# Transcript of Record — Dow Co. v. Halliburton Co. > Briefs, arguments, decisions, and more. URL: https://www.frixlaw.com/law-library/documents/brief%3Amicro_IA40386404_0119%3A01 ## Record - **Collection:** Supreme Court brief - **Document type:** Transcript of Record - **Published:** January 1, 1945 - **Citation:** 324 U.S. 320 ## Text Vol. I TRANSCRIPT OF RECORD (Pages 1 to 500) Supreme Court of the United States OCTOBER TERM, 1944 No. 50 THE DOW CHEMICAL COMPANY, PETITIONER, vs. HALLIBURTON OIL WELL CEMENTING COMPANY No. 61 HALLIBURTON OIL WELL CEMENTING COMPANY, PETITIONER, vs. THE DOW CHEMICAL COMPANY ON WRITS OF CERTIORARI TO THE UNITED STATES CIRCUIT CUURT OF APPEALS FOR THE SIXTH CIRCUIT (APRIL ©, 1944. PETITIONS FOR CERTIORARI FILED /APRIL iv. 1944. CERTIORARI GRANTED MAY 15, 19414. Supreme Court of the United States OCTOBER TERM, 1944 No. 50 THE DOW CHEMICAL COMPANY, a Corporation, Petitioner, VS. HALLIBURTON OIL WELL CEMENTING COMPANY, a Corporation, Respondent. TRANSCRIPT OF RECORD On Petition for Writ of Certiorari to the United States Circuit Court of Appeals for the Sixth Circuit Volume I—Pages 1 to 500 WILser OweEN, 1601 Nicholas Building, Tolede, Obio, Catvin A. CAMPPELL, The Dow Chemical Company, Midland, Michigan, RusseLt WILEs, Board of Trade Bldg., Chicago, Illinois, Donatp L. Conner, The Dow Chemical Company, Midland, Michigan, Attorneys for Petitioner. Kart Bapscock, Duyean, Oklahoma, Leowfhp S. Lyon, S11 West 7th Street, Los Angeles, California, Attorneys for Respondent, IN THE UNITED STATES CIRCUIT COURT OF APPEALS FOR THE SIXTH CIROUIT Tue Dow CHemicat Company, a CORPORATION, Plaintiff-A ppellant, vs. Hauursurton Om Wei Cementine Company, a CoRPORATION, Defendant-A ppellee. Appeal from the United States District Court for the Eastern District of Michigan, Northern Division Cavin A. CAMPBELL, The Dow Chemical Company, Midland, Michigan, Attorney for Plaintiff. Wiser Owen, 1601 Nicholas Building, Toledo, Ohio, Russet, Wigs, Board of Trade Bldg.; Chicago, Illinois, Dowatp L. Conner, The Dow Chemical Company, Midland, Michigan, Of Counsel for Plawmtiff. Eart Bascock, Duncan, Oklahoma, Attorney for Defendant. ~ Laonagp S. Lrox, 811 West 7th Sireet, Los les, California, Of Cownsel for Defendant. INDEX TO VOLUMES I, Il AND III ; Pages CI, 5 ok cco ccaveneetesccecctvacerdsccrecteeotuses 2,3 Bepended Anawer of DelemGant.« ow. cccccccccvcecsocvcesess 4-12 aa ara dW We euinn @aib dace «wee enw 13 Stipulation re Previous Litigation..................... toaee apa Ce es ca ceeckscanevatcecsunsenedes 1403, 1408, 1425, 1434 Proceedings on Settlement of Findings of Fact............. 1435-1477 NS Cas oo oe suka hac Sus eccdaeoawesuvenceksuaran 1478-1491 CE EM ca cacehessesu ee cas webs 0 ox oteen ee bate 1492 CN oe es waaeeke we wes Caan eand keee sna ceeeee wee 1492-1493 es nc Cavece near spe doncecd veces seeds Renee 1494 Ce I ace Nas aeatadetawes san eee 1494-1495 Stipulation Eutemding Time. .... «2005 .y% cuscccccseccveesss 1496 Statement of Points on Which Appellant Will Rely......... 1497-1500 Stipulation Approving Printed Record on Appeal........... 2048 Pra Facte WITNESSES Direct Cross Redirect Recross 300 PROCEEDINGS IN UNITED STATES CIRCUIT COURT OF APPEALS—SIXTH CIRCUIT 159 PAGB Entry—Cause Argued and Submitted.............. 2051 NS co nexewendaeh dais vote cones ecucanoren tases 2051 ME SUGLOLA GS, che bunk de eovucsenewenatetiecee. 2052 PS Se A cr cecSvasseanesevees sees 2061 Order Denying Petition for Rehearing.............. 2077 Maerk’s Cortifieata N77 ; patie 2, 134 Orders allowing certiorari 2OTS Miller, H. C. (Stipulation).... 935-239 TAR icwotas, Carl A... .. ceccccels 263 283 283 Penhaligen, Chas. ............ 160 163 i. SB ee eee 501 614 794, 837 833, 843 Putnam, Sherman W......... » 143 150 Rebbeck, James W............ 43 6 Shelley, Paul G............... 286 295 300 300 Steelman, Joseph F............ 301 304 Verser, Joe Kinnard.......... 258 iv Derense WITNESSES Direct Cross I gr ee RS ce 8 AT 1061 1063 Colley, Robert H.............. 1053 A ee ane ae 896 947 I eat uit esc aee 1040 1048 | ae mises 853 869 i tery =a cae 1076 Knappen, Russell S............ 1077 1082 (Stipulation ) Knappen, Russell S............ 1090 1099 McKain, Bessie G............. 1054 1055 Neubauer, John J............. 1057 1059 Nichols, Howard M.......;:.... 1030 1034 Pes OND Wisk sce ccavwewcae 1902 1006 Spruance, Frank Palin........ 989 997 Thomas, William A............ 1010 1028 Wescott, Blaine B............. 1110 1122 WM I EA ob vcd a ce cas cae 1065 8069 ResuttaL WITNESSES Direct Cross Alquist, Francis N............ 1359 Blum, Edward D. (Stipulation).1161 Crampton, Fred .............. 1290 1291 Dougherty, Chas. I............ 1195 1213 Riga SO ee te 1166 1182 eee re 1300 1307 Luman, Edw. D. (Stipulation) .1156 Poffenberger, Ira N........... 1409 1413 i. at |. 2 JER een eee 1130 1151 Rebbeck, James W........... 1320 1338 Sprenger, Walter ............ 1256 1273 Staggs, Horace M............. 1158 (Stipulation) wee, See ee ee 1298 1299 Weygandt, Arthur S.......... 1201 Wolmer, Clifford FE............ 1295 1297 Redirect 1051 1089, 1090 1109 1039 1007 1001 1074 Redirect 1250 1194 1314 1418 1357 1289 Recross 1052 1090 1109 1001 1074 Reeross 1254 v INDEX TO EXHIBITS Puarntirr’s ExHIsits z Exhibit Pages ; Number Identified Printed , 1 Grebe-Sanford patent in suit 1 877 04 15 1501 2 Grebe patent 1,916,122.............. 15 1504 3 Grebe- gy toesser ‘patent 1,998,756...... 15 1509 4 Chamberlain patent 2,024, | eRe 15 1512 7 Bureau of Mines Bulletin 148........ 29 Vol. I, 29 9 Chart of patent ap he sled involving use of acid in wells, filed from 1866 2 BESS A eee 63 1515 9% Revision of Exhibit 9............... 80 1516 10 Chart entitled ‘‘Streams of Knowl- See EES Re eee 65 1517 10% Prior Art Patents and Publications. . 1518-88 Sherwood 3 65 1518 Roberts 59,936 kes sin as 46 1521 Dickey See 47 1525 Roberts | eer ee 49 1528 Looney eee 66 1530 Aiken are 86 1531 Ball See 70 1533 Mitchell Se 50 1537 Dunn Es os Nos vcuecs 50 1541 Muehl DIETS 9 6acdu'c Chua 71 1546 Lake et al. =: 11,498,045. ........... 73 1549 Tilton 1,608,869. ........... 74 1552 Atkinson 1, NT coca oe 53 1558 Ranney et al. 1,806,499 Po. Ue 75 1565 . Bowman IDS sas vba se0s 77 1570 33 Young EE cna «0% ees 55 1575 British Patent 158,768. ........... 94 1578 Millon article (1845).............. 83 1581 Conroy article (1901)............. 87 1584 Watts article (1912).............. 89 1587 Corbett article (1918)............. 98 1588 4 12 Summary of Dow Shipments of acid : 3 with inhibitors February 11 to Novem- 4 Oe we EE eee aia k nebessacsse's 118 1591-96 . = 13 Letters, dated June 13, 1932, to Jan- 4 uary 19, 1933, from oil industry inquir- % ing about new Dow process of acid x treatments for oil wells.............. 148 1597-1625 4 14. ~=Item in Midland paper regarding new hs Dow well treating process, dated June J Dy asst cacs vet lecvstesnevess: 148 1626 vi PLAINTIFF’s Exutsits Exhibit Pages Number Identified Printed 19 First invoice of defendant for acidiz- ing well, dated March 11, 1935........ 248 1627 20. Second invoice of defendant for acidiz- ~ ing well, dated May 25, 1935......... 248 1628 21 Third invoice of defendant fer acidiz- ing Well, dated May 25, 1935......... 248 1628 23 Purchase order from Erle P. Hallibur- ton, Ine;-dated 5/21/34, for acid treat- ment of well by Dowell, Ine........... 250 1629 26 Ditto, dated October 24, 1934........ 250 1630 27 Bulk material sales receipt for 1,000 gal. Dowell X acid delivered by Dowell Inc., to Erle P. Halliburton, Inc., dated November 9, 1934................... 250 1631 31 Agreement dated March 15, 1934, for acidizing two wells by Dowell, Inc., . for Steen Drilling, Ine............... 251 1632 34 Agreement dated April 20, 1934, for acidizing ten wells by Dowell, Inc., for Steen Drilling, Ine., or Erle P. Halli- fog a pa Mo RE EP CARP eg ey 251 1635 38 Order from Steen Drilling, Ine., dated ° ‘ 3/15/34, for acid treatment by Dowell, EE eT ee a 25 1639 40 eutte, Gated G/37/94......... oce.. 254 1639 43 Ditto, dated 4/20/34................ 254 1640 46 Purchase order from Erle P. Hallibur- ton, Ine., dated 5/9/34, for 2.000 gal. acid job by Dowell, Ine............... 254 1640 o2 Receipt, dated 7/10/34, for well treat- ment performed by Dowell, Inc., for Erle P. Halliburton, Inc............. 25 1641 54 Ditto,, dated 7/24/34................ 254 1642 57 Ditto, dated 8/15/34................ 25 1643 59 Ditto, dated 9/16/34................ 254 1644 60 Purchase order from Steen Drilling, Ine., dated 9/16/34, ‘for 1,500 gal. acid job by Dowell, Inc...°........... 1... 254 3 41645 62 Receipt, dated 10 /24 /34, for well treat- ment performed by Dowell, Ine., for irle P. Halliburton, Ine............. 254 1646 64 Ditto, dated 11/14/34............... 254 1647 66 Ditto, dated 12/19/34............... 25 1648 67 Stipulation re testimony of R. FE. cechaie a, «4, aT Oe CIOL Oe EES 213 Vol. I, 213 68 Stipulation re testimony of H. C. Mil a Aa Ree ie MI NT id iy 235 Vol. T, 235 All exhibits are printed in Volume TV unless otherwise indicated. . , “~ a ee wrk ia Se i dere Exhibit Number 71 93 94 159 vil PLAINTIFF’s EXHIBITs Pages Identified Printed Sketches of defendant’s truck tank... 262 Article in Oil City Derrick of October 10, 1895, entitled ‘‘A Great Discov- ery,”’ reporting acid treatment of well by Frasch and Van Dyke.........--. 1194A Table of Dowell, Inc., statistics show- ing growth from November 16, 1932, to 1940, inelusive. (See also Plain- tiff's Bixhibit 262.) .....-cccesceseess 161 Well completion data Greendale (Michigan) oil field............-+--- 168 Carnegie Library Card cataloging available issues of Oil City Derrick... 11944 Item in Oil City Derrick for October 98, 1895, reporting acid treatment of wells by Frasch and Van Dyke....... 1194A Ditto, for November 9, 1895......... 11944 Ditto, for January 15, 1896.......... 194A Ditto, for February 20, 1896.......-. 1194A Ditto, for February 22, 1896......... 194A Ditto, for March 26, 1896............ 194A Ditto, for August 10, 1897........... 1194A Stipulation re Williams Bros. record... 15 Gypsy Oil Company correspondence and reports re removal of ‘*Gyp’’ scale and prevention of formation of ‘*Gyp”’ in oil wells of the Glenpool, Okla., SN fe acceacreVaaweedda cans bie ene. 1087 Bartell Table showing results of cor- rosion tests with defendant's truck (treating) acids on strap iron test DIOGO oe ccuccdexsarsseaseen ce seedweny 329 Ditto, showing results on test pieces of oil well pipe from National Supply Ditto, showing results on test pieces “ of oil well pipe from Oil Well Supply Re ee ae een ani y cad. Ditto, showin® results on test pieces of oil well pipe from Atha Supply Co.. 334 Bartell Table showing results of cor- rosion tests with defendant’s storage acids on strap iron test pieces........ 545 Ditto, showing results on test pieces of oil well pipe from National Supply Oe seri wasnvcecexceehis coir Corre 345 1649 1651-54 1655 Vol. 1, 168 1656 1656 1657 1658 1659 1661 1661 1663 Vol. 1,18 1664-1704 1710 All exhibits are printed in Volume TV unless otherwise indicated. Vili PLAINTIFF’s EXHIBITS Exhibit Pages Number Identified Printed - 160 Bartell Table showing analyses of de- fendant’s truck (treating) acid sam- SOG ied cue dond cote eeeb es wee aaeens 376 1711 161 Bartell Table showing analyses of acid samples taken from defendant’s stor- ON SHRINE: oc vvkne cs cate enrn teak aces 378 1712 162 Bartell Table showing analyses of acid aamples taken from defendant’s stor- age tanks and diluted to strength of defendant’s truck (treating) acid sam- ee eerie sictie = (ete Aca Waar 379 1712 163 Bartell Table showing content of cop- ¢ per, lead and iron in acid used by de- fendant in treating Zahn well, and same as to acid from defendant’s stor- SG ROME 5 os Sia he oe ee ek 380 1713 Bartell Table showing content of cop- r, lead and iron in acid used by de- idant in treating Stella Wilcox , and same as to acid from defend- PUGntty GUNES nino d60 coe ctess ss 383 1714 165 Barthll Table showing content of cop- 164 idee eta tise nue kek ahs es 384 1715 166 | Bartéll Table showing results of cor- \ rosion tests using ¢. p. (chemically pure) hydrochloric acid solution con- taining different amounts of copper, NE WN is nb ns ca veccccurns B.. 394 1716 167 Bartel! Table showing effect of agita- tion and inereased quantity of acid op corrosiveness of acid solutions con- taining different amounts of copper, NO BN ISS clic cence kav cheeses 6: 407 1719 169 Bartell Table showing amounts of cop- per, lead and iron in defendant’s truck (treating) tank acids and storage tank Re Sr a8 Bree mae Wyaar ey my ie 424 1720 170 Bartell’s chart showing effect of add- ing copper, lead and iron to 15.1% e. p. WYGTOOMMOTEC BCI 2... occ ceeccec cess 428 1721 Pe eo et ey All exhibits are printed in Volume IV unless otherwise indicated. ix PLaInTIFF’s EXHIBITS Exhibit Pages Number Identified Printed 171 Bartell Table showing percentage re- duction in corrosiveness of hydro- chloric acid resulting from addition of different inhibitors named in Grebe- Banter MORE ode ck ccc i cesssciess 451 1723 172 Data showing dates when samples of defendant’s treating and storage acids Le were taken by plaintiff and dates of ; receipt of acid by defendant......... 494 1724 173A Prutton Table showing results of small scale tests of corrosiveness of hydrochloric acid containing different amounts of iron, lead and copper..... 516 1726 173B Table comparing results of some of tests shown in Exhibit 173A......... 516 1727 yp 8 RR ie ae CR ra A SAE aioe on Aya ee 516 1727 173D Ditto, and description of tests, mate- rials and equipment used and explana- IN i ko ns he dco 3 oe ce wses te 516 1728-33 176 Prutton Table showing amount of iron dissolved from Series 1 oil well tub- ing in large scale Run 1A using 15% ee Bein kk ee ae a 508 1734 177 BO MD BRIN cock vxscccosues ces 515 1735 178 Ditto re Run 2A using Series 2 tubing 515 1736 179 Ditto re Run 2C using Series 2 tubing 515 1737 180 Ditto re Run 1B using Series 1 tubing and 15% commercial HCl] containing small amounts of copper, lead and iron Ss 5 va eek ease tne vcs cateess 517 1738 181 Ditto re Run 2B. Similar to Run 1B, but with Series 2 tubing............. 517 1739 182. Ditto re Run 2D. Similar to Run 2B, but with different amounts of copper, NY WE I og va cscs sehen sccccs 517 1740 183 Ditto re Run 2E. Similar to Run 2B, but with different amounts of copper, EE I oo y cue aa eats 517 1741 184 Prutton’s summary and conclusions with respect to runs in Exhibits 176- eet ee rae foal hie css oan Casa os 534 1742-45 185 Prutton Tables showing results of Runs 1M, 1N, 2M and 2N, using com- mercial acid from specia! tank embody- ing features of defendant’s truck tanks 537 1746-49 Sketch showing equipment used in Runs 1M, 1N, 2M and 2N............ 537 1751 All exhibits are printed in Volume TV unless otherwise indicated. Exhibit Number 186 187 188 189 205 216 218A-218D 219, 220 998 -- 231A-231J 232 233 x PuaIntTiFF’s ExHIBITs Pages Identified Printed Defendant’s booklet re Howco method 587 Prutton graph showing results of runs of Exhibits 176-183................. 