X - R A X DIFFRACTOMETER STUDIES OF SOME VAUADIUM SILICATES By John C, Hathaway Trace Elements Inveetigations Report UNITED STATES DEPARHMEIlfT 07 tERE UTTERIOR GEOLOGICAL SURVEY IN REPLY REFER TOt UNITED STATES DEPARTMENT OF THE INTERIOR GEOLOGICAL SURVEY WASHINGTON 25. D.C. AEC-275/6 October 26. 1955 Mr * Robert D. Hininger, Assistant Director Division of Raw Materials U0 S» Atomic Energy Commission Washington 25, D. C» Dear Bob; Transmitted herewith are three copies of EEI-^S, "X-ray diffractometer studies of some vanadium silicates," by John C, Eathaway* This report was prepared entirely on Geological Survey funds, but we are transmitting it to you because we believe that it will be of interest to geologists and mineralogists working on the Atomic Energy Commission program. ¥e plan to publish this report in the proceedings of the National Clay Conference. Sincerely yours, W. H. Bradley Chief Geologist JAN 2 3 2001 Geology and Mineralogy This document consists of 21 pages Series A. UNITED STATES DEPARTMENT OF THE INTERIOR GEOLOGICAL SURVEY X-RAY DIFFRACTOMETER STUDIES OF SOME VANADIUM SILICATES By John C, Eathaway September 1955 Trace Elements Investigations Report This preliminary report is distributed without editorial and technical review for conformity with official standards and nomenclature* It is not for public inspection or quotation. USGS - GEOLOGY AHD MINERALOGY Distribution (Series A) Ho. of copies Argonne National Laboratory .»»*».„,.„.„.*.»<,.»*».,**»„„».....<.,. 1 Atomic Energy Commission, Washington I**,.........,.......,...... 2 Division of Raw Materials, Albuquerque ......»«.»..,.........».. 1 Division of Raw Materials, Butte »»..,.......•........*......... 1 Division of Raw Materials, Casper .,*„„*..»,„.„„«,...»..„..»*... 1 Division of Raw Materials, Denver .,.„„„„„„,»<..«,„„,,,,,«,,,«,,,„,,<,,,„*,,„ 1 Division of Raw Materials, Hot Springs ....»..*... .*.,««».,,».,» 1 Division of Raw Materials, Ishpeming „,,. „„,„„.. 0 «,..„...„.„,,... 1 Division of Raw Materials, Phoenix e .,» 0 ,«.....o.o...,«,o«, *,..... 1 Division of Raw Materials, St. George ... e »..,, 0 « 0 .o 0 ,„.,„„«,«.,„ 1 Division of Raw Materials, Salt Lake City ..,...»..«,.....»*..„, 1 Division of Raw Materials, Washington „.„.„„•.........«....»•».. 3 Exploration Division, Grand Junction Operations Office „„«.«.„„.. 1 Grand Junction Operations Office ....,..........*....»...,...... 1 Technical Information Service, Oak Ridge *......,...........«... 6 Tennessee Valley Authority, Wilson Dam .„..,.«,...,..=... = ..,«,..,. 1 U. So Geological Surveys Fuels Branch, Washington B . 00 ,...... ..,,.,..,,«,,«,,-...««».„>»*.. 1 Geochemistry and Petrology Branch, Washington ...«...*....»<,*... 20 Geophysics Branch, Washington ......,..»..„„„„„,,.»„.«.,»«,„«*,,»,,..,» 1 Mineral Deposits Branch, Washington ........ 0 * 8 ,.... 0 .. „.„..„„„„ 1 E„ H„ Bailey, Menlo Park ae . 0 . 0 ,..,«,» 0 ...,.«,.. 0 .»....o.. 0 ..«.. 0 o 1 A. L, Brokaw, Grand Junction ...«»o 0 . 0 .«*-»».«. OB »»«»««.».«eo.«.» 1 N» M. Denson, Denver .,.».........».„..«,«,««,.»...««.».„..»«... 1 R. L 0 Griggs,, Albuquerque .................................oo....*. 1 M» R. Klepper, Spokane ...*„. .. ew . oe ,o.,..,»....««.« e .«»«.o.«.««..« 1 A, H. Koschmann, Denver ................ p .,....,.....*.,,.*...». 1 L. R0 Page, Washington o..,..,o.... f ....«o.».o*,».«,..»*.,.«.... 1 Q, D, Singewald, Beltsville .........ft.....,...*..*.*.........*. 1 A. E. Weissenborn, Spokane .»..,..«.„.»».....*.„..*..,,....»»..... 1 TEPCO, Denver .................................................. 2 TEPCO, EPS, Washington, (including master) ......,*....»...*,... 2 65" CONSENTS Page Introduction <>« e „ *«»»».. oo a ««»aa«*»»a»a<><»a«p4» <.ooae..>.>aoaa«att»a*<>ao 4 .KeSUJL uS ao»aQ»a4oaoe»«4¥0G»a»aaoeaao<tQaao*»<ya4<yaoQa*ox>g>aoo4»ooa» O Conclus ions ,«****.,+**.*«. + *.**.*.„,***«„,»,<,* t>aa <xttta. 000 * a * a.*.». 19 ILLUSTRATIOIS Page Figure 1. X-ray diffraction patterns of two roscoelite samples . 7 2. Comparison of X-ray diffraction patterns of oriented of roseoelite and glauconite „.«.«.. = „..„.. 10 X-ray diffraction patterns of oriented aggregates of five Colorado Plateau samples in which mica is the principal constituent ... 0 . 0 , BOO ooo«,<,a 00000 oo oa .«<,oo <.* 11 X-ray diffraction patterns showing expansion of vanadium silicates treated with ethylene glyeol 0 «,««». 