The Methods of the Chemists of the United States Steel Corporation for the Sampling and Analysis of Ferro-alloys and Bearing Metals

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Stevenson & Foster Company, 1920 - Steel - 71 pages
 

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Page 15 - One gram of the sample is transferred to a porcelain dish, dissolved in 15 cc. of hydrochloric acid, and the solution is evaporated to dryness. The residue is dissolved in 50 cc.
Page 65 - Standard sodium thiosulphate solution (about 25 grams per liter) is added until the yellow color becomes faint, when lOcc. of starch solution are added, and the titration is continued until the blue color is bleached. In the same manner, 25 cc. of a deci-normal potassium permanganate solution are added to a beaker containing 400 cc. of water, 10 cc. of 10% potassium iodide solution, and 10 cc. of hydrochloric acid (1:1); the resultant iodine is titrated with sodium thiosulphate solution. The permanganate...
Page 21 - ... of iron in the sample. PHOSPHORUS. One gram of the alloy is fused in a platinum crucible with 10 grams of sodium carbonate and 1 gram sodium nitrate. The fusion is leached with water, and the solution boiled and filtered. The filtrate is acidified with hydrochloric acid and evaporated to dryness.
Page 13 - ... thoroughly, and set aside for a day or two with occasional shaking. After the final subsidence of the heavier residue, the starch solution is siphoned into a container and the settlings rejected. The zinc chloride is added as a preservative. Preliminary boiling of water tends to lessen frothing, or the formation of large bubbles on the addition of the starch. Standard Iodine or lodate Solution. Ten grams of potassium iodide and 4.5 grams of resublimed iodine are transferred to a one liter flask,...
Page 11 - ... acid. The dish is cooled, 35 cc. of concentrated hydrochloric acid are added and heat is applied until the soluble salts are again dissolved. The cover is removed, and with the dish placed upon a suitable asbestos ring in order to prevent the formation of a crust of the metallic salts upon the sides, the solution is evaporated to the first appearance of the separation of the chlorides, which are then dissolved by the addition of a few drops of concentrated hydrochloric acid; three drops should...
Page 49 - Volumetric Method The nitric acid solution of the impure copper oxide in the No. 2 beaker obtained as above described, is rapidly evaporated to the removal of the bulk of the free acid, and the solution diluted with cold water to volume of 150 cc. Strong ammonia is then added from a burette until the addition of a final drop causes the permanent blueing of the solution, after which there is added by means of a pipette six drops of acetic acid.
Page 60 - After the copper sulphide has settled, it is removed on a paper and well washed with hydrogen sulphide water containing a little sulphuric acid. The precipitate and paper are ignited in a tared platinum crucible, cooled and weighed immediately to prevent absorption of moisture by the copper oxide, which is hygroscopic. The weight of the oxide multiplied by the factor 79.89 and divided by the weight of the sample taken gives the percentage of copper. If desired, the ignited copper oxide may be dissolved...
Page 45 - ... water. In no case is the funnel permitted to become entirely empty, and the stop-cock is closed while some of the wash water still remains above the surface of the zinc. By working in this way, no air is permitted to pass through the reductor. The molybdenum salt is green as it passes through the lower part of the reductor, but on coming in contact with the ferric salt it is changed to a bright red, due to its immediate partial oxidation, which is, of course, accompanied by reduction of a corresponding...
Page 45 - In no case is the funnel permitted to become entirely empty, and the stop-cock is closed while some of the wash water still remains above the surface of the zinc. By working in this way, no air is permitted to pass through the reductor. The molybdenum salt is green as it passes through the lower part of the reductor, but on coming in contact with the ferric salt it is changed to a bright red, due to its immediate partial oxidation, which is, of course, accompanied by reduction of a corresponding...
Page 44 - After allowing it to cool somewhat, 5 cc. of nitric acid (sp.gr. 1.42) are added and the evaporation is repeated. The evaporation with 5 cc. portions of strong nitric acid is repeated several times until the filter paper has been completely destroyed and every trace of yellow color, due to carbonaceous matter, has disappeared. When this has been accomplished the solution is fumed strongly for a short while, cooled, 5 cc. of water are added and the liquid is again taken to fumes of sulphur trioxide...

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