602 Prutton graph comparing results of Runs 1M, 1N, 2M and 2N (Exhibit 185) with average of Runs 1A, 144A, 2A and 2C (Exhibits 176-179)........ 604 Prutton graph showing results of tests of 15% ¢. p. hydrochloric acid with different added amounts of copper, SE I ice sh oeas Cast ee teens 605 History of oil development in lime- stone fields prior to 1932 and history of acidizing in those fields beginning in 19232, prepared by the witness Fitz- OO alr sre tka scat ss Gas Sk ales. ose 178 Item from Montana Oil & Mining Journal for January 26, 1935, report- ing increase of production in Pondera (Montana) field, due to acidizing..... 186 Bulletin of Montana Oil Conservation RPE BAA Ce ea en Oe 189 Letter, Dow Co. to Oil Makers, 9-25-32.1171 Letter, Grasselli to Oil Makers, 10-14- RA RS Sara bare ek elegy De Ae 1174 Letter, Grasselli to Oil Makers, 11-1- Be eon eeuede eke Ceasdew ea heties 1175 Letter, Grasselli to Oil Makers, 1-26- Be ocd ae see cc aan ware ek 1176 Letter, Grasselli to Oil Makers, 9-15- Be ee eee sae ale hol Pee coe ak 1179 Letter, Oil Makers to Grasselli, 10-8- chao ek bares oie cas So eu eet 1179 Oil Makers checks to Penn. Salt Co.. .1196 Letter, Lee to Oil Makers, 2-7-3383... ..1243 Pages from notebook kept by the wit- NE IN so ens occ caeen ys 1257 Photograph of standing valve and WE FI ho ode ch eae cece aekx 1268 Letter, Prutton to Rebbeck, 1-28-41... 799 Dow Company’s records of shipments of acid to Pure Oil Company during period from February to May, inclu- ae SRE TNR penn ey Sa Sk ee 149 Table supplementing Exhibit 94...... 845 Summary of well treatments made by licensees of Dow other than Dowell... 845 Vol. II, 587 1752 1753 1755-70 1770 Vol. I, 187 Vol. ITT, 1172 Vol. ITT, 1174 Vol. ITT, 1175 Vol. ITT, 1178 Vol. ITT, 1179 Vol. ITT, 1180 Vol. ITT, 1196 Vol. ITT, 1242 1772-74 1775 1776 1777-86 1787 1788 All exhibits are printed in Volume TV unless otherwise indicated. vat * © seacetet aa Lac Fao a eee, Dee xi Puarntirr’s ExHIsBITs Exhibit Pages Number Identified Printed 234 Sketch and data prepared by Dr. Prutton showing rates of attack on oil well tubing of 15% c. p. hydrochloric acid and of 15% synthetic defendant’s | RS er ee 840 1789 242 Dowell advertisement in Petroleum World, September, 1938............. 846 1790 243 Ditto for January, 1939............. 847 1791 245 Dowell, Inc., Service Price Schedule ee ee OO os swe bape se 852 1792 246 Record of shipments of hydrochloric acid and arsenic inhibitor by Dow Company for period January to June, eR Oe el a ee 121 1793 305 Affidavit of Robert Quinlan on the first treatment of a Pure Oil Company well with inhibited hydrochloric acid. .1028 1794 328 Table showing results of acid treat- ments of gas wells by Dowell, Inc., prepared by the witness Lyons....... 191 1796 329 Ditto, showing additional treatments ii rabesceuvny aces 193 1797 330 Table showing time acid was in tubing in each of 122 acid treatments made by Dowell in Kansas from March to Sep- tember, 1936, in 97 consecutive Ar- buckle dolomite wells................ 197 1798 331 Data showing average time acid was in tubing in making the 122 treatments itemized in Exhibit 330.............. 197 1799 337 Chart showing combinations possible under claims of Gravel] Patent SE ee 1320 1800 343 Alquist Table showing rate of corro- sion of mild steel in various concen- trations of hydrochloric acid......... 1365 1801 Charts forming part of Exhibit 343. . .1365 1802-03 344 Alquist Table showing acceleration of the rate of corrosion of hydrochloric acid containing an acid regulator caused by the addition of tin, cobalt i ea Ia ae a a 1370 1804 Chart forming part of Exhibit 344... .1370 1805 347 Table supplementing Plaintiff's Ex- ee ca aces can gs¥esecee ss 1404 1806 348 Table showing treatments by Dow licensees other than Dowell.......... 1404 1807 All exhibits are printed in Volume TV unless otherwise indicated. 356 3957 308 360 362 363 364 366 xii PuiaintiFr’s Exursirs P age Identified Printed Table showing summary of royalty charged by Dow Company to licensees. 1404 Table showing quantities of inhibited acid and other materials used by WO Be oo esaeteo ee 1405 Graph illustrating data in Exhibit Se chine} uectacwehnanat one ee 1407 Acidizing orders, tickets and other data from defendant’s files relating to wells at which plaintiff secured sam- ples of defendant’s truck (treating) MONE Sic kanevensssvedkuanaehedaaacus 1406 Dowell advertising data for years 1932 OD FE nance lec canaacenauese eerie 1407 Photograph of one-half gallon con- tainer used in Alquist’s tests, and WN. os ahama senayen ened pasemians teed 1376 ~ Photographs of 10-gallon drum and of equipment used by Alquist in making tests, and tables and graphs showing Wome OF OT SOME. io oko ccs eee 1380 Table, graphs and drawing of equip- ment used by Alquist in making tests showing loss of strength of 15% hy- drochloric acid when in contact with iron for different periods up to 24 i Rt OPN Mae tater REE, uct, 1398 Bartell Table showing summary of corrosion tests of various commercial hydrochloric acids of 15.1% strength... 499 Table showing Dowell advertising 1932 Ob Ti, BOOMING. Soci ac her ee 1408 Poffenberger’s report on acid treat- ment of Dow Company’s brine well WG Ae cea inseec ul eee ee 1418 Poffenberger’s report on acid treat- ment of Dow Company’s brine well DT ag cv csketuedtuedidedsetuen 1418 Poffenberger’s report on tests of in- hibiting value of arsenic compounds in hydrochloric acid................. 1423 Carr and Humphrey patent applica- tion for method for increasing fluid production from oil wells............ 1427 1808 1809 18105 1911-24 1825 1827-29 1830-40 1841-46 1847 1848 1842 -53 1855 1857-64 All exhibits are printed in Volume IV unless otherwise indicated. J ri . Number Exhibit 367 368 370 105 eee PuaIntTirF’s ExHIBITs Identified Printed a Carre and Humphrey patent applica- tion on chemical reagent fer use in of elk: co oc cance bvanseacens tes wevs 1428 Carr and Humphrey patent applica- tion for method for igtroducing acid reagents into’ oil wells by gas pres- ein ce ese cededduue ae we hu aee 1428 Agreement between The Dow Chemical Company and The Pure Oil Company dated January 31, 1933.............. 1428 Agreement between The Dow Chemical Company and The Pure Oil Company dated June DD, IGGs...... ccc ccwccsss 1428 DeEFENDANT’s EXHIBITS Excerpts from article by R. Van A. Mills, dated December, 1923, entitled ‘‘The Paraffin Problem in Oil Wells’’. 35 Letter from M. G. Harper to J. W. Van Dyke, dated December 5, 1895. . .1033 Telegram, Harmon to Van Dyke, dated January 24, 1896............-. 1033 Memo from C. F. Lufkin to Van Dyke, ee SS aR ee ee eee Prey 1033 Telegram, J. C. Donnell to Van Dyke, dated November 25, 1895............ Telegram, Harper to Van Dyke, dated December 6, TENG. oc. cccacsccspacess Letter, The Grassel!i Chemical Com- pany to Van Dyke, dated July 26, 1899 Letter, Herman (Frasch) to Van Dyke, dated September 22, 1895...... Letter, Harper to Van Dyke, dated ee De, Se eee 1033 Letter, Harper to Van Dyke, dated December 16, 1606. ......,..--2-+5-; 1047 Letter, Ohio Rubber Company to Solar Refining Co., dated September 21, pees en er Ce rope 1047 Letter, Ohio Rubber Company to Solar Refining Co., dated September 25, | Re Pet eine er AR Memo re Crossley Well No. 3 of Ohio RR NE ne ocr cakes we cee 1047 Pages 1864-68 1868-72 1873-77 i877-82 1883 1884 1885 1886 1887 1887 1888 1889 1890 1891 1892 1893 1894 All exhibits are printed in Volume TV unless otherwise indicated. Exhibit Number xiv Derenpant’s ExHIsIts Pages Identified Printed Letter, Harper to Van Dyke, dated OES OOO waa waccctsccceatess 1047 1895 Correspondence between Lufkin, Van Dyke and Donnell re acid treatments (July, 1895, and February, 1896)... .1047 1896 Letter, Lufkin to Van Dyke, dated WO Ee ie hve tanae cues oceu aes o> 1900 Letter, Harper to Van Dyke, dated SRE Ss 6 d's acca nundesaess 1047 1902 Letter, Grasselli Chemical Company to Van Dyke, dated November 21, 1895. . 1903 Letter, Van Dyke to Grasselli Chemi- cal (o., dated November Se ND.» «e's 1904 Memo dated November 2], 1895...... 1905 Letter, Frasch to Van Dyke, undated. 1905 Letter, Grasselli Chemical Co. to Van Dyke, dated July 19, 1895............ 1906 Letter, Lufkin to Van Dyke, dated Au- Oe EG TR gn Pe 1907 Report on scale formation in wells by Blaine Os I Soe ag ee ies da 1081 1908-21 Report by F. W. Karl, dated February 1, 1929; re treatment of William pea, eS Oe eee eee 1087 1922 Same as Plaintiff’s Exhibit 153...... 1087 1664-1704 ea ee 750 ~=—-: Vol. IT, 752 Letter, Robinson to Prutton, 9-12-39.. 769 Vol. II, 769 Letter, Rebbeck to Prutton, 1-24-41.. 771 Vol. II, 772 Letter, Prutton to Rebbeck, 2-19-41.. 774 Vol. IT, 775 Letter, Rebbeck to Prutton, 7-10-41.. 791 Vol. II, 791 Letter, Rebbeck to Prutton, 7-9-41... 792 Vol. II, 791 Letter, Rebbeck to Prutton, 7-9-41... 792 Vol. IT, 793 Letter, Rebbeck to Prutton, 7-11-41.. 792 Vol. II, 793 Hathorn’s chart re tests on hard steel oe SD ad ee nye age GA 854 1924 Hathorn’s chart re tests on hard steel i NPB EIN PCE eared TK SNS 854 1925 Hathorn’s chart re tests on hard steel NE ss bos ne eb eee cee 854 1926 Hathorn’s chart re tests on soft steel gE a RRS Ry RECN) 854 1927 Hathorn’s chart re tests on soft steel ES pe! ad ok ae ne ot) 854 1928 Hathorn’s chart re tests on hard steel tank No. A] SS Sg ge Ee AS LP AIS nt pop 854 1929 Hathorn’s chart re tests on soft steel i ls ook ew ae ete eee 854 1930 All exhibits are printed in Volume IV unless otherwise indicated. haat et teak igs pare laren ako. suai xv DEFENDANT’s EXHIBITS _ Exhibit - Pages Number Identified Printed 287 Index for Hathorn’s corrosion experi- ee ee iad ale an aah aie 855 1931 288 Photograph of Hathorn’s hard steel I a a ws 855 1932 289 Photograph of Hathorn’s soft steel ES Sd ae le a oa ge sae 855 1933 294 og Sd eee 912 1935-88 I calcweeeédee ce 68 1935 Laverty 856, Dee aes SPSS a 913 1939 caches 914. he eo ou eu vig 915 1941 * Gravell 1,398,507 Be ate oe 1943 NE EE oc ccc wcwccececes 916 1945 SE RED 4 oc vawececcecs 95, 897 1947 Gravell and Douty 1,678,776....... 1950 Fischer et al. 1,736,282............ 917 1954 BUN IIE oa os nc ccucccccesse 918 1957 IE os cc ccouhice vers 920 1961 AE I i cob ce lew dee eas 920 1964 Harrison. ee 921 1968 ee ee Re ay 0S 921 1971 Lawrence 1,780,594 ............... 922 1974 Lawrence 1,760,506 .......5....0.. 1976 NE UIE o's do in cic bic acce sc 923 1978 ND NID 5. dow vo oo cio'd noes es 9223 1980 RO IEE Og oc cha dcacoccs os 923 1985 Se oD wacwsecsecee 76 1988 300 Memorandum given by Grebe to de- fendant’s witness Thomas........... 1012 1993 301 Letter, C. Plummer to The Dow Chem- ical Company, dated December 1, 1932.1016 1994-97 302 Memorandum of conversation with Ross T. Sanford, dated December 8, TSE Gaeta a aa cae 1016 1998-99 303 Memorandum of conversation with John J. Grebe, dated December 8, : Ta et re red 1023 2000-02 304 Preliminary draft of patent applica- tien of John J. Grebe, dated June 7, ce ree aces 6c. 1025 2002-09 312 File history of Grebe and Sanford pat- WR TI oon csc uccvcucescccecs: 2010-46 314 Conception data sheet signed by John OS SL See ee 2047 All exhibits are printed in Volume IV unless otherwise indicated. bitRy pee IN THE United States District Court EASTERN DISTRICT OF MICHIGAN - NORTHERN DIVISION Pleadings and proceedings before the HonoraJe Arthur J. Tuttle, Judge of the United States District Court for the Eastern District of Michigan, in the following entitled cause : )- - No. 45 ] Tue Dow CHemicaL Company, a CORPORATION, : Plaintiff. ‘ vs. 3 Hauursurton Or WeLL CEMENTING COMPANY, A CoRPORATION, : Defendant. ; ij ; & 2 Complaint COMPLAINT (Filed June 15, 1939) (1) This is an action for infringement of United States Letters Patent. (2) Jurisdiction is founded on the Patent Laws of the United States. (3) Plaintiff is a corporation created and existing under the laws of the State of Michigan, and has a principal place of business at Midland, Michigan. (4) Defendant is a corporation created and existing under the laws of.the State of Delaware, having a principal place of business at Duncan, Okla., licensed to do business in the State of Michigan, and having a regular and estab- lished place of business at Mt. Pleasant, Isabella County, Michigan, within the Eastern District of Michigan, North- ern Division, where, and elsewhere, it has committed the acts herein complained of. (5) Letters Patent of the United States were duly and regularly issued to plaintiff as follows: No. 1,877,504, on September 13, 1932, for ‘‘Treatment of Deep Wells,’’ as assignee of John J. Grebe and Ross T. Sanford, both of Midland, Michigan. (Here are listed three other patents that are not in- volved in the appeal, viz., Grebe 1,916,122, for Method of Treating Wells with Acid; Grebe and Stoesser 1,998,756, for Treatment of Deep Wells, and Chamberlain 2,024,718, for Treatment of Weils.) Proffert of said Letters Patent, or duly certified copies thereof, is hereby made. (6) Since the dates of issuance of said Letters Patent plaintiff has been and still is the owner thereof. (7) Letters Patent No. 1,877,504, aforesaid, were held valid and infringed by the United States Circuit Court of Appeals for the Tenth Circuit, in the case of The Dow Chemical Company vs. Williams Brothers Well Treating Corporation. (81 Fed. 2d 495.) VP Ri OS ’ 3 ~~ yr % 6 C Amended Answer of Defendant inventors of the Letters Patent in suit, and wholly uysup- ported by any invention disclosed by the patents in suit. 11. Defendant avers that it is not using any invention claimed, or even disclosed, by any of the Letters Patent in suit. On the contrary, defendant is utilizing methods de- veloped or designed by others than the patentees in the patents in suit. Defendant is utilizing, among others, meth- ods described and covered by the following Letters Patent of the United States issued to defendant as assignee: No. 2,122,483, Paul L. Menaul, July 5, 1938, ‘‘ Methods and Means for Acidizing Wells”’; No. %,149,617, Paul L. Menaul, March 7, 1939, ‘‘ Meth- ods and Apparatus for Handling Acidie Solutions.”’ 12. Defendant avers upon information and belief that the Letters Patent in suit, and particularly the claims thereof herein charged to be infringed, and each of them were so restricted and limited in secpe by the procedure in the Patent Office prior to the issuance of said Letters Patent that such claims, and each of them, if valid at all, are not entitled to a construction which will include or cover any device, composition of matter or process made, sold, used or practiced by defendant; wherefore, defendant de- nies infringement of any of the claims of said Letters Patent. 