EXAMINATION OF TRON, STEEL AND BRASS RY WILLIAM T. HALL ASSOCIATE PROPESSOR OF ANALYTICAL CHEMISTRY, MASSACHUSETTS INSTITUTE OF TECHNOLOGY AND ROBERT S. WILLIAMS ASSOCIATE PROVESSOR OF ANALYTICAL CHEMISTRY AND MUETALLOGRAPEY, MASSACHUSETTS INSTITUTE OF TECHNOLOGY Tinsr Eprtiow McGRAW-IIILL BOOK COMPANY, Inc. NEW YORK: 370 SEVENTH AVENUE LONDON: 6 © 8 BOUVERIE 8T., B.C. 1921Copyricet, 1921, By THE McGraw-Hit Boox Company, Ic.recognized but modern methods of manufacture and.the use of metals under conditions of severe strain demand additional information which can best be obtained by the examination of polished specimens. Both of these branches of metal inspection are considered in this book. Part I deals with the Chemical Analysis of Alloys and includes well tested methods of analysis selected mainly from reports of the United States Bureau of Standards or from papers of the Ameri- ean Society for Testing Materials. Although most of the standard methods of steel analysis are included, special emphasis has been placed on those methods which are both rapid and accurate. Part If considers-the physical rather than the chemical in- spection of metals and describes the methods of preparation and examination of polished metal surfaces as an independent means of detcrmining the quality of material as well as an aid in getting representative samples for chemical analysis. A brief introduction to metallography, in so far as it applies to the inspection of alloys, is included. The authors wish to express their sincere ‘appreciation to Messrs. Bauer and Deiss whose book on the “Sampling and Analysis of Tron and Steel,” translated by them in 1915 and published with many additions and modifications suggested the idea of combining chemical and metallographic inspection. Assmall portion of the translation is included in this book, notably several tables and a number of photomicrographs for which the authors again express their thanks. Grateful acknowledgement is made to Professor Henry Fay fot the use of several photomicrographs and to Dr. W. P. Davey for an X-ray Photograph. Special thanks are duc to Mr. V. O. Homerberg who prepared and photographed inany of the speci- mens used in illustration, Winns T. Have Rosert S$. WILLIAMS. Massacuvserts Instiruts or TECHNOLOGY, August, 1921. vCONTENTS Paaw PRErAcR. . . AEE v PART L The Chemical Analysis of Iron, Steel and Brass CHAPTER I Inrropuerion 2... 2s , uh SPce ane CHAPTER II Cannons Mase GRR BSS SARS Rese ene sens benesBeeeeeeneenee 7 1. Determination of Carbon by Direet Combustion in Oxygen . . 11 2. Direct Combustion af Carbon in Oxygen—Rapid Method 19 3. Combustion of Carbon in the Wet Way, Corleis Chrome— Sulfurie Acid Method . 23 4. Determination of Total Carbon by the Potassium-Cupric 7 Chloride Method . +e . 382 5, Determination of Carbon by the Deiss Method aren ons7 Determination of Graphite and Temper Carbon, Seeeeeeee Colorimetrie Method for Carbon in Steel. . . . . ae 46 CHAPTER II Mancaress yah eee Cesc Ric aRacncn aces 47 1. Determination of Manganese by the Bismuthate Method 49 2, Determination of Manganese by the Ford-Williams Method. 56 3. Determination of Manganese by the Volhard Method 50 4, Determination of Manganese by the Persulfate Method . . . . 69 5. Gravimetric Determination of Manganese rea saic0 CHAPTER IV Paosrorus. . . . 90 1. Determination of Phosphorus in Steel by the Malybdate- Magnesia Method... 1 2. Determination of Phosphorus in Steel by the Alkalimetrie Method! BARS Anes P en BSee near RSC n rarer 94 3. Determination of Phosphorus in Cast Iron. . : - 96 4 Determination of Phosphorus by the Johnson Method. 100 5. Determination of Phosphorus by the Acetate Method of A. A. Blair (Modified)... see ee 101 viiPace 6. Determination of Phosphorus by the Permanganate Titration . 104 7. Determination of Phosphorus in Materials Insoluble in Nitric eee eee eeneeeeneneaeen - 109 8, Determination of Phosphorus in Materials Containing Arsenie | 110 9. Determination of Phosphorus in Materials Containing Tungsten 111 10. Determination of Phosphorus in Materials Containing Vana- 113 Sisco 16 1 115 2. .. 119 ; 3. Nitric Acid Method for Silicon... ........0.. 121 4. Determination of Silicon in Materials Insoluble in Acid 124 CHAPTER VI Sureca Pye Pee ese arearaen: APSARA ESPN Fi 2s) 1. Determination of Sulfur in the Presence of Iron... .. . . . 