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The Development of Calcium Carbonate - Iron Oxide Protective Coatings on Iron

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The Development of Calcium Carbonate - Iron Oxide Protective Coatings on Iron THE DEVELOPMENT OF CALCIUM CARBONATE - IRON OXIDE PROTECTIVE COATINGS ON IRON rjahmoud 0 . Ab du 11 ah. AN ABSTRACT Submitted to the College of Graduate Studies of Michigan State University of Agriculture and Applied Science In partial fulfillment of the requirements for the degree of Doctor of Philosophy Depart rent of Chemical Engineering 19 3 C THE DEVELOP] [TNT 0- CALC ILL I CARBONATE - I HON OXIDE PROTECTIVE COATINGS ON IRON A3STRACT The development of useful protective coatings for pre­ vention of corrosion in water systems has been under inves­ tigation using both static and dynamic tests. All work has been with water containing calcium hydroxide, carbon dioxide, oxygen, and nitrogen. Review of the literature indicated that a good under­ standing of the effects of pH, temperature, salinity, and other factors on the equilibrium of calcium carbonate in water has been reached. However the nature of the scale and the factors influencing its formation have not been com­ pletely established. It has been the ob'ect of this research project to de­ velop ’uniform coatings in a dense impermeable form that will provide high anti-corrosion protection, and to investigate and evaluate the effect of certain physical and chemical en­ vironmental conditions on the formation of these coatings. Petrographic methods were used to identify the minerals developed on the specimens. Coating materials developed on cast iron specimens were largely limonite. Live to forty percent calcite was commonly present. Siderite and magnetite were usually observed covered by limonite. Uith stainless steel specimens, only calcite was found* Polarization studies Indicated that CaCO^ acted pri­ marily as a cathodic Inhibitor# The action of calcium car­ bonate in developing good protective films seemed to lie in forming a physical mixture with corrosion products. Under favorable conditions the mixture bonded well to the cast ir on specimens and was hard and relatively tough. Better protection and better Bonded, harder, and tougher coatings resulted from solutions containing colloi­ dal CaCOg than from Identical solutions of the same pH and hardness with no colloids present. Colloidal CaCOg was found to have a positive charge In the pH range 6-11 and may be represented as (CaCO3 ) Ca++JoiI"* Calcium carbonate crystals In suspension did not have a favorable effect on formation of coatings from s rcsrsaturated solutions. Relatively high flow velocities of about 2 feet per second were desirable In the formation of hard durable coatings. Static tests generally produced soft coatings. A saturated level of oxygen was found to be optimum for de­ veloping good coatings under the conditions conducted In this study. A high momentary excess of CaCCg led to the formation of chalky soft coatings. Low momentary excesses and high saturation excesses of CaCQg led to the formation of h a v*''‘!, Thus, it has been established that when a water is sa­ turated with dissolved oxygen, Is of pH 8.2 to 8.7, contains a momentary excess of 2.5 to 5*5 ppm CaCOg In the presence of colloidal CaCO^, and flows at a velocity of about two feet per second, a uniform, hard and well bonded coating can be developed on cast iron specimens in one dayTs time at room temperature. THE DEVELOPMENT OF CALCIUM CARBONATE - IRON OXIDE PROTECTI RE COATINGS ON IRON By Mahmoud 0. Abdullah A THESIS Submitted to the College of Graduate Studies of Michigan State University of Agriculture and Applied Science in partial fulfillment of the requirements for the degree of Doctor of Philosophy Denartment of Chemical Engineering 19 08 Approved ProQuest Number: 10008565 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a complete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest. ProQuest 10008565 Published by ProQuest LLC (2016). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States Code Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 ACIQiOULEDGhENT This thesis was only possible with the sincerely ap­ preciated support of a N.I.H. grant. The author wishes to express his sincere appreciation to Dr. R.F. McCauley and Dr. C.F. G-urnham for their valu­ able guidance and assistance in connection with this thesis. Thanks are also extended to Dr. H. Storehouse and Mr. C. Star for their help In the analyses of the coatings de­ veloped. TABLE OF CONTENTS Page INTRODUCTION.............................................. I LITERATURE REVIEW........................................ .3 TUEORETICAL C0N3JDEEATIONS................................9 A. Electrochemical Theory of Corrosion of Iron.......... 9 B. Typical Corrosion Cell on the Surface of Submerged Iron......................................13 C. The Action of Inhibitors................ ....... ...,l5 D. Polarization and the Rate of Corrosion..............19 E. Different Indexes Used for Calcium Carbonate Equilibrium......... 2k 1- Langelier Saturation Index...................... 2k 2- Ryznar Stability Index.......................... 2? 3- Saturation Excess......... 27 k“ Momentary Excess .......... .....28 EXPERIMENTAL APPARATUS AND MATERIAL...... 29 A. Static Test Unit*..*................. ............... 29 B. Dynamic Test Unit with Rec irculated Water............31 C. De-ionizing Units................. 38. D. Electrical Measurement '"nit..*.......... ....36 1- Potentiometer. ..... 36 2- Batteries ...... .36 3- Standard Cell 3q k- Galvanometer* .......... * . 39 5- DC Power Supply.*.............. 39 EX PER I MENTAL PROCEDURE ....... * ..*.'■ 0 A. Static Tests........ ...IQ B. Dynamic Tests with Recirculated Water*............. kl C. specific Investimations, . « , . , . * . , .in 1- Potential Measurements * , '• 3 2- Preparation of Colloidal Calcium Carbonate......' 3- Determination of ElecJ-rima l Charge of Colloids ..' ? k- Analysis of Specimen Coatings After the Tests...' C 5- Routine Analytical Determinations .... 1 Page CONDITIONS OF THE TESTS AND ANALYSIS OF THE COATINOS DEVELOPED.................................................50 DISCUSSION OF RESULTS.............. .61 Mineral Contents of Developed Coatings •.......01 Polarization Studies.......... , . ....... 62 Formation of Colloidal CaCOQ.................... .*.68 Electrical Charge of Colloidal CaCOo.............. .7J-J- Effect of Colloidal CaCO^ on Coatings Developed....76 Effect of Momentary Excess on Coating Development••85 Effect of the Age of Colloidal Particles on the Rate of Deposition of CaCO^ and Coating Development......... 93 Effect of Dissolved Oxygen Levels on Coatings Developed............... 98 Effect of Specimen Surface Conditions on Coatings Developed. ..................... 107 Effect of Iron Oxide on Coating Development on Stainless Steel Specimens......................... 112 Static Tests VS. Dynamic Tests....... llh CONCLUSIONS............................................. 116 RECOMMENDATIONS.......... 118 BIBLIOGRAPHY............. 120 LIST OF FIGURES Figure Page 1 Schematic Diagram of Corrosion Cell on Surface of Submerged Iron....................... lR 2 Typical Polarization Curves..................... 20 3 Types of Corrosion Control Curves....... 23 Ur Equipment for Dynamic Tests , . .28 3 Equipment for Static Tests...................... 30 6 Flow Diagram of Dynamic Tests with Recirculated Water........... 32 7 Test Cell Construction.......................... 33 8 Large Two-Bed lon-Exchanger ........ 35 9 Potentiometer Circuit Diagram....... ........... 37 10 Wiring Diagram of Electrical Equipment....... Jgli 11 Polarisation Curves of Dynamic Test 1*.......... PR 12 Polarization Curves of Dynamic Test 2 .......... 65 13 Polarization Curves of Dynamic Test 3 ........ 66 ll- Curves Showing the Relationship of Momentary Excess and Saturation Excess Values to the pF Levels of Supersaturated Solutions at 'filch Colloidal CaC03 Formed. ..... .72 15 Schematic Diagram of Colloidal CaCO^ PartIcle...77 16 Potential-Time Curves showing vhe Effect of Colloidal CaCOg on Coatings Developed In Dynamic r’ests h and 3 . ......... q Figure Page 17 Potential-Time Curves Showing the Effect of Momentary Excess Levels on Coatings Developed in Dynamic Tests 7 , 8, 11, and 12............... 89 18 Potential-Time Curves Showing the Effect of Fate of Deposition of CaCO^ on Coatings Developed in Dynamic Tests 15 and 19........... .95 19 Potential-Time Curves Showing the Effect of Rate of Deposition of TaCOy on Coatings Developed in Dynamic Tests 12 and 13............97 20 Potential-Time Curves Showing the Effect of Dissolved Oxygen Levels on Coatings Developed in Dynamic Tests 20, 21, 22, and 21g............ 103 21 Potential-Time Curves Showing the Effect of Dissolved Oxygen Levels on Coatings Develo :sd in Dynamic Tests 17, 18, and 19................ 105 22 Potential-Time Curves Showing the Effect of Cast Iron Specimen Surface on Coatings Developed in Dynamic Test 11........ 109 23 Potential-Time Curves E:: owing the Effect of Stainless Steel Specimen surface on Coatings Developed in Dynamic Tests 12 and 13..........,111 LIST OF TABLES Table Page 1 Conditions and Analysis of Coatings of Static Tests . .. ....... ......... ............ 52 2 Conditions and Analysis of Coatings Developed of Dynamic Tests...................... 57 3 Percent
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