13. Defendant avers upon information and belief that the claims of the Letters Patent in suit herein charged to be infringed cover mere aggregations or old combinations of method steps and riot new patentable methods and are, therefore, invalid under the law. 14. Defendant alleges upon information and _ belief that the claims of the Letters Patent in suit herein charged to be infringed distinguish over the prior art existing at the time of the alleged inventions only by the substitution of known equivalent steps in the methods of the prior art. 15. Defendant alleges upon information and _ belief that the patentees of Letters Patent 1,877,504 in suit sur- reptitiously and unjustly cbtained the patent for things which are in fact the invention of W. A. Thomas of Sagi- DP TEL Es SE yawee ie oie nd 7 Amended Answer of Defendant naw, Michigan, now of Mt. Pleasant, Michigan, who was using reasonable diligence in adapting and perfecting the same. 16. Defendant avers upon information and belief that the claims of Letters Patent 1,877,504, charged to be in- fringed by this defendant, are inivalid and void and of no effect for the following reasons: (a) That the methods desgribe -d and claimed in each of said claims, respectively, ot materia! and substantial parts thereof, were patented or tteseribed in printed publi- cations prior to the alleged invention or discovery thereof by the patentees of the patent in suit, or more than two years prior to their application for Letters Patent therefor, as follows: United States Letters Patent Number Patentee Date of Issue 288,150 B. F. Aiken, Jr. Nov. 6, 1883 372,154 A. Krause Oct. 25, 1887 556,651 J. W. Van Dyke March 17, 1896 556,669 Herman Frasch March 17, 1896 670,577 G. L. Ball March 26, 1901 856,644 C. E. Laverty June 11, 1907 914,916 J. C. Beneker March 9, 1909 1,194,542 N. H. Raymond Aug. 15, 1916 1,221,735 A. F. Hoffman, et al April 3, 1917 1,325,293 L. S. Hoon Dec. 16, 1919 1,365,141 M. A. Adam Jan. 11, 1921 1,382,337 G. C. Bellis June 21, 1921 1,398,507 J. H. Gravell Nov. 29, 1921 1,399,651 Adolph Pessi Dec. 6, 1921 1,410,827 W. F. Muehl March 28, 1922 1,421,706 R. Van A. Mills July 4, 1922 1,428,085 J. H. Gravell Sept. 5, 1922 1,433,579 Otto Vogel Oct. 31, 1922 1,460,395 Otto Vogel July 3, 1523 1,470,225 Harry N. Holmes Oct. 9, 1923 1,476,747 F. H. Wolever Dec. 11, 1923 Amended Answer of Defendant Number 1,498,045 1,513,371 1,524,435 1,531,173 1,549,411 1,608,709 1,605,869 1,615,121 1,619,835 1,632,833 1,635,500 1,678,775 1,678,776 1,713,653 1,719,167 1,719,650 1,721,389 1,723,923 1,729,097 1,734,990 1,736,282 1,746,677 1,746,678 1,748,494 1,750,651 1,756,311 1,757,829 1,766,902 1,773,953 1,780,594 1,780,595 1,785,513 1,789,805 1,796,839 1,804,078 1,805,052 1,806,499 Patentee F’. W. Lake A. C. Campbell A. F. Hoffman, et al J. D. Brady ~- J. H. Gravell R. Van A. Mills Elvin Tilton M. E. Fyleman B. S. Summers J. H. Gravell H. FE. Potts J. H. Gravell J. H. Gravell J. H. Gravell G. D. Chamberlain G. D. Chamberlain J. H. Gravell J. G. Davidson I. H. Derby A. H. Ackerman Chas. Fischer, Jr. Fred H. Rhodes Fred H. Rhodes Paul I. Murrill James (, Vignos W. L. Semon Viktor Bertleff M. M. Harrison H. P. Corson, et al R. E. Lawrence R. E. Lawrence W. S. Caleott, et al F. D. Burke J. H. Gravell, et al M. W. Baden L. B. Sebrell Leo Ranney, et al Pa Date of Issue June Oct. Jan. March Ang. Nov. Nov. Jan. March June July July July May July July July Aug. Sept. Nov. Nov. Feb. Feb. Feb. March April May June Aug. Nov. Nov. Dec. Jan. March May May May li, 28, 27, 24, 11, 30, 30, 18, 1924 1924 1925 1925 1925 1926 1926 1927 1927 1927 1927 1928 1928 1929 1929 1929 1929 1929 1929 1929 1929 1930 1930 1930 1930 1930 1930 1930 1930 1930 1930 1930 1931 1931 1931 1931 1931 OMS 08 RT FT eee 9 Amended Answer of Defendant Number 1,808,185 1,808,188 1,808,200 1,809,621 1,822,271 1,823,439 1,823,440 1,829,705 1,843,376 1,843,783 1,850,757 1,861,176 1,861,177 1,873,083 1,873,084 1,881,721 1,891,667 1,892,205 1,894,759 163,519 Iron’’; Patentee DD. H. Tomkins @ D. H. Tomkins T. W. Bartram, et al H. P. Corson G. W. Coggeshall Melvin DeGroote Melvin DeGroote J. C. Walker Richard Stusser August Regal S. I. Levy Melvin DeGroote Melvin DeGroote J. C. Walker J. C. Walker J. M. Leaper R. H. Carr Melvin DeGroote Melvin DeGroote Date of Issue June June June June Sept. Sept. Sept. Oct. Feb. Feb. March May May Aug. Aug. Oct. Dee. Dee. Jan. BRITISH LETTERS PATENT Martin FE. Fyleman May PRINTED PUBLICATIONS Builetin 233 of U. S. Bureau of Mines (1925 )entitled ‘* Pro- tection Against Corrosion in Oil & Gas Fields’’; Industrial and Engineering Chemistry, June 1928, Vol. 20, No. 6 pp. 582-587, article entitled ‘‘The Electrochemical Action of Inhibitors in the Acid Solution of Steel and 2, 1931 2, 1931 2, 1931 9, 1931 8, 1931 15, 1931 15, 1951 27, 1931 2, 1932 2, 1932 22, 1932 31, 1932 31, 1932 23, 1932 23, 1932 11, 1932 20, 1932 27, 1932 17, 1933 26, 1921 Petroleum Development & Technology (1926) ‘Corrosion in an Oi] Refinery’? by H. F. Perkins, Port Arthur, Texas, pp. 560-570 and diseussion 479-480. Corrosion—Causes and Prevention--1926, by Frank N. Sheller; : = Amended Answer of Defendant Chemical and Metallurgical Engineering, Vol. 36, No. 9, September, 1929, pp. 539, et seq. ‘Inhibitors as a Means of Reducing Corrosion’’ by E. L. Chappell. Bulletin of Bureau of Mines entitled ‘‘Water Problems in the Northern Part of the Cushing Field, Creek County, Oklahoma’’ by D. P. Wardell, et al., February, 1927; Chemical and Metallurgical Engineering, July, 1927, Vol. 34, No. 7, pp. 421-424, articles entitled ‘Practical Ap- plication of Inhibitors in Pickling Operations”’ by Speller & Chappell, and ‘‘Removing Rust from System with Piping Acid’’ by Speller, et al; Principles of Electrochemistry by Blum and Hogaboom (First Edition) (pages 64-67) ; Bureau of Mines Technical Paper No. 15, (1913), entitled ‘‘An Kiectrolytic Method of Preventing Corrosion of [ron and Steel’’ by J. K. Clement and L. V. Walker and also other patents and printed publications, the names, numbers, dates and authors of which are not at present known to defendant, but which when ascertained defendant prays leave to add hereto. (b) The methods described and claimed in each of the claims of Letters Pateat 1,877,504 in suit do not involve invention over the prior art cited ir paragraph (a) hereof, but represent, at most, the exercise of mere skill in the art. (c) The patentees of Letters Patent 1,877,504, in suit, were not thevriginal and first inventors or discoverers of the things patented thereby, or of any material or sub- stantial part thereof, but prior to the alleged invention thereof by the said patentees of said Letters Patent, the same were, if invention be involved therein, invented by or known to the patentees listed in paragraph (a) hereof, at the addresses given in the Letters Patent and applica- tions involved, and by: Muskegon Oil Corporation, Muskegon, Michigan: Gulf Oil Corporation, Pittsburgh, Pennsylvania, and its subsidiaries; Girasselli Chemical Company, Cleveland, Ohio: Ohio Oil Company, Cleveland, Ohio: 11 Amended Answer of Defendant Solar Refining Company, Lima, Ohio; and American Chemical Paint Company, Ambler, Penn- sylvania, Gulf Oil & Refining Company, Pittsburgh, Penn- sylvania | and also by others not now known to defendant, but which when ascertained, defendant prays leave to add hereto. (d) That prior to the alleged invention by the paten- tee in Letters Patent 1,877,504 in suit, or more than two years prior to the filing of the application for said Letters Patent, the alleged invention thereof had been in public use or on sale in the United States by: Muskegon Oil Corporation, Muskegon, Michigan, at or near Muskegon, Michigan; Gulf Oil Corporation, Pittsburgh, Pennsylvania and its subsidiaries, in or near Lee County, Kentucky; in or near Claiborne Parish, Louisiana; and in various places in Oklahoma; Grasselli Chemical Company, Cleveland, Ohio, at East Chicago, or Grasselli, Indiana; Ohio Oil Company, Cleveland, Ohio, at or near Lima, Ohio and Findlay, Ohio; American Chemical Paint Company, Ambler, Penn- sylvania, at Ambler, Pennsylvania ; Gulf Oil & Refining Company, Pittsburgh, Pennsyl- vania at Homer, Louisiana, and by the patentees listed in paragraph (a) hereof, at the addresses given in their respective patents and applications therefor, end also by others not now known to defendant, but which when ascertained, defendant prays leave to add hereto. (e) That Letters Patent 1,877,504 are invalid and void because granted by the Patent Office through inadvertence, accident or mistake. Defendant alleges that the Primary Examiner was interviewed during the pendency of the ap- plication which matured into Letters Patent 1,877,504, while the Assistant Examiner, who was an expert in the art, was away on his vacation. At this interview the Ex- ¥2 Amended Answer of Defendant — ———_$. —___. uminer was given to undérstand, intentionally or otherwise, that, contrary to the facts, the prior art did not disclose the use of hydrochloric acid for the treatment of oil wells. The Examiner informed counsel, in writing, of this understand- ing. Counsel did not correct the Examiner’s mistaken views, but immediately paid the final fee and had the patent issued, (f) That the invention or discovery purported to be covered by Letters Patent 1,877,504 alleged to have been the joint invention of John J. Grebe and Ross T. Sanford was in fact the sole invention of John J. Grebe only. (g) That the invention or discovery purported to be covered by Letters Patent 1,877,504 alleged to have been the joint invention of John J. Grebe and Ross T. Sanford was in fact the sole invention of Ross T. Sanford only. (h) That the invention or discovery purported to be covered by Letters Patent 1,877,504 alleged to have been the joint invention of John J. Grebe and Ross T. Sanford was in fact the joint invention of John J. Grebe, Ross T. Sanford and W. A. Thomas. (i) That the invention or discovery purported to be covered by Letters Patent 1,877,504 alleged to have been the joint invention of John J. Grebe and Ross T. Sanford was in fact the joint invention of John J. Grebe and W. A. Thomas. (j) That the invention or discovery purported to be covered by Letters Patent 1,877,504 alleged to have been the joint invention of John J. Grebe and Ross T. Sanford was in fact the joint invention of Ross T. Sanford and W. A. Thomas. Wherefore defendant prays that said Letters Patent No. 1,877,504, be declared invalid and of no force or effect ; that defendant be decreed to not infringe the aforesaid Letters Patent; that costs herein be taxed against the plain- tiff; and that the Complaint herein be dismissed, and for such other and different relief as to the cotrt may be just and equitable, 13 Stipulation Re Previous Litigation COUNTERCLAIM The Answer included a Counterelaim based on Gravell Patent 1,678,775, issued July 31, 1928, for storage and transportation of acid mixtures in steel drums, which counterclaim was dismissed and no appeal tuken therefrom. STIPULATION RE PREVIOUS LITIGATION The following stipulation was entered into with re- spect to previous litigation on Grebe and Sanford Patent No. 1,877,504: ‘1. That snit was brought by the Dow Chemical Com- pany vs. Williams Brothers Well Treating Corporation, on or about the 24th day of April, 1934, for the alleged in fringement of United States Patent to Grebe et al., No. 1,877,504. “92 That said suit eame on for trial in the United States District Court for the Northern District of Okla- homa, before the Honorable Judge F. E. Kennamer, during the month of September, 1954. ‘3. That by final decree on or about January 15, 1935, the Bill of Complaint was dismissed. 4. Plaintiff, The Dow Chemical Company, thereupon took an appeal to the United States Cirenit Court of Ap peals for the Tenth Cireuit, which appeal was docketed as No. 1285. 14 Stipulation Re Previous Litigation ‘5. That the decision of the Tenth Circuit Court of Appeals was as reported in 81 Fed. (2d) 495. ‘6. That for the purposes of this stipulation, the transcript of testimony and the copies of exhibits printed in the transcript of record on appeal to said United States Circuit Court of Appeals, for the Tenth Circuit, entitled ‘The Dow Chemical Company, Appellant, vs. Williams Brothers Well Treating Corporation, Appellee,’ shall be considered as being true, complete and correct copies of such testimony and exhibits before the District Court, sub- ject to correction of such copies of exhibits on comparison with originals thereof, should error appear. ‘*7. That if called and sworn to testify as witnesses lerein, the following individuals, L. C. Case W. A. Hower S. C. Kiser R. S. Knappen Harry F. Wright R. L. Wright who gave testimony in the aforesaid case of the Dow Chem- ical Company vs. Williams Brothers Well Treating Corpor- ation, either on examination in open court or by deposition taken out of court, each would testify to the same facts as they testified to in the said’ former cause, subject to correc- tion by any additional testimony of any of said individuals taken on behalf of either party hereto. | ‘*8. That insofar as the same may be relevant to any issue herein, either party hereto may offer as evidence in this cause, any portion of the fact testimony of the above identified witnesses named in paragraph 7 hereof, or any portion or portions of any exhibit offered in the aforesaid Williams Brothers case, with the same force and effect as though such testimony had been taken or exhibits had been offered herein, subject to the right of the opposing party to object to any such offer on any ground that might be urged against it herein, if said witnesses had been sworn and examined, or such exhibit had been offered in this cauge, whether or not such testimuny or exhibit was objected to at the time it was taken or offered in said former cause.’’ a eg Toe ae. 15 Statement of Testimony and Proceedings in District Court NARRATIVE STATEMENT OF TESTIMONY AND PROCEEDINGS IN DISTRICT COURT Following is a statement of the testimony and pro- ceedings in the District Court, portions of which are in narrative form and other portions in question and answer form. The following exhibits were marked and offered: Copy of Grebe-Sanford Patent 1,877,504 as PX-1. Copy of Grebe Patent 1,916,122 as PX-2. Copy of Grebe-Stoesser Patent 1,998,756 as PX-3. Copy of Chamberlain Patent 2,024,718 as PX-4. Copy of Gravel] Patent 1,678,775 as DX-5. JAMES 0. LEWIS, a witness called by plaintiff, testified as follows: DIRECT EXAMINATION I live in Houston, Texas, and am a consulting petro- leum engineer. I got my technical training at the Univer- sity of Stanford where I graduated as a geologist, prepared for petroleum geology. After graduation I spent two vears with the Associated Oil Company in California as a field geologist, and after that I spent three years employed by 16 James O. Lewis Harry R. Johnson of Los Angeles and Robert B. Moran then of San Francisco. My work was partly field geology, concerned with oil, except for one special job of a few months, and also some engineering problems in the produc- tion and valuation of oil, and the drainage of oil under- ground. I then went with the United States Bureau of Mines in the fall of 1914, and was with them for six years. My first position was that of oil and gas inspector, doing joint investigation work for the United States Bureau of Mines, and the Indian agency of Muskogee, Oklahoma. I worked jointly with the Indian office and the United States Bureau of Mines investigating the causes and remedies for the waste of oil and gas which were then taking place in Oklahoma. I was in that work for one year, and I was then employed by the Bureau of Mines directly for two years in investigative work, mainly concerned with methods for in- creasing the recovery of oil; methods for estimating the future production of oil and gas, and other methods for conserving oil and gas. During that time I wrote three technical bulletins and papers for the Bureau of Mines. In 1918 I was placed in charge of the Bureau of Mines Petroleum Experimental Station at Bartlesville, Oklahoma. The station was just being founded. It was the first pe- troleum station of the Bureau of Mines. Also during that year we had outside work—I mean in addition to the or- ganization of the station, in helium problems, which were then active, working out methods for the Bureau of Internal Revenue, for estimating the reserves of oil and gas, to be used in connection with depletion allowance in income taxes, and other activities in Oklahoma, and elsewhere in the United States dealing with conservation. During 1919 and 1920 I was chief petroleum technol- ogist of the Bureau of Mines, that is, I was in charge of all petroleum work of the Bureau of Mines during those two vears, and was located in Washington, D. C. I left the Bureau of Mines in 1920, and went to Marietta, Chio, and hecame a member of the firm of Smith & Dunn. The firm ae Sia a IS ye pt, Wet, CBS one ie Te saa Ce a . YR ESS Pa eae RAE MEE EAST ALE IETS SOT NR ORE AER Pa NS iis Bo Se ERR SSIES ey et ae 17 James O. Lewis of Smith & Dunn had a patented process for increasing the recovery of oil by injecting air or gas into depleted oil fields. In the fall of 1920 I moved to Tulsa, Oklahoma, with Mr. Dunn, and we formed the firm of Dunn & Lewis, which _ was in business together until about a year ago. Mr. Dunn _Was the inventor of this process of increasing the recovery of oil, also other processes for cleaning out wells, and help- ing recovery of oil and gas. Our business there was a gen- eral petroleum engineering business but specializing in methods for recovering oil and gas. We had a number of properties which we took over, some under management, some under ownership, to which we applied this process of Mr. Dunn’s and other processes. We also had consulting work from larger companies, advising on various matters, namely, South Penn, Central, New Jersey, Tidewater, Pe- troleum Gas Company, and some other gas companies. During these vears I have done a great deal.of consulting work on valuation, estimations of oil and gas and various problems relating to the production and recovery of oil and gas. Mostly my work has been on the conditions which exist underground, and the methods for bettering the re- covery of oil and gas therefrom. About a year ago, I dissolved partnership with Mr. Dunn and have been located in Houston, Texas, as a con- sulting engineer in such problems. At present I am en- gaged in a joint problem for a group of companies in Cal- ifornia, one of the largest fields there—the Kettleman North Dome Field—working out problems connected with what is known as the cycling of gas from the very deep sand which should be used by these joint operations. These companies include most of the larger operating companies in California. I also have similar problems on increasing the recovery of oil in some properties of an English com- pany in Trinidad which company happens to be the largest producer of oil of any British-owned colony. Q. Now, I wish you would tell the court, please, what were the actual conditions, we will say, before acidizing 18 James O. Lewis became popular, as to the percentage of the oil in the ground whieh was actually gotten out. Tell them both as to lime stone and sandstone. A. It has always been rather a difficult question to estimate how much oil actually is in the ground, and hard to give general answers in magnitude and figures. Also, there have been changes in the character of fields which haye been fdund at different times and in the methods of producing that oil and gas. In the earlier part of the industry tnost of the oil was produced from what is known as tight sands—they call them sand but really they are sandstones, originally laid down as loose sands but in the course of geological changes have been cemented and the permeability had become quite low. The oil and gas found in them was quite difficult to obtain. While that character of field was being produced, the re- covery was obviously quite low. In 1917 I estimated the average recovery was between 10% and 20%. That is, from 80% to 90% of the oil was being left underground. That was probably a little low. Probably they were getting a little more than that, as we since have found out. It wasn’t very far from the real order of magnitude. Since that time the character of fields has been different. We have been finding more deep fields, more oil has come out from sands, nore permeable, and have made advancements in recovery. So the efficiency of recovery is better, considerably. Prob- ably at the present time the recovery is of the order around 40%. Now, as to the limestones, there is much greater vari- ability in the question of limestohes, and consequently the percentage of extractable oil—probably on the average, the percentage of extractable oil is somewhat higher in lime- stones than it has been in sandstones. That is, instead of it being of the order 20% in the tight sands, so-called in lime- stone, it is more likely to be 30%, possibly a little greater. That was up prior to the extensive use of acid. Q. Now, how long has it been since this increasing of the production of wells was recognized as a real problem to be met by the industry? A. Well, it was almost recug- SOPRA. AEE AES LAIRD NO BB I BS WENGE Sabie aay f = sid aa a i ang 19 James O. Lewis —_—_- nized from the beginning to some extent. That is, the first producers found that the wells would come in in large vol- umes, comparatively large volumes, and then quickly the amount of oil which the well would produce would shrink, so they were almost immediately confronted with the fact of a diminished return following the completion of the well, and became interested in methods which would tend to increase the daily production. They did not so quickly become conscious of the fact that after the well had ceased producing, they had not ex- hausted all the oil, but it was not many years before they commenced to sev that they were not getting all the oil, though jt took quite a long while for them to get a means of estimating quantitatively how much that was. They knew they were losing some of the oil, and it must be a con- siderable quantity. The original first Drake well, the first petroleum well in this ‘country, was in 1859. Q. And how long was it after that before they had some recr~* evidence of efforts to increase the productivity pf the wells? A. Well, from the standpoint of merely in- creasing the daily production of wells, with no respect to whether or not the ultimate production was increased, there are records almost immediately of going in and cleaning out wells. They recognized that the formations wowld cave off the walls of the hole and fill up the hole. They would go in and clean that out. Also they had devices for-lifting the oil by various pumping means. Gas lifts were first applied very early in the industry, at least, tried out, and as soon as a well ceased to flow under its natural pressure, there were many ex- pediencies applied to increase its daily production, ’ Then, in 1865, the first method which went further than that, which went more than merely cleaning out the hole it- self and bettering the lifting means, was applied by Colonel Roberts, who was the colonel in the U. S. Army during the Civil War *ho invented the torpedo, as he called it. That is, his method was to put in a charge of nitroglycerine into the well, explode it there, which would enlarge the hole and crack the formations back from the hole some distance, just 20 James O. Lewis oe - ——-— how far he did not know, and also tend to clean off the walls of the hole of obstructing materials. Mr. Lyon: Your Honor please, it seems to me that from the wit- ness’ last statement, something that happened in the Civil War, judging by the fact he said he was a graduate of Stamford University, and Stamford was not founded until the 90’s, this witness is not testifying to anything of his own knowledge. The Court: I take it this is the recorded history, like who dis- covered the steamboat. Mr. Lyon: It seems to me this is not the proper way to prove it; to prove the history, | mean, by an oral witness. The Court: Well, if it is history, it cannot affect the decision of the lawsuit really. It is just background, and I don’t want him to use up very much of my time or their money in order to prove this. I take it that if he isn’t corrected by some of the people connected with your side he is cor- rect about it. I take this as background and history of an art that goes way back beyond anything I will use in de- ciding the lawsuit, and yet it is interesting. Mr. Wiies: Of course, we want to show that this has been a prob- lem ever since the industry started. The Court: I will let him go ahead, and he will come down to something more recent. By Mr. Wiles, continuing: Q. This process that you have just mentioned as shooting wells, that continued to a considerable extent up to rather recent times, did it not? A. Yes, it has con- tinued right up to the present time, and is still in use. Shooting is not effective in all formations, either in all sandstones or all limestones, but it has favorably affected production, above the rate, and the ultimate recovery in many limestone fields. 21 James O. Lewis Q. Is there a rather localized effect, close to the weli, or can it be extended for a considerable distance? A. We know from measurements of the size of the hole after shooting that it has not enlarged the hole very greatly, tnat is where the hole was originally six to eight inches in diameter, it may enlarge it to some twelve inches, some- thing like twelve inches, and occasionally eighteen inches, but it also cracks the rock, but how far it cracks it I do not know, and I have never heard any figures which would prove how far back it cracks it. The Court: Is there anything about whether or not the fact it might make a well to it,—like where you applied it to the stump out here or a hole in the ground? It doesn’t take it with this rock, as I understand; it tends to split it rather than throw pieces back? A. It can’t throw the rock back because there is no place for it to go, and it can’t blow up because you have the formations holding it down, unless you put in an overcharge, and if you put in an over- charge, of course, it might do damage to the top of the well if the well was shallow. The figures T gave in 1917 were made in view of shooting the wells and the processes of increasing recovery except the use of injected air or gas, and except the use of flooding. In other words, they were for methods used prior to those two processes. The Court: Shooting them would increase it, it helped? A. Oh, yes, very greatly. The Court: What other method did you say besides the shooting of them? A. They used various methods for cleaning out the hole itself, and at a later date in 1869 they applied what is known, what they then called a gas pump which Was a vacuum pump. And, the principle on which they “perated was to remove the atmospheric pressure and per- mit the gases in the rock to expand an additional few pounds. 22 James O. Lewis The Court: You mean pump the air out and make a vacuum? A. There wasn’t any here in the underground, but they made the casing head tight, and connected the pipe to the casing head and applied this suction pump to it. The vacuum has been used up to the present time. The Court: You made your vacuum above. Wouldn” that tend to make that oil come up? A. It would tend to make the oil flow more freely and expand the gas which was in the rock. You see, your oil is flowed from the pores of your producing formation in the wells. The Court (Interposing) : Held under pressure? A. Originally, your oil with the gas in solution is under considerable pressure, and that gas expands and pushes the oil with it to the well from which it is lifted to the surface by either natural flow or various mechanical means. In time your natural gas forces become depleted and become ineffective until finally if you don’t do something to replace these natural forces you wouldn’t have enough force to force your remainug oil to the well. At that stage these old operators would go and put on their vacuum pumps, or gas pumps they then called them, and by removing atmospheric pressure it was the same as if they put into the sand another twelve or thirteen pounds of pressure, because it allowed the gas to expand against that much less pressure, and your gas in expand- ing had atmospheric pressure, which is about 14.7 pounds at sea level, and by using a gas pump you could remove that pressure from it and allow the gas to expand that additional amount. Mr. Wiles: Q. To get some idea of how important this vacuum is in per cent, proportion, what is the urderground pres- sure likely to be like, say, at several thousand feet? A. The underground pressure, that is the original under- ground pressure has an extremely wide range. It is usually in approximate proportion to the depth, and usually it is 23 James O. Lewis about 43 pounds pressure for each 100 feet of depth. That is an approximation which isn’t true, but is generally true, so that the first wells, which were shallow, had original pressures of maybe less than one hundred pounds. In recent years where they have been drilling to great depths wells of ten thousand feet or more they have pressures of five or even six thousand, even seven thousand pounds ini- tial pressure. So that pressure varies with those great ranges in accordance with the depth more than any other factor. Q. In view of those figures, the 15 pounds difference that you can make with a vacuum would be rather insig- nificant, would it not? A. The amount of push which the vacuum or gas pump would