adjust the composition of the white lead produot. Moreover, the number of control titrations that are required hove been greatly reduced. As a result of these savings the period requirod to effeot adjustment of the composition of the white lead produot has been reduced to about 8 minutes on the average. The method of the invention described in the above-mentioned application has resulted In substantial operating savings. For example, to oontrol operation of a tank room containing forty-eight cells by the process described In United utatea patent IIo. 1,845,713 required one circulation man, one titration man, and two oell mon. Under -3- P**C0000S45 the method dosoribed In the above-mentioned applioation only one circulation nan and one cell man are required to control operation of the same tank room. ./iiliam J. Knox, Jr. Subscribed and sworn to before me this of Deoember, 1939. day Notary Public -4- ptiXC- OOOO 8^b