130 2, Bamber Method for Determining Sulfur in Iron or Steel . . . 131 3. Determination of Sulfur by the Ether Method . . pjeeeeie de 4. lodometrie Determination of Sulfur in Steel. . - 133 5. Determination of Sulfur by the Simplified Evolution Method 135 6, Evolution Method and Absorption of Hydrogen Sulfide in Bromine and Hydrochloric Acid. . . . . : Seaeeeeenl 7. Determination of Sulfur in Insoluble Materials .. 2... . 141 y CHAPTER. VIT Corre : Waipu 1. Precipitation as Sulfide from Acid Solution, . . 142 2 Determination of Copper after Removal of Iron with Ether . . 144 3, Removal of the Iron with Sulfuric Acid... 2... 144 . 4, Electrolytic Determination of Copper... . 2.2... . 148 ; 5. The Rapid Determination of Copper in Steel... 2... . 146 CHAPTER VIII Ounomrom. SCAR ICSCRIER CMA ACns 150 1, Determination of Chromium by the Barium Carbonate ee eee eee eee eenee see ae . 150 2, Determination of Chromium by the Method of Barba (Modified) 5 3. Determination of Chromium by the Chlorate Method 153 4, Determination of Chromium by the Bismuthate Method . . . 15: 5. Determination of Chromium by the Ether Method... . . . 155 6. Determination of Chromium by Fusion of the Oxides with Sodium Peroxide. eed eee . 165 7. Determination of Chromium in Materials Insoluble in Acid |. 167CHAPTER Ix Paow Tnow eee eee Reale eRe! PSERAEI7O 1, Determination of Iron in Materials Soluble in Acid” (A) Mohr’s Iodometrie Method... 2... . . 170 (B) Zimmermann-Reinhardt Method... . 2... 2... 172 2. Determination of Iron in Insoluble Materials... . . . . . . 178 CHAPTER X NickEL. 2. ee ee oe on . 175 1. Determination of Nickel by the Dimethylelvoxime Method | | 175 2, Determination of Nickel by Electrolytic Deposition . . . . . 178 3. Volumetric Determination of Nickel by Potassium Cyanide . . 182 4. Determination of Nickel by the Volumetrie Dimethylglyoxime Method... . . 185 5. Determination of Nickel by Potassium Cyanide after ther Extraction... 2. ee ee acaeeeeeeeee CHAPTER XI Mouyspenum.. 2... 188 1. Determination of Molybdenum by the Sodium Peroxide Fusion Meshod Aye Seer esr aeae 190 2. Determination of Molybdenum by the Ether” Ixtraction Method of Blair. . PES PaPeseNPaPashic2 3. Volumetric Determination of Molybdenum... 2... . 198 CHAPTER XII TUNGSTEN, 7 tee 195 1. Determination of Tungsten as ‘Trioxide by Precipitation from an Acid Solution Containing Cinchonine Hydrochloride - 195 2. Determination of Tungsten by the Deiss Mcthod . 197 3. Determination of Tungsten by the Sodium-Peroxide Fusion Method... ... 202 4, Determination of ‘Tungsten in Materials Insoluble in Acid... 204 CHAPTER XII ‘Vawaprom, 206 1. Determination of Vanadium by the Phospho-Molybdate Pre- cipitation Method . . . ounwsra 1208) 2. Determination of Vanadium by ‘the Blair Method. aan 210 . Determination of Vanadium by an Iodometric Method . . . . 212 4. Determination of Vanadium by a Fusion Method. . 216 5. Gravimetric Determination of Vanadium. . . . QTCHAPTER XIV Avumasius . 2... CHAPTER XV ARSENIC. © 0 SEecRaCeceace es CHAPTER XVI Copant . . CHAPTER XVII FrANs Ce anes eC e Ce Cee 1. Determination of Titanium in Materials Soluble in Acid” (a) Colorimetric Determination . (b) Volumetric Determination. (c) Determination of Iron in Impure Titaninm Oxide . 2. Determination of Titanium in Insoluble Materials CHAPTER XVIII Neraogen sac EaP Eee R eae ceca: 1. Determination of Nitrogen in Steel (Method of A. H, Allen) 2, Determination of Nitrogen (Method of L. E. Barton). . CHAPTER XIX Oxyarn. 1. Ledébur’s Method for Oxygen 2. Method of Walker and Patrick for Determining Oxygen CHAPTER XX Zuconium. aCe ALUMINIUM... CeCe (@) In the Absence of Chromium (b) In Steels Containing Chromium acorn (c) In Steels Containing Uranium Seseeseeeeeene (d) In Steels Containing Vanadium Derersinarton of ZIRCONTUM AND TITANIUM CHAPTER XXI ELucrkomeriie Miraovs Arricasis ro Stee, ANALYSIS . Electrometrie Determination of Chromium in Steel Rapid Method for Determining Chromium in Stecl . . 3, Determination of Manganese by the Bismuthate Method 4. Determination of Manganese by the Persnlfate Method 5. Determination of Vanadium . . 6. Determination of Vanadium and Chromiuin in Fervo Vanadium Tue Expcrnomerric DerpraiNarion or Carson IN STBEL Paar 220 + 224, . 227 . 231 21 234 +. 236 - 238 239 243 ~ 243 - 246 248 248, - 252 258 - 259 250 260 - 260 260 261 264 280 283 285 287 288 289 295