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Systematic Analysis of Silicates

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Systematic Analysis of Silicates Systematic Analysis of Silicates By LEE C. PECK GEOLOGICAL SURVEY BULLETIN 1170 Methods for silicate analysis and a discussion of problems involved in their use UNITED STATES GOVERNMENT PRINTING OFFICE, WASHINGTON : 1964 UNITED STATES DEPARTMENT OF THE INTERIOR STEWART L. UDALL, Secretary GEOLOGICAL SURVEY Thomas B. Nolan, Director The U.S. Geological Survey Library has catalogued this publication as follows : Peck, Lee C 1904- Systematic analysis of silicates. Washington, U.S. Govt. Print. Off., 1964. iv, 89 p. illus., diagrs. (part fold, in pocket) tables. 24cm. (U.S. Geological Survey. Bulletin 1170) Bibliography: p.88-89. 1.Silicates. 2.Rocks Analysis. 4.Geochemistry. I.Title. (Series) For sale by the Superintendent of Documents, U.S. Government Printing Office Washington, D.C. 20402 Page Abstract__ ________________-_____-_-_-_____-____--------_-------_ 1 Introduction. ___._____..-____-______-_._.._.---_.--_---__-_-._---- 1 Special equipment_--________-_____-_--__-_-_-_--_-__---_---------- 2 Discussion of the methods___--__-----------__---------------------- 2 Foreword to the geologist_.__._________._.____._-_-_____-.-_-_ 2 Sample preparation. __._---_____--_----_--_----_----_---------- 10 Total water_ ............................................^... 17 Moisture......_____-.__.-_.-_-_--.-_.-.-_--_-_.-----.--_-_--- 20 Silica. ....................................................... 21 Ammonium hydroxide group___-___-_--__.-____.-_---.---__-_-.. 26 Removal of manganese.-.-------------------------------------. 30 Calcium oxide_________.-._.__---_-__..-_.._.--.--...._------ 31 Magnesium oxide_ ^.......................................... 33 Recovery of silica__-_ _-_-_--_----__-_-----_-_--..._--_-_--_- 35 Titanium oxide___ ..............................^............ 36 Total iron oxide.-_-_-_-_--__--__-_-_---_--_----------_---_-_-- 37 Ferrous oxide..._-.--..._.___._.----_.__---_--_----.._-_-__.-. 39 The alkalis........____..___..__.._-------_____. 42 Manganese and phosphorus oxides...____..____.._._.__.__._.__._ 45 Carbon dioxide.,.-.--..._._...--__-.._-_ _---__-_---._--_ 48 Barium oxide._________________________________________________ 50 Total sulfur__-_-----.---....-.---.___--_-------.-_-------_ 51 Sulfur trioxide.-..-_-.__--.-___.--___-__--__-------.__-_--__.. 52 Standard procedures._----___--_----.-----___-----__--.-------_-_-_ 53 Foreword to the analy8t_-_---__-_---__--_--_-__----------__--_- 53 General instructions.___..-..____.___..__-_----..--__...._____. 57 Weighing._-___....-_..._...__--._.._..___._-._.__._._..._ 57 Colorimetry__ _ -_-_-__-_._---------_----_-----_--__-._.. 58 Electric radiator_______.__..____...___._.____._____._____ 59 Globar furnace.------------_--____--__----__---____-____-_ 59 Sample preparation._-_----_-_--_--__--._--_----_-.-.-._._-..-. 60 Total water_________________________________________________ 61 Moisture (H2O-)------------------------_------__-------- 61 Silica.-_-..._-------..--....._.----_.----_---..---_..._..._.- 62 Ammonium hydroxide group...-.._--___-__-_.____-___.___.__.__ 64 Removal of manganese._---..____--_----------.__-_--__._.__._- 66 Calcium oxide__-_-____-_---____--_-------_----_______.__-___ 67 Magnesium oxide._ ..................i......................... 68 Recovery of silica____________________________________________ 69 Titanium oxide___----_---_---------------_-_--_--_----__---_ 70 Total iron oxide.---------_---------------------__----_-___--._ 72 Ferrous oxide.---------_--___------------_----_-_---__-___-_-_ 73 The alkalis..-------------------.--------_-------_-.-.-_-.--_. 73 in IV CONTENTS Standard procedures Continued Page Manganese and phosphorus oxides_______________________________ 76 Preliminary procedure__--__-_-------____--____-__________ 76 Manganese oxide._________________________________________ 77 Phosphorus oxide__________________________________________ 78 Carbon dioxide..________________________________________'______ 79. Barium oxide_________________________________________________ 80 Total sulfur___._____.______________1__._____________________ 82 Sulfur trioxide._______________________________________________ 82 Preparation of apparatus and reagents._-_-_-__--___--_______..______ 83 Total water______._______...._____________ 83 Ammonium hydroxide group________--___:.______________-_______ 83 Removal of manganese..____.---______-._-.__--_.-.___-__-_____ 83 Calcium oxide.________________________________________________ 84 Magnesium oxide____________________________________________ 84 Titanium oxide______--__________-_-____.___...____..__._____ 84 Total iron oxide.______________________________________________ 85 Ferrous oxide.________________________________________________ 86 The alkalis...._____.