make was not large and was negligible in the deeper sands. In some of the shallower sands it was rather important, but it could not be a highly effective process. Q. Now, there is a process known as re-pressuring, is there not? A. Yes. The word ‘‘re-pressuring,’’ I might say, is used in a good many different senses, but in the sense T believe you mean it is the injection of either com- pressed air or compressed gas into a depleted field. That is, instead of what you might say putting a pull on the sand by a gas or vacuum pump you can put a push on it by taking air or gas and compressing it in a compressor, and injecting it into one well and allowing it to flow through the sand into producing wells around it. And, of course, the pressure which you can generate in that man- ner is unlimited, whereas the additional pressure which you release from the sand by a vacuum pump was distinctly limited. The Court: T suppose you have tried to apply your air to some low place in the pool and get it out at a higher place? A. There have been various theories and the theories have been applied very largely in accordance with loeal condi- tions. In some pools it seems to be better to distribute your output and input wells, producing weils as they eall 24 James O. Lewis them, in some structure which seems to be best to put all your gas in the high part, and force your oil down so that the oil will flow with gravity in addition to the aid of your pressure. In other cases they have them put it in at the edge of the pool and forced it up. Generally the best prac- tice, at least a practice which the engineers seem to agree upon, is to put it in the high part of the structure if there is a pronounced depth to the sands. In limestone formations the repressuring systems have not been markedly successful. It has been tried in a good many cases, and it is very seldom successful. The reason seems to be that the pores in your limestones are of a dif- ferent origin, and have a different nature than sands, and your air or gas will, of course, take the lines of least re- sistance, and usually in limestone there are channels of resistance which are so much less than the body of the limestone that your air and gas would pass through, doing very little good. For example, in the Trenton pool, an application I Know of, they injected the air into the formation, and in- stead of that air showing itself about the nearest wells, it followed a line across the field and appeared in wells a distance of a mile away, apparently having followed a frac- ture zone. That seems to be the most logical explanation. The exact conditions we were unable to get any proof of. Q. There are methods also where you add water, are there not? A. Yes, instead of putting in a gas, you can put in a liquid, and practically the only liquid which would be commercially feasible was water. I do not know of any case where it has been very effective. Also, prior to 1931 we used various reamers which would go into the ground and enlarge the drill hole from its six or eight inches to so much as three feet in diameter, that is, ream it out mechanically. That was used to a lim- ited extent, and did some good. It increased production some, but not to a highly important degree. There were also methods for removing the paraffin which would accumulate in the pores; that is, as the well ES GO 25 James O. Lewis gets old, certain oils have paraffin waxes in them, which would separate out; and this paraffin would accumulate in the pores of the sands immediately around the hole and clog it up. There are various treatments for that, such as steaming it’ out, circulating hot oil, putting in chemicals, electrical’ heaters, which would remove the obstruction. That also applied to old holes where mineral matter had been deposited in the pores of the sands and clogged it up. To remove that they have put in light shots, which would erack it off. Q. As far as wells in limestone are concerned, aside from the shooting process which came in, as you said, in 1865, was there any serious method developed that went into practical use to any extent? A. Well, up to acidizing, I don’t recollect any methods which came into general use and were of any importance. Q. When did proration come in? A. The first pro- ration was generally effected about 1926 in Oklahoma and created a special reason for obtaining maximum daily pro- duction from a well. The formulas for prorating the pro- duction of wells were based upon what they call the poten- tial of the well, either wholly or largely. That is, if the well had a capacity to produce, say, one thousand barrels if it were allowed to produee its full quantity, it would be given a higher allowable than a well which, say, could only pro duce five hundred barrels a day. So the incentive on the part of the operator was to put his wells in condition se that they would make the best showing when these poten: tial tests were made. Q. Now during this same time, do you know of pro- cesses for increasing the production of wells which were tried experimentally and abandoned? A. Oh, I used to hear of various methods and ideas of increasing recovery. Of course, it is my business— Mr. Lyon (interposing) : Your Honor please, I con't think we ought, if this evi- dence is going to be used, to receive evidence about what this witness heard, which he characterized as abandoned or experimental. 26 James O. Lewis The Court: If it is something you dispute, I would adhere to that, 1 think. (). Name the methods you know about or which be- came known in the industry so that, as an expert, you would know about it? A. One of them I know of personally was the idea of heating up the rock by either forcing in steam through the producing formation or hot water or some other fluid which would be a conveyor of keat into the rock, the theery being that you thus reduce the viscosity of oil and also you generate gases from the gasoline which was a part of the oil in the rock. The idea was to pump the hot water in through the wells right into the formation. The Court :, li would get cold before it could get down there. A. That is exactly what happened. All ef those methods, how- ever, were tried, and personally I made many, many calcu- lations on them. They all failed Hecause the mass of heat in the rock itself was so great that it was not feasible. (ne plant they tried it and got a good increase, but they ‘ound that putting steam into the ro*k, they found it took all the additicnal oil they recovered and all they produced hefore to raise steam to heat up the rock. The Court: What is the temperature down there a couple of miles? A. When you get down a couple of miles it is likely to be around 250 degrees Fahrenheit. One hundred feet down it will generally be the average surface temperature, which in this (Michigan) climate, if you average the year round temperature is about 45. That is my guess. The Court: You get down a mile and it would be how much? W. Van Dyke. Van Dyke also assigned one-half of his to Herman Frasch. And the drawings are signed by Charles J. Hedrick in both instances. 69 James W. Rebbeck Q. And, isn’t it a fact that the drawings are the same in both instances, and that the specifications are almost word for word in both instances except the Van Dyke re- fers to the use of sulphuric acid and the Frasch patent re- fers to the use of hydrochloric acid? A. That is what I ‘gather from the reading of both these specifications. There are differences in statement as to the chemical effects pro- duced by the two acids, of course, because in the Frasch patent the reaction of acid on the rock is to produce a cal- cium chloride solution out of the rock, whereas the action of the Van Dyke patent employing sulphurie acid is to con- vert the solid limestone into a suspension of calcium sul- phate which can not be forced out of the rock pores. By Mr. Owen: _ Q. Now, will you. take up the next patent on that list? A. There is some of the Frasch specification, perhaps, that differs from the other that might be included. It states that after a rest of, say, twelve hours, milk of lime is pumped down to neutralize any trace of acid that might exist. The well is then cleaned out and the tubing replaced. The Court: That was to check further eating. They had the danger that might come if it kept on eating and ate out into the brine, I suppose? A. I presume that is se. The Court: Does Frasch also describe protecting his metal in the same way? A. The description of that is practically iden- tical with that in the Van Dyke patent, the means of pro- tection being to employ an enameled, lead-lined or rubber- covered pipe, _ The Court: Aren’t there any acids except sulphuri@ and hydro- chlorie acid that will do the trick? Aren’t there some other acids? A. Yes. There are many acids which will form solutions with caleium carbonate. There are a great many that will do that. But, as to how many acids there are which will dissolve oil producing rock is something I am net prepared to answer. 70 James W. Rebbeck The next patent reference on the B side of the chart is « patent to George L. Ball, numbered 670,577, dated 1901, the application being filed in 1900. He makes a disclosure of introducing an acid into a well, and an alkali to react and produce heat. It is similar to Looney. However, this patent discloses also that in order to put the acid in you may em- ploy a dump bailer. The patent states: ‘‘The chemicals may be introduced into the well by dropping or pouring them therein and, as they are heavier than the oil, they sink to the bottom of the well, so that the heat is generated in the cavity where it is required; but the chemicals, or at least the acids, may be put in an ordinary bailer, and lowered into the well and then dumped.’’ By Mr. Owen: Q. Will you explain the operation of these dump bail- ers to which the patent refers? A. I am not well advised in dump bailers. However, it is my understanding that it consists of a length of pipe of such diameter as will enter the well and be capable of being lowered to the bottom, and at the lower extremity of the pipe there is some sort of valve means whereby the contents of the pipe may be emptied when the lower end of it strikes the bottom of the well, by a kind of a trip arrangement. Mr. Lyon: It is just a bucket that you can drop on the bottom of the well and it will then empty its contents. A. (Witness continuing): On the chart there is next shown a 1923 reference of Mills. It is a Bureau of Mines report of investigations, Serial Number 2550, to which Mr. Lewis has made reference in his testimony. It is Exhibit 8. There is a portion of that report that refers to the use of an acid in a well, and my recollection of what I heard from Mr. Lewis is that that portion of this reference has already been read into the record. On page 9 the use of hydro- chloric and sulphuric acid both are mentioned. It describes what we have been finding heretofore in the patents, and in addition this bulletin of the Bureau of Mines also makes this statement with regard to sulphuric acid: i os f i = ee. Se = g. a Ce ay *s on 3 ‘ee 71 James W. Rebbeck ‘*Sulphuric acid should not be used in oil wells because of the danger of plugging the sands with precipitated sul- phate salts, more especially calcium and barium sulphate.”’ The next reference is patent 1,410,827 issued to Wil- liam F. Muebkl, dated 1922, on an application filed 1920. It is for a method of cleaning oil wells. For that method he states that he uses acid. He introduces a suitable acid, such as hydrochloric acid, which will attack calcium silicate and other accumulations, to clean a well— The Court (interrupting) : It’s the same chemical action we have been talking about but he doesn’t seem to be thinking about its going out inland but, more, he thinks this lime from the rock is going to get down in there and into the well proper and he wants to eat that out. Witness continuing: That is true. The use of the acid is more local than in the Frasch or the Van Dyke patents. The Court: Does he say anything about how he does that? A. Yes, he does. In fact, his specification includes a drawing of an apparatus showing a means for getting the acid to the loca- tion where he wants it to work, and it consists of a dump bailer similar to the one previously described, but for the valve in the lower end of the bailer he has provided zine closures, a form of zine disk. And these, of course, are dis- solved by the acid, thereby emptying the bailer after a time. The discs last long enough to permit the acid to be lowered into the well. Regarding the number of discs to be used, the patent states that these can be varied according to the length of time that the acid is to be allowed to remain in the bailer. Quoting from the patent: ‘‘T prefer to use hydro- chlorie acid, which readily attacks zine, and T prefer to have the zine wafers or dises of such thickness that a given time will be required for the acid to eat through each dise. By way of example, each wafer may be designed to resist the acid for five minutes; therefore, if it requires five 72 James W. Rebbeck minutes to lower the receptacle from the top of the well to the point of discharge, one dise will be placed in the bottom of the receptacle. If ten minutes are required, two discs will be used; fifteen minutes, three discs, and so on.’’ Mr. Lyon: I call Your Honor’s attention to the fact in that patent, page 2, line 22, the inventor says: ‘‘The particular ad- vantage of providing the container is that the acid may be applied locally in the well, thereby reducing the quantity to a small portion of that which would be required if it were necessary to pour the acid from the top of the well.’’ So the inventor was deliberately just putting down a bucket- ful of acid and calls attention to that is why he uses a bucket—because he doesn’t want to use as much acid as would be involved pouring it down the pipe. Witness continuing: Another feature about that disclosure is that the size of the bucket which can be introduced is obviously small because he puts it down through the innermost tubing of the well. As to whether there is anything to indicate the charac- ter of the formation in which this invention was intended to be used, I think the disclosure in the specification of the problem that this method was intended to solve indicates that the producing formation would probably be unaffected by the acid because the invention seems to be directed to- wards removing the accumulation of paraffin, calcite or acid-soluvle deposits. The Court: And the amount cf it indicates, as you say, a small amount, so he evidently wasn’t thinking about getting out into the rock formation but getting some accumulation in his well. Mr. Lyon: Page 2, line 17, he refers to the lime or silicon or other accumulations on the side clogging the walls or screen will be relieved of the accumulation, and the oil from the sur- rounding stratum may flow into the well unimpeded. So I 73 James W. Rebbeck don’t see anything in here to say it isn’t a limestone weil, becanse he refers to lime. A. No, I found no reference to lime. It refers to calcium, silicon and other accumulation. Mr. Lyon: You don’t find any reference to lime? I call your at- tention to line 17, page 2 of the patent. A. Yes. But that, of course, taken with the statement on the previous page, as to the deposits which are there, would seem to indicate that he is not talking about the structure of the producing formation. Mr. Lyon: How could there be any lime in that well along the walls if there was not lime in the formation into which the well was dug? A. There is no necessary connection be- tween the existence of lime deposit in the sand well and the producing formation’s composition. Mr. Lyon: ° Well, the lime must come from the formation in the well somewhere. A. That is an assumption. — Mr. Lyon: / What? A. That seems to be an assumption. There is no necessary connection between those facts. The next patent is one issued to Lake and Phelps No. 1,498,045, dated June 30, 1924, on an application filed in 1923. His invention relates to a process of cleaning wells and apparatus therein, and it has for an object a provision of a novel process which readily removes colloidal muds, clays, etc., from the walls of the well hole or from any ap paratus or members within said well hole, and which muds would tend to clog or otherwise obstruct the flow of oil or gas through suck apparatus or well hole. Some acids chemically react with mud, or with clay, depending on the composition of the clay, but in this pro- cess according to the specification as I understand it, the way he states it at any rate, is that the acid solution seems to have greater affinity for the colloidal muds than it has for the metal casing through which the acid is introduced into the well hole. It would appear that the acid would re- 74 James W. Rebbeck act quite readily with this mud, maybe far more, maybe so readily that it does so more actively than it does on the metallic part of the well. Mr. Lyon: Would you read that particular part to the court be- ginning at line 100, because here is a man that says this acid which includes hydrochloric, if handled properly in the pipe will not injure the pipe. A. I don’t gather that from this specification. Mr. Lyon: Read beginning at line 100, will you please? ‘‘It is found that the acid or acids used for these pur- poses will not aj preciably attack the metallic structures in the well hole such as tubing and casing, collars, and the like, where mud is present in the hole, unless used to excess, inasmuch as when an approximate balance between the amount of acid and colloidal mud is maintained, the acid action will be expended upon the mud rather than in -at- tacking the metal.’’ The next patent is Tilton, No. 1,608,869 issued in 1926, on an application filed in 1922, and renewed in 1925. He proposes to generate a heat in a well to melt paraffin using the action of concentrated sulphuric on water followed by a neutralizing sodium hydroxide. The Court: Now, what did he have that was new over Looney and somebody eise? He had that idea of having a chemical re- action creating heat and melting paraffin. A. There is this possible novelty in it, there may be, of the use of a concen- trated sulphurie acid, which, when added to water, liber- ates a large amount of heat, and then after that heat has been obtained he can get a further kind of heat by neutral- izing the acid solution previously formed, using sodium hydroxide for the neutralization. The Court: Did he put thern in separately? A. Yes. iy Mr. Owen: (). What did the patent state or show as to the meth- goinbiy Haig Sua heed ala ‘ e Cask : er id ah as Se ia eI soul Pats 3 . eRe Bi gree #7 ae 2 iS Ne re RT CD SN Es 75 James W. Rebbeck ~ ods used for lowering the acid into the well hole? A. It is my recollection that the container used for this was a lead- lined container. The patent states, beginning with line9 of page 1: ‘‘The acid container proper is an elongated re- ceptable, provided at its lower extremity with a valve dis- gharge orifice 4. The valve for closing the discharge ori- ‘ fice 4 comprises a stem 5, extending through the orifice, sand a head 6 lying within the receptacle. The head 6 of the valve comprises a conical lower portion 7 arranged to fit the wall of the container adjacent the discharge orifice 4, and an upper portion 8, which is shown as conical, but which may be of any desirable rounded or tapered form. ‘*Cooperating with the valve head 6 are a plurality of spheres 9 disposed within the container 1. When the con- tainer is lowered into operative position, the valve stem 5 comes into contact with the bottom of the well and moves upwardly within the container. When the valve head 6 moves upwardly, the spheres 9 run downwardly in the con- tainersand wedge between the conical portion 7 of the valve head and the correspoading inner surface of the container adjacent the discharge orifice 4. These spheres are of suf- ‘ficient diameter to prevent them from passing out through the discharge orifice around the valve stem 5, and also to prevent their upward displacement around the valve stem and pass the valve head into the body of the container. If desired, however, the head portions 7 and 8 may be sepa- rated by the ridge or bead 10 shown in figure 6 of the draw: ings, to additionally insure against displacement of the spheres from between the lower portion 7 of the valve head and the inner surface of the container.’ When the stem 5 strikes the bottom of the well and raises the valve the acid, or whatever liquid is contained in the container,will flow out into the well hele. The next patent on the chart is the patent to Leo Ran- ney, 1,806,499, issued in May, 1931, on an application filed in 1928 for a method of facilitating flow from wells. He states, ‘‘The invention is especially applicable to the clean- ing of oil wells in which deposits of paraffin, caleite or the ~ 76 — James W. Rebbeck like have obstructed the flow from the oil bearing forma- tion.”’ Briefly he proposes to introduce into the well an acid and a gas-generating chemical which reacts with the acid to liberate the gas. Specifically, he puts in either hydro- chloric or nitric or sulphuric acid or other acids or mixtures and then a charge of this gas-generating chemical, as an example specifically noted here is calcium carbide and that reacts with the acid solution making acetylene, and he also states that he may allow that acetylene to be ignited, there- by obtaining additional heat, that is, heat in addition to that produced by the reaction of the carbide on the acid. H{e does not state how he is going to get air to ignite. The Court: It wouldn’t burn, would it, down there? A. I don’t believe it would burn. Nevertheless, le would obtain the heat of the reaction of the carbide with the acid. He men- tions that there will be parrafin in the well and this in- vention serves to remove those deposits. Acid and gas do not react as far as I know. The Court: I think he was doing probably what we have been read. ing about before where his acid reacted with whatever was in the well, various things in there would be likely to be something that would react with that acid, and in that way he might clean it out. A. Well, presumably he uses enough acid to obtain neutralization, although there is a statement on page 2 beginning with line 18 as follows: ‘Since the acid is neutralized or almost neutralized by reaction with the added chemicals or the calcite, ete., there is no substan- tial corrosion of the equipment.’’ In other words he ap- parently does not use any more acid than is necessary to use up the gas-generating chemical he has put in, and the deposits of calcite, and so forth, that may be there. Mr. Lyon: If that is the last one of the patents on this phase of the chart that vou intend to include, might I ask why vou did net include patent 1,891,667 granted to Mr. Carr of 77 James W. Rebbeck Pure Oil Company on an application which was a continu- ation of an application filed April 28, 1932? I am sure you are familiar with that patent and the application. The parent application is earlier than the patent in suit. Why didn’t you include it in this Stream B, in Exhibit 10? A. That was not prior art to the Grebe and Sanford patent. Mr. Lyon: Do you know that of your own knowledge? It is an earlier filed application, and we have taken depositions here which will show the fact. Here is a patent of the Pure Oil Company that describes all about acidizing wells. The evidence in the depositions show that before Mr. Grebe made any invention at all, that Pure Oil Company came over with the idea to— Mr. Owen: I beg your pardon, that isn’t true. That doesn’t show that at all. The Court: Strictly speaking, application is not prior art. Mr. Owen: No. Witness continuing: In making up Exhibit 9 I took this Carr application into consideration. In making up that line I also considered Bowman patent) No. 1,809,546, dated 1931, but no others. The Court: Then there would be twelve. Then he has got this a little bit above, vou see. A. Yes, sir, the 12th application to be filed was the Grebe-Sanford. The Court: There were 12 applications filed on which patents later or at some time were issued. Mr. Owen: There really would be 11, hecause this Mills is not a patent. The Court: Oh, yes. Witness continuing: I want to make a correction be- 78 James W. Rebbeck cause I had forgotten when I made that out as to the num- ber that I had omitted the plaintiff’s application. That one is out. So, there are ten, and the Grebe-Sanford patent in suit is the 11th application that was filed up to that time, on which patents at some time issued. Mr. Lyon: «} Well, which one of these kinks on Exhibit 9 represents the Carr application I have referred to? Is that on there at all? A. That comes after the Grebe-Sanford patent. Mr. Lyon: You just arbitrarily put it afterward. A. It is chron- oligically subsequent to it. The Court: Which one? A. This Carr patent has a later number. It issued in December. The application was filed on the same day as Grebe and Sanford. Mr. Lyon: And it was a continuation of an earlier filed applica- tion, so it states. A. The application on which the Carr patent issued was filed June 30, 1932. Mr. Lyon: And this application states it is a continuation of a prior application filed April 28, 1932. A. No patent issued on that application. The Court: But, it is a continuation of it. Mr. Lyon: Yes. My point is if your chart is exactly as good as stated it was, according to my view the Carr application should come here and should affect this curve and change the curve. The Court: In other words, it would make this one a little steeper and this one not quite so steep. Mr. Lyon: It would also show that this upturn started with the Carr application instead of with the Grebe and Sanford. That is the significant part of it. But, I am willing to just 79 James W. Rebbeck . have the record show for the present that this curve does not correspond to the curve as it would be if the Carr ap- plication was in there ahead of the Grebe application. By Mr. Owen: . Will you explain what patents issued between 1920 and 1932 which caused the r‘se in this line on Exhibit 9, and state what those particular patents relate to, that is, just briefly? A. I cannot state the cause which brought on the issuance of these additional patents in that period of time. The Court: Well, here is one thing that I see (indicating on the chart): We had just nicely got through with the war and the boom period came on. I do not know whether that means anything in the oil industry, or not. Mr. Lyon: It meant a whole lot to the oil industry. The Court: You see this upturn here about the time that we got through with the war in 1918, or it may be a little past that. : Witness continuing: From the point about 1922, where the curve starts to go up, to where it flattens out in 1930 er 1931, very few patents are in consideration in that space. In 1922 the patent issued to Muehl, and that was the sixth application. That is the one at the angle here, right above or just past the 20 mark. The next one was Lake and Phelps, issued in 1924. That is the next point right here (indicating). The next to the right of that, and up a little, is the issuance of Tilton in about 1926. Then the next hump in 1928 is the issuance of the Ranney patent. Then the next is going off to the right, Bowman, 1931. The Muehl patent was dumping acid into a well with a dump bailer to clean out paraffin and calcite deposits and such like. The Lake, et al., patent was for breaking up mud colloids in the well hole. Tilton was fur melting out paraffin deposits. Ran- ney was for melting out paraffin deposits, and Bowman was 80 James W. Rebbeck oo for cleaning the well liner. That had not been mentioned previously. The Court: Here’s the way I understand this graph has been made. Here he starts with the first patent down here (indicating 1865), the next patent he made a date for that, the next patent, and so on; moving up according to the number, getting at the place in the elevation, representing the num- ber of patents, and the date of the application would fix its date for right and left. And then having fixed all, those marks, he just hitched them all together. Isn’t that the way you made it? A. Yes, sir. Mr. Lyon: Yes, but I don’t understand this flat one which ap- parently separates this portion of the curve from that. It seems to me according to the witness’ prior testimony there was another additional application between this point (in- dicating) and this, and necessarily this curve shouldn’t show that break, which, in my opinion, unduly emphasizes something that does not exist. The Court: What I am going to do right now, instead of spending a lot of time about it, is to ask that they hand you their book of patents and you make one of those graphs. Mr. Owen: I am perfectly willing to do that, and have Mr. Reb- beck make his curve. The Court: T like things of that kind. There is that continuity. * They might ea ily make a mistake in that. Mr. Owen: At the time of the adjournment last evening, Your Honor, we had been discussing the correctness of the chart, Exhibit 9, and T asked Mr. Rebbeck to make a new chart showing where each patent enters the picture, and we have that here, and T would like to have him explain it to vou. The Court: We will call that Plaintiff's Exhibit 914. (The chart was thereupon marked PX-914.) 