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The Analysis of Silicate and Carbonate Rocks

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The Analysis of Silicate and Carbonate Rocks DEPARTMENT OF THE INTERIOR UNITED STATES GEOLOGICAL SURVEY GEORGE OTIS SMITH, DIRECTOR 422 THE ANALYSIS OF SILICATE AND CARBONATE ROCKS A REVISION OF BULLETIN BY W. F. HILLEBRAND CONTENTS. Page. Introduction.............................................................. 13 Object and scope of the present treatise................................ 13 Acknowledgments.................................................... 15 Silicate rock analysis.............:........................................ 16 Part I. Introduction.................................................. 16 1. Importance of complete and thorough analyses .................. 16 2. The constituents occurring in silicate rocks ...................... 22 3. The distribution and occurrence of certain minor constituents..... 23 4. Summation of analytical results and limits of allowable error ..... 27 5. Statement of analyses.......................................... 29 6. Time needed for making an analysis............................ 30 7. Useful appliances and apparatus.......................'......... ' 30 A. Crucible tongs............................................ 30 B. Kadiators for volatilizing liquids and solids.................. 31 C. Perforated disk for crucibles................................ 32 D. Weighing scoop or trough................................... 33 E. Colorimeters.............................................. 33 a. First Survey form ..................................... 33 b. Second Survey form (Steiger's)......................... 35 c. Schreiner's form.....................................'.. 37 8. Preliminary qualitative analysis................................ 38 9. Quality of reagents............................................. 39 Part II. Methods applicable to silicate rocks........................... 41 1. Introductory remarks...'....................................... 41 2. Specific gravity (porosity).......... '. ............................ 43 General remarks............................................. 43 A. By suspension in water.................................... 43 a. Ordinary method for specific gravity.................... 43 b. Method for specific gravity and porosity combined.....'.. 45 c. Penfield's method for mineral fragments................. 46 B. Pycnometer method....................................... 47 a. Ordinary method.................................... .. 47 b. Kefined method ,. s..................................... 48 C. Heavy solutions not suitable for rocks ...................... 50 3. Preparation of sample for analysis .............................. 50 A. Quantity of rock to be crushed............................. 50 B. Crushing..................................'............... 50 a. Survey methods...................................... 50 b. Washington's method................................. 52 C. Grinding ................................................. 52 . D. Abrasion of mortar and pestle.............................. 56 E. Weight of sample ......................................... 56 3 4 CONTENTS. Silicate rock analysis Continued. Part II. Methods applicable to silicate rocks Continued. Page. 4. Water. General considerations....... ......................... 57 A. The r61e of hydrogen in minerals.......................... 57 B. Water taken up or lost on grinding........................ 64 C. Importance of employing air-dry powder for analysis........ 65 D. Argument in favor of including hygroscopic water in the summation.............................................. 66 5. Water. Methods of determination.............................. 67 A. Indirect methods. ......................................... 67 a. General considerations................................. 67 b. Methods involving the use of dehydrating agents"..'...... 67 c. Methods involving application of heat................... 69 a. Fractional determinations.......................... 69 P. "Loss on ignition" method for total water.......... 71 B. Direct methods without absorption tubes Penfield's methods. 72, a. For minerals easily deprived of their water.............. 72 b. For minerals not easily deprived of theircwater.......... 73 C. Direct methods with absorption tubes................... 1.. 73 a. General considerations................................. 73 b. Penfield's procedure................................1.. 74 c. Steiger's application of the toluene oven................ 75 d. Chatard's oven for temperatures up to 300° and over..... 76 e. Gooch's apparatus..................................... 78 f. Merits of the above forms of apparatus.................. 82 g. Jannasch'smethods...........'......................... 82 6. Silica, separation from alumina, etc............................. 83 A. Alternative methods of decomposing the rock............... 83 a. General considerations.................................. ' 83 b. Decomposition of refractory silicates by hydrochloric acid under pressure...................................... 85 c. The boric-oxide method of Jannasch and Heidenreich... 86 a. Preparation of the boric oxide...................... 86 ft. Treatment of easily decomposable silicates........... 86 y. Treatment of refractory silicates.................... 86 S. Further treatment after fusion...................... 87 s. Possible objections to the boric-oxide method-....... 87 d. The sodium-carbonate method.......................... 87 a. Advantages of sodium carbonate over sodium potas­ sium carbonate.................................. 87 /?. Purity of the sodium carbonate.................... 88 y. The fusion with normal sodium carbonate.......... 88 8. Fusion with sodium bicarbonate.................... 90 £. Treatment after fusion.............................. 90 B. Subsequent treatment..................................... 91 a. Separation of silica.................................... 91 a. Reasons for adoption of accepted procedure......... 91 /3. Procedure in absence of notable amounts of fluorine. 92 y. Procedure with rocks" and minerals containing fluorine. 94 b. Ignition of silica...................................... 94 c. Correction for impurities in the silica................... 95 d. Accuracy of the silica determination .................... 96 e. Composition of the residue obtained from the silica '...... 96 f. Platinum in filtrates.............................'....... 97 7. Metal precipitable by hydrogen sulphide....................... 98 CONTENTS. 5 Silicate rock analysis Continued. Part II. Methods applicable to silicate rocks Continued. Page. 8. Aluminum total iron......................................... 98 A. Indirect method for aluminum (titanium).................. 98 a. Preliminary remarks................................... 98 b. Precipitation of aluminum, iron, etc., without precipitat­ ing manganese.................................. 99 a. Precipitation by ammonia......................... 99 j3. The basic-acetate precipitation..................... 100 c. Precipitation of 'iron, aluminum, etc., together with manganese...................................... 102 a. By ammonia and ammonium persulphate.......... 102 ft. By ammonia and ammonium sulphide.............. 103 d. Kecovery of iron and aluminum from the filtrates....... 103 a. After an ammonia precipitation.................... 103 ft. After a basic-acetate precipitation.................. 103 y. After precipitation by ammonia and ammonium persulphate..................................... 104 e. Ignition of the precipitate of iron, aluminum,' etc., oxides.. 104 f. Recovery of silica and possible barium in the alumina pre­ cipitate. ........................................ 105 a. Silica............................................. 105 P. Barium........................................... 107 B. Determination of iron in the precipitate of alumina, etc...... 107 a. Without regard to the presence of vanadium.... t ....... 107 a. Eeduction of the iron............................. 107 ft. Titration of the iron............................... 108 y. Further treatment of the solution after titration..... 109 b. Having regard to the presence of vanadium............. 109 c. Determination of the true value for ferric iron........... 110 C. Methods aiming at the more or less direct determination of aluminum .......................................... Ill a. After first removing iron as sulphide.................... Ill b. By extraction with a fixed caustic alkali................ Ill c. Methods of Dittrich.................................... 112 d. Direct precipitation of aluminum by phenylhydrazine... 112 9. Manganese, nickel, cobalt, copper, and zinc..................... 113 A. Difficulties in the way of a correct gravimetric determination of manganese........................................... 113 B. Precipitation of the group and separation of its constituents.. 114 a. The ammonium-sulphide method....................... 114 a. Its advantages and disadvantages.................. 114 ft. Precipitation by ammonium sulphide and separation of manganese and zinc from nickel, cobalt, and copper. 11.5 b. Manganese and /inc................................... 115 c. Nickel, cobalt, copper.................................. 116 C. Colorimetric determination of manganese................... 116 a. Preliminary treatment................................. 116 b. Colorimetric determination of manganese by ammonium persulphate......................................... 117 10. Calcium and strontium (barium)............................... 118 A. Separation from magnesium...............................
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