-___.____________________________ 86 Manganese and phosphorus oxides.______________________________ 86 Carbon dioxide._______________________________________________ 88 Sulfur__________....._________________________________ 88 Sulfur trioxide________________________________________________ 88 Literature cited.___-___---_-____-___-_-____-__._____________---___ 88 ILLUSTRATIONS [All plates are In pocket] PLATE 1. Details of Globar furnace. 2. Details of electric radiator. 3. Details of desiccator. 4. Details of total water furnace. Page FIGURE 1. Laboratory arrangement._______________--__-_-___----_-_ 3 2. Hood___--_----_--___----_----_ _-___--_--_--_.__----- 4 3. Globarfurnace_-__-___----___----_----_-_--_----___-_--- 5 4. Electric radiators_____________--__--____-_____-__-__---_- 6 5. Funnel racks____________________________^________-____ 7 6. Spray trap______^_________--____-__-__-__-_-----.--__- 8 7. Silver reductor._________________________________________ 9 8. Four-chamber desiccator.__---__--_--_---_--.------------ 10 9. Sample splitter.._________________________.-__--__-.----_ It 10. Sample mixer_______________________---_-___--_---_---_- 12 11. Carbon dioxide apparatus.. __--__-_----------_----------- 13 12. Total water furnace_____________-_---_---_------------ 14 13. Accessory equipment for total water determination.____-___. 15 14. Apparatus used for the determination of ferrous oxide _____ 17 15. Flow diagram of carbon dioxide apparatus.-_--------------- 79 SYSTEMATIC ANALYSIS OF SILICATES By LEE C. PECK ABSTRACT Detailed procedures are given for the analysis for 17 constituents commonly present in silicates: SIO2, A12O3, Pe203, FeO, MgO, CaO, Na2O, K2O, H2O+, H2O-, TiO2, P205, MnO, C02, BaO, total S, and SO3. Problems in analysis that may occur are also discussed. The use of special equipment to facilitate analysis is stressed. INTRODUCTION Methods are described in this bulletin for the determination of constituents that, in the Geological Survey, compose a "standard analysis" (SiO2, A1203, Fe2O3, FeO, MgO, CaO, Na2O, K20, H2O+, H2O-, Ti02, P2O5, MnO, and CO2) and for the determination of BaO, total S, and SO3. -Once the basic techniques required for the analysis of these constituents-are mastered, they may be easily ap­ plied to the determination of additional constituents. Although this bulletin is primarily a manual for the instruction of beginners, in both the Geological Survey and other laboratories, rather than a comprehensive treatise on the subject of silicate analy­ sis, it is directed also to experienced analysts who would like to com­ pare procedures and to the geologists who must interpret the data furnished by analysts. Most of the so-called conventional methods .date back to the 19th century, and the ones "described in this manual do not differ basi­ cally from similar ones described in available texts. The speed of these methods, however, has been increased by the use of special equipment. Detailed procedures for three relatively, new methods are given: the use of the silver reductor for the determination of total iron oxide, Kitson and Mellon's method for the determination of phosphorus, and the removal of manganese before the determination of cajcium and magnesium. Special equipment is described in the immediately following sec­ tion; the methods are explained, conditions are listed under which these methods failj and some modified procedures are given for the analysis of unusual samples under "Discussion of the methods," page 2; detailed .procedures are given under "Standard procedures," 2 SYSTEMATIC ANALYSIS OF SILICATES page 53; and the preparation of apparatus and reagents is described in the section "Apparatus and reagents," page 83. SPECIAL EQUIPMENT Although excellent analyses have been made by using standard items of equipment, time is saved, techniques are simplified, the number of accidents is reduced, and the reproducibility of results is improved by the use of special apparatus. Thus, if adequate amounts of automatically controlled equipment are available, several operations that do not require the attention of the analyst can be carried out concurrently. Making a pyrosulfate fusion is simple when an electric radiator is used, but making this fusion without loss over a burner requires skill. Accidental boiling over or spat­ tering of a solution containing solids can be largely eliminated by the use of electrical equipment whose temperatures can be repro­ duced. It is difficult to bring some precipitates to their equilibrium weights by heating them over burners, sometimes because of insuffi­ cient temperature and sometimes because of variable temperatures from burner to burner. The reproducible high temperature of the Globar furnace eliminates this difficulty, and as the furnace can be brought to temperature in
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