81 James W. Rebbeck The Witness: This chart, Exhibit 914, contains the same information that was on the chart we had yesterday, Exhibit 9, with the exception that the curve representing the information is now drawn in a stepwise manner, to bring out the fact that in each of the periods of time involved where there is no change in the number of applications that issued into patents the line of the curve is horizontal. Beginning at the left-hand side of the chart, in the year 1886, the first patent involving the use of an acid in a well was issued, and is shown by this rise here to thé level of the first step. Then from that time until about 1872, there were no more applications filed on which patents issued. In that year another one issued, carrying the level up to here (indicat- ing). Then no more applications were filed on which pat- ents issued until 1895, when there were two filed that be- came patents. That raises the level up to here (indicating). Then from 1895 to 1900, no more were filed until we get to 1900, and then there was a new one filed. That brings the level up to here (indicating). That makes a total of five in those thirty-five years. And then from 1900 to 1920 no application was filed for which we have discovered an issued U.S. patent. Thereupon one more was filed, bringing the number up to 6, and then in about 1922 another one was filed making 7, and then in 1923 or ’4, another one was filed making 8. I have put the Carr application in when the continuation was filed and not when the original was filed. The Court: You pvt it in when the continued application was filed, and not when the original one was filed? A. That is cor- rect. The Court: If it was put in with the original application, it would come in just over the line somewhere? A. It would come in in 1932, April 28. It would have made this kick up here a little higher, perhaps. It would have made three in here instead of t..o, as we have it now. 82 James W. Rebbeck By Mr. Owen: Q. In other words, if the original Carr application were included it would make this first vertical line to the right of the year indicated by the line 30 a little higher than it is now; is that right? A. Yes, that is right. Now, from 1929 until 1932 there weren’t any applications filed on which a patent issued excluding the original of the Carr continuation which is included in this jump. The continua- tion is included in here and the Grebe-Sanford patent is not included inasmuch as that is one of plaintiff’s, but this kick here is due to the filing of the Carr patent, 1,891,667, and a Carr-Humphrey application which issued in 1935, I believe, and I don’t recall the number of it. This vertical line at the right of the line indicating the year 1930 includes the Carr continuing application which we have been con- sidering. Even if it was with reference to the original application it would come in the same space. It would just raise this kick up, this step. This little tiny step here would be one notch higher. The Court: Now, as he says, as you get higher up you would arrive at the same point all the way up. It just depends whether you cross that road over to the vertical line one notch sooner or not. By Mr. Owen: es Q. Now, will you continue from the point vou left off and state the number of applications indicated in each year by each vertical line? A. Reading from the graph, the first break above the date corresponding to the filing of the Grebe-Sanford represents two more applications on which patents issued, making 12. This step indicates 15 at some date here, I think 1934. The next step indicates about 23 or 22 applications on which patents issued, up to the year 1935. And 25 applications up to 1936. Then we go to that step up here indicating a total of 40. That means there are 28—or there is 30 more than at this time here. And this point is 47, indicating 37 more. And this is 54 indicating 44 more. And that is 56 indicating 46 ap- RA es 83 James W. Rebbeck plications filed :p to this year 1939 on which patents issued involving the use of acid in an oil well. Q. Referring row to Exhibit 10, please take up the patents indicated under Stream A on the left side of the chart and explain what they disclose. A. On the left-hand side of the chart there have been listed a number of refer- ences composed of patents and publications in which some knowledge is given of the use of inhibiting agents to reduce the corrosiveness of acids on iron or steel. The first entry on the list is dated 1845 and is an article appearing in the French publication, Comptes Rendus, by Millon, in which he reports numerous tests made of the corrosiveness of some acid solutions and the effect of the presence in that acid solution of small amounts of metals in the electre- motive series on the corrosive action of the acid. This journal apparently has been in publication for many years. T have seen a complete set of them. We have such a set in the Dow Chemical Company’s Midland library. I have also seen sets of this journal in other technical libraries, and it is my understanding that it is widely disseminated in the libraries of the world where scientifie and other informa- tion is kept. I would like to quote a few parts of the trans- lation of this article: ‘‘The impairment of metais either by pure water or by water charged with acid or saline principles is a phenom- enon that occurs frequently in the laboratory. This phe- nomenon also concerns our domestic uses and among in- dustrial facts it certainly has an important place.”’ The next paragraph goes on to state: ‘‘The experiments that I am about to describe are all connected with this impairment of metals by water in the presence of acids or salts. They only comprise in a word a simple indication of some circumstances under whose action the common metals, iron, zine, tin, copper are at- tacked and sometimes preserved but among all these cir- cumstances there is one that I shall point out at once be- canse T think its intervention has been almost unnoticed heretofore. I wish to call attention io the influence of smalf quantities.’ 84 James W. Rebbeck ‘‘This influence, if I do not mistake the first impres- sion that I have received, is considerable. If one should say, indeed, that a little quantity of metallic solution, added in the proportion of one thousandth, of one hundred- thousandth, and often in a smaller proportion, was suffi- cient to increase hundred-fold the action of an acid on a metal, or to annihilate this action, or to provoke it when it did not exist, or finally even to change the nature of the products to such a point that hydrogen replaces nitrous compounds, one would seem to be, in such an assertion, as far from the facts as from chemical predictions. ‘*Nevertheless, that is what happens.’’ Those are his introductory remarks, and then he goes on to describe some of these experiments. The method of his experiments, I think, is summarized in this paragraph which T will now quote from page 2 of the translation: ‘‘Thus, rolled zine has been brought into the presence of dilute sulphurie acid to which has been added some traces either of platinous chloride, or of tartar emetic, arsenious acid, copper sulfate, silver sulfate, ete. The metal, weighed before the reaction, was weighed again after the reaction had lasted for a definite time. In other in- stances, the gas was collected and measured. T shall in- dicate the principal conditions of the experiments made by means of zine and dilute sulphuric acid. The zine was rolled in sheets thin enough to give 100 to 102 centimeters of surface per weight of 15 grams. The sulphurie acid was composed of one part of monohydrated sulphurie acid SO.H,O to 12 parts of distilled water. The zine was weighed exactly, and six nearly equal quantities of water were introduced into six glass flasks, each of which con- tained 1% decilitres of the‘one-to-twelve sulphuric acid.’’ The flasks were distinguished by the numbers 1, 2, 3, 4, 5 and 6. Now, I will pass over these experiments on zine and go to those he performed on iron, inasmuch as we are here interested in iron. Here we have the essentials of his method. He weighs a zine piece or metal piece and puts it in the acid for a given length of time, withdraws it, 85 James W. Rebbeck weighs again, and determines by the loss in weight what has happened. Now, the experiments on iron and tin are referred to on page 11 of the translation: ‘Tron and tin have been subjected to tests analogous to those of zine. One-to-twelve sulfuric acid dissolves iron turnings rather rapidly; some drops of platinous;chloride communicate an extreme intensity to this action. Arsen- ious acid, on the contrary, stops all action on iron by sul- furie acid; this influence is sufficiently pronounced for the metallic iron to keep for a whole month, and without doubt still longer, in one-to-twelve sulfuric acid which dissolves it rather rapidly. When the iron is well cleaned, some drops of an aqueous solution of arsenious acid are suff- cient to preserve it from the acid; at the same time it pre- serves metallic reflection whose shade becomes only rather darkened. Tartar emetic slackens the action of sulfuric acid on iron, but does not stop it. Mercurous chloride acts like tartar emetic. Copper sulfate aceclerates strongly the evolution of hydrogen; silver sulfate also accelerates it, but less appreciably.”’ By accelerating the evolution of hydrogen it means that the iron test piece is dissolving at an accelerated rate. ‘*Hydrochloric acid receives, from small quantities of metals, the same influence as dilute sulfuric acid: these re- actions can even be observed with rather concentrated hydrochloric acid; it is sufficient to dilute the pure fuming acid with 2 or 3 volumes of water. In some cases the addi- tion of a small quantity of copper sulfate has suspended very appreciably the action of hydrochloric acid. The iron becomes covered with metallic copper and remains for sev eral hours without furnishing hydrogen; but it has not always been thus, without it being possible to ascertain whether this difference depended on the hydrochloric acid or the iron.’’ These tests contiuue with some other acids. The next one mentioned is arsenious acid, and according to Millon arsenious acid stops all reactions as it did with the two pre- ceeding acids, the preceding being sulphuric and hydro- Nye 86 James W. Rebbeck chlorie. It goes on to say :‘‘Tartaric and racemic acids are identical in all the influences that ‘they undergo; more abundant evolution with platinous chloride; hindrance to reaction with arsenious acid; almost complete indifference on the part of other metallic solutions.’’ I believe that that gives the essence of this part of the article. The next reference on the chart on'the left-tand side is dated 1883 consisting of a U. 8. patent No. 288,150 to Benjamin F. Aiken, Jr., for wire or metal cleaning bath. This, I believe, is one of the first U. S. patents to mention the addition to a corrosive acid of something to obviate its corrosive effects, those corrosive effects being the action of the acid on iron and steel. This patent is in the pickling art, which is briefly stated to be as follows in the patent specification, page 1, column 1: ‘*In the successive processes of drawing wire the iron becomes fibrous and requires to be annealed to render it ductile and in the operation of annealing its surface be- comes more or less covered with an oxide scale which must be removed before the operation of drawing can be con- tinued. This is commonly done by immersing the wire in a hot bath of dilute sulfuric acid for a short time and then checking the action of the acid upon the metal or devitroliz- ing it by immersing the wire in a bath of hot water or sub- _jecting it to a current of cold water, otherwise the excessive action of the acid bath would render the wire brittle and unfit to be drawn. The wire or wire rods are then coated or covered with a paste of meal or flour, clay or a solution of salt, or of lime, or of a salt and lime, either alone or in connection with oily and fatty substances which act as lubricants to the surface of the wire as it passes through the die plates.’’ Now, coming to his invention, he says: ‘‘I use instead of the bath of dilute sulfuric acid above mentioned a bath formed by adding to water a cleaning corrosive acid. In case the wire is to be drawn I use sulfuric acid; in other cases such as when coating with zine or tin, hydrochloric or nitro-muriatic acid may be used and to the acid and - oitibeds - yoy 2 7, EE RC Le Lee eS TPA SO ec dere a wee TTS Pe ay eee oe ee . 2 a ; q ; j : q 3 ” 87 | James W. Rebbeck water I add cyanogen generally, and for convenience in the form of a metallic cyanide.’’ Now he goes on to say what he gains by doing that as follows: ‘‘By the combination with an acid cleaning bath of cyanogen in the form of a soluble metallic cyanide I in- crease the efficiency of the acid bath and effect a great sav- ing in the cost of cleaning. I also obviate to a considerable extent the injurious results of the excessive action of the sulfuric acid bath in rendering the iron brittle arising either from the absorption of free hydrogen or from other causes. ’’ The Court: Is that a very good description of an inhibitant? A. Yes. For the reason that the inhibitants that we find in these patents out of the pickling art are used to correct this hydrogen embrittlement which would otherwise occur if an inhibitant was not used. Mr. Lyon: ‘ I would just like to have the court have in mind that this is a selection of patents which the defendant in this case has not selected, and it is a different selection from what was before the court in the Williams Brothers case. Mr. Owen: , I want to make it clear that the purpose of this chart was not to make a complete disclosure of the prior art. We couldn’t do it on a chart of this kind. But we merely se- lected illustrative patents or publications which would show the developments. Witness continuing: Now, the next one on the chart, left-hand side, is dated 1991, and is a publication called The Journal of the Society of Chemical Industry in which there appears an article by James T. Conroy on page 316, entitled ‘‘The Rate of Dis- solution of Iron in Hydrochloric Acid.’’ This article opens with this paragraph: ‘“‘The behavior of acids towards metals is a problem of great interest both to the chemist and the manufacturer and such behavior has been the subject of considerable in- vestigation. 88 James W. Rebbeck ‘‘Sometimes, perhaps most frequently, it is the manu- facturer’s object to obtain a metal not acted upon by some particular acid. At other times, action is desired, and in this case a knowledge of the course of the reaction, its rate and the conditions under which it occurs is of the greatest importance, ‘*To take a particular instance, I may refer to the clean- ing of iron by acids, the so-called pickling process, a pre- liminary operation in the preparation of this metal for the galvanizing bath.’’ This article goes on with experiments performed on the rate of dissolution of iron in hydrochloric acid at different temperatures and with different concentrations of acid, hydrochleric acid being capable of many concentrations. Then when we come towards the end, in fact it is the end, he refers to the fact that the foregoing experiments were all done with distilled hydrochloric acid, practically free from impurity of any kind. (Reading) : ‘*In practice commercially pure acid is employed. Such acid must be free from arsenic, the presence of which is prejudicial during the pickling stage apart from the trouble it causes later on in the galvanizing bath. The ef- feet produced when arsenic is present in small quantities is shown in Table 4. When larger quantities are present the iron becomes completely covered with a film of arsenic which at ordinary temperature almost completely checks further action even with the more concentrated acids.’’ Now, by referring to this table, we see that the experi- ments were performed with hydrochloric acid of concentra- tions between 180 and 216 grams per liter, and with amounts of arsenious oxide of from 0.04 grama to 0.16 grams per liter and at temperatures from 18 to 61.5° C. In this experiment he measured the cubic centimeters of hydrogen evolved per hour both before arsenic had been added and after arsenic had been added, and he sets down the rate of evolution figures thus observed. To take one example out of the list, the one that appears on the chart, and converting the concentration given here in grams 89 James W. Rebbeck per liter into weight per cent we get the Pollowing figures: Two hundred grams per liter of hydrochloric acid is approximately a 20 per cent hydrochloric acid solution. The addition of .16 grams per liter of arsenic trioxide is ap- _ proximately a 0.015 per cent solution of arsenic, and the rate of hydrogen evolution without the arsenic is given here as 26 cubic centimeters per hour, and when the arsenic is present the rate drops to 19 cubic centimeters per hour or a reduction in the rate of evolution, computed by me to be about 27 per cent. The next one is dated 1912, an article by Oliver P. Watts, which appeared in the Transactions of the Ameri- can Electrochemical Society, Volume 21, beginning on page 337, entitled, ‘‘The Effect of Various Substances on the Rate of Corrosion of Iron by Sulphuric Acid.’’ The title is a little bit misleading, because he also works with hydro- chloric. His opening paragraph is as follows: ‘‘In volume 8 of the transactions of this society C. F. Burgess called attention to the remarkable reduction in the corrosion of iron by sulphuric acid brought about by the addition of a small amount of arsenious oxide to the acid.’’ Later he explained the protective action as follows: ‘The explanation which has been offered for this phenomenon is that the iron receives by contact with the solution an extremely thin coat of arsenic which resists the action of the acid and protects the underlying metals.”’’ He also gave experimenta! proof that the iron was coated with arsenic. The second paragraph states: “It has long been known that by dipping clean iron into solutions of suitable composition and concentration thin coatings of gold, silver, platinum, copper and several other metals may be deposited on the iron. It is generally conceded that such coatings are not sufficiently continuous and impervious to protect the underlying metal from cor- rosion, even though the metal forming the coating may it- self be thoroughly resistant to the corrosive agent. Instead of being a protection, such coatings are usually considered to be stimulators of corrosion."’ 90 James W. Rebbeck We started at the place where we had an acid solution containing arsenic in the solution as arsenious chloride, presumably. There is no metallic arsenic in this solution at all. The element is there but it is not present as little bits of metallic arsenic that you could fish out. It is dis- solved. Now, this third paragraph goes on to discuss the theory of this protective action as follows: ‘‘Since all metals which thus deposit upon iron when it is immersed in a solution of the metallic salt are electro-negative to iron, a short-circuited voltaic cell is formed, of which the iron is anode and the metal deposit is the cathode. So long as any iron remains in contact with the electrolyte, it would seem, except for certain considerations which will be presented later, that the corrosion of the iron ought to be stimulated by this condition, and that the only way in which such a coating could afford good protection would be by covering the iron completely, so that no electrolyte could come in contact with it. ‘‘Speaking of the effect of other metals in contact with iron, W. H. Walkes says: ‘Tin is a metal which, like cop- per, accelerates the corrosion of iron by aiding in the oxi- dation of the hydrogen set free by the reaction.’ M. P. Wood calls attention to the injurious action of metals, ‘The use of anti-corrosive, or anti-fouling paints, contain- ing salts of any metal, is attended with the greatest danger to the coated (iron or steel) structure. These pigments are extremely sensitive to the presence of saline elements in moisture, their action being to rapidly dissolve portions of . the iron, and to deposit the metal which they contain upon the surface of the plates, and these deposits, exciting ener- getic galvanic action, cause corrosion and pitting to go on with alarming rapidity. Both mereury and copper salts are offenders in this way.’ ’’ - IT am going to read direct'y from paragraph 2 on page (Reading): ‘‘It appears then, that arsenic is unique among the metals which precipitate themselves upon iron from solution, for arsenic protects iron almost completely on ede? 91 James W. Rebbeck from powerful corrosive agents, while the other metals are generally considered to aggravate eorrosion aid rusting. “If the coating of arsenic is so porous and imperfect as the action of acids show the coating of copper, for ex- ample, to be, how can the arsenic protect the iron any bet- ter than copper does? It occurred to the writer that the explanation lay in a high over-voltage or excess potential of hydrogen on arsenic, and the experiments which follow were undertaken to discover whether this is the explana- tion of the singular and mysterious protective action of arsenic. If the above explanation is correct, among the metals which deposit upon iron when it is immersed in a solution of their salts those having a high over-voltage for hydrogen should protect iron, and those of very low over- voltage should aggravate the corrosion.’’ The Court: Does that mean that silver and copper, and those other things that he mentions actually tend to corrode, destroy iron when they are present, worse than if they are not pres- ent? A. Yes. The article goes into the matter of the electrode po- tentials of the metals involved here, that is the voltage as- sumed by the metal with respect to the solution in which it is immersed, and he gives a table of what is called single potentials of many of the metals in the electromotive force series of metals between iron and mercury, and including those metals. Then he goes on with his theory as follows: ‘*On the theory that the protection of iron by a deposit of arsenic is due to the high overvoltage of hydrogen on the latter, the action would be as follows: Iron dissolves and by so doing deposits arsenic upon the surface of the iron. Since the arsenic is deposited simultaneously with the dissolving of the iron and only as a result of this dis- solving it is hardly possible that the iron should be com- pletely covered by arsenic, but here and there holes will exist allowing the iron to make contact with the electrolyte. Voltaic cells are thus formed.’’ 92 James W. Rebbeck The Court: Is this chap right in his theory? A. I subscribe to this theory. (Continuing reading): ‘‘The iron is anode and the arsenic cathode, and just as in any other primary cell with sulfuric acid as electrolyte, hydrogen is deposited on the cathode, but when hydrogen is liberated on arsenic the po- tential of the latter is raised 0.39 volts higher than 0.277, the potential at which hydrogen is liberated on platinum black. This would raise the potential of the arsenic to +0.113 volts or higher than the potential of the iron anode. This means that in our iron-arsenic cell there can be no vis- ible evolution of hydrogen on the arsenic for before this can occur the potential of the cathode has become equal to that of the anode and corrosion of the iron ceases. In other words, this particular primary cell polarizes so badly that after a few seconds of action its electromotive force has fallen to zero.’ Then he goes on to say (reading): ‘‘If the above ex- planation is correct, protection should be afforded by those metals which plate out on iron by immersion, and whose over-voltage for hydrogen is great enough to raise their potentials to at least equal the single potential of iron. The potentials of the following metals are far enough below that of iron to expect that they will deposit on iron even in moderately strong sulphuric acid.”’ By Mr. Owen: Q. In this Watts article, I notice that on page 352 he gives a table under several headings: One of them is ‘‘Re- tarders of Corrosion,’’ and another on page. 352 is ‘‘ Aeceler- ators of Corrosion.’* Now, I would like to have you state to the court which metals are contained under each of these headings, first under the heading of ‘‘Retarders of Cor- rosion.’’ A. The first here is arsenate of sodium. Of course, that is not a metal but it is a compound containing tlhe metal which he used. Arsenic sulphate, chloride of manganese, chloride of mercury, chloride of sodium, chlor- ide of tin, chrome alum, chromium § sulphate, mercuric chloride, mercurie sulphate, and stannate of sodium. Stan- nate of sodium is a tin compound, 93 James W. Rebbeck Under the heading ‘‘ Accelerators of Corrosion’’ the . first in order is bismuth sulphate. Then chromium chlor- ide, copper sulphate, gold chloride, mercurous nitrate, platinum chloride, potassium chlorate, chromate, dichro- mate, nitrate, permanganate. The next reference on the chart, Exhibit 10, is a pub- lication from the Bureau of Mines, Department of the In- terior, dated October, 1919, entitled ‘‘Substitution of Nitre Cake for Sulphuric Acid in Pickling Steel,’’ by E. E. Corbett, Chemical Engineer, U. S. Bureau of Mines. On page 2, under the heading of ‘* Mechanism of Pick- ling Reactions,’’ it states (reading): ‘The free acid in hot, dilute solution attacks the metal very readily, etching it away from beneath the coating of scale and consequently throwing off the particles of oxide from the surface. Iron goes into solution as ferrous sulphate; and the hydrogen which is liberated at the face of the metal is carried rapidly to the surface cf the solution, where it escapes into the air with the steam and other gases rising from the pickling bath. * @ ©»? Now, the portion of this publication which is of inter- est in this connection here is that part beginning on page °) under the heading of: ‘‘ Inhibition, or moderation of metal attack,’’ as follows: ‘The activity of the acid, then, is directed to attack- ing selectively and dissolving the sound metal rather than the more resistant oxide or scale; but in well regulated pickling practice the selective attack is limited, and, in- deed, materially re-directed and controlled by the use of bodies of a colloidal or semi-colloidal nature whose in- fluence serves to protect the metal during seale removal. These bodies are for the most part of vegetable origin, and comprise Various wood sugars and gums, and cereal starches and intermediates occurring in commercial grain milling.’’ And then he goes on ta mention other types of inhibit- ing agents as foilows: ‘*Tin and copper salts are representa- ° tives of the inorganic type of semi-colloidal inhibitors; but their action is of inferior consequence and their use re- 4 James W. Rebbeck stricted because of the cost of adding to the bath quantities sufficiently large to exercise a sensible influence, as well as their tendency, undesirable for most purposes, to plate out from solution upon the metallic surface.’’ Mr. Lyon: I would like to ask a question before we leave this Corbett article. Was this article ever published? If so, where, or from where, by whom, and when? A. I can re- fer to an article which appeared subsequently to this as a result of the issuance of this article by Mr. Corbett in the Automotive Industries for 1918, December 5. This article was almost re-written word for word in that publication, which, of course, has wide circulation in the metal trades. The next reference under Stream A of Exhibit 10 is dated 1921. It is the British patent No. 158,768, having a complete accepted date of February 17, 1921, for improve- ments in pickling iron or steel. This patent is apparently the counterpart, or the British application corresponding in many particulars to one filed in this country in the name of Vogel, so I have put the name Vogel against this British patent. This teaches about the corrosive action of the acid during the pickling operation, and some of the evil effects resulting from that, and proposes the addition to the pick- ling bath of certain substances to overcome those diffi- culties. Quoting from the specification, page 2, column 2, begin- ning with line 73, it reads as follows: ‘*A modification of the process consists in adding to the pickling liquor, not the protective substance itself but a suitable extract thereof. It has been found that it is not the main constituent of the substance in question, namely, anthracene, naphthalene, phenol or the like, that has a par- ticularly good effect, but other constituents the chemical constitution of which has not been elucidated, but which nearly always accompany the main constituent. The ac- tive substance may be extracted by inorganic acids, neutral or acid salts, organic solvents such as hydrocarbons (petro- leum, tar oil). Advantageously the parent substance may 95 James W. Rebbeck be treated with 3 to 4 parts of sulphuric acid of strength which may vary, or of hydrochloric acid or of other suitable extracting agent and, according to its strength, 1 to 10 per cent of the extract may be added to the pickling liquor. ‘*There is added to the liquor a quite small proportion of a material which causes formation of the thin protective layer. For forming such a layer, having regard to suffi- ciency of supply and cost, the following has been proved particularly suitable additions:—-Crude anthracene, sul- phite lye, residues from the production of naphthalene and the like-’’ There are some other substances mentioned which might be used. ‘‘There may also [Text truncated at 120,000 characters. The full text is on the page linked above.] --- Source: Frix Law Library, https://www.frixlaw.com/law-library/documents/brief%3Amicro_IA40386404_0119%3A01. Public record. Not legal advice.