13 5. X-ray diffraction patterns of AW-67-5- (a mixture of two or more minerals ) showing shift in peaks caused "by treating with ethylene glyeol and "by heating 0 « » 0 . » 15 6. X-ray diffraction patterns of sample G-53-53 untreated, after ethylene glyeol treatment , and after heating . 16 7. X-ray diffraction patterns of oriented aggregates of two samples from the Mineral Joe mine, Mont-rose County, X-RAY DIFFRACTOMETER STUDIES OF SOME VAHADH3M SILICATES By John C a Eathavay ABSTRACT A group of claylike silicates containing vanadium nave been examined by X-ray diffraction methods to determine their mineralogic composition. The results indicate that mica and chlorite are the principal minerals. The micas resemble roscoelite but depart from it in two different ways;; by interstratification with montmorillonitic layers and by -variation in octahedral substitution. Some of the chlorites also exhibit mixed-layered expanding structures, but no interstratification of mica and chlorite layers has yet beep noted. The chlorites show some variation in the temperature of decomposition, presumably because of differences in composition and degree of crystallinity,, IMEOBUCTIOI Identification of the claylike materials occurring in zones of vana­ dium mineralization in the sandstone type deposits of the Colorado Plateaus is often hampered by the fine particle size and poor crystallinity of these materials, although mica-type minerals have been recognized through usual X-ray diffraction methods and have been variously reported as roscoelite or vanadium hydromica. In this investigation, X-ray diffraction procedures commonly used in the study of clay minerals have been applied to the problem of differentiating these poorly crystalline materials„ Materials The samples studied were as followss AMNH 13565, roscoelite, Coloma, California ALB~3^-5^» roscoelite, Fall Creek mine, Placerville, Colorado AW-207-5^A, vanadium silicate from oxidized ore, Rifle, Colorado AW-207*!i&B, vanadium silicate from unoxidized ore, Rifle, Colorado A¥~1^6-52, vanadium silicate from Cougar mine, San Miguel County, Colorado AW-lW—52, vanadium silicate from Sunnyside mine, east of Carrizo Mountains, San Juan County, New Mexico AW-67-51, vanadium silicate, Little Pittsburg Ko. 5 mine, Thompson district, Grand County, Utah G-53-53? vanadium silicate, Bitter Creek mine, Montrose County, Colorado p-l-M-53» Mineral Joe mine, Jo Dandy group, Paradox Valley, Montrose County, Colorado P-l-P-53* Mineral Joe mine, Jo Bandy group, Paradox Yalley, Montrose County, *, Colorado Procedure All of the samples except AMNH 13565, p-l-M-53, and P-l-P-53 had previ­ ously been purified by water elutriation, bromoform separation, or both* Sample AMNE 13565 consisted of a group of fairly pure roseoelite crystals and therefore did not require further separation,, A portion of these crystals was crushed in a mullite mortar to pass a 230-mesh sieve. This material as well as a portion of each of the other purified samples were placed in plastic test tubes and dispersed in distilled water using a motor-driven brush« A small amount of sodium metaphosphate was added to each sample as a dispersing agent. 6 Oriented aggregates were prepared "by pipetting portions of each suspension onto each of three glass slides. The suspension remaining in the test tube •was allowed to stand about four hours and the material still in suspension at the end of this time -was pipetted on three additional slides. The mate­ rial placed on these two groups of slides will hereinafter "be referred to as coarse and fine, respectively. Samples P-l-M-53 and P-l-P-53 were dispersed in distilled water, wet sieved to remove particles larger than 62|i, further dispersed using an end- over-end shaker, and centrifuged repeatedly to separate the silt (2-62|x) and clay (<2u) fractions. Excess water was removed from the clay fraction using porcelain filter candles under vacuum and portions of the resulting concentrated suspensions were pipetted onto glass slides. The remaining suspensions were dried at room temperature and the clay removed and crushed, X-ray diffractometer patterns were made for each sample as follows: Oriented aggregates 1. Untreated 2. Treated with ethylene glycol 3* Heated to kQQ° C b. Heated to 500° C 5, Treated with hot concentrated HC1 (samples AMNH 13565, AW-67-51, G-53-53, P-l-M-53, and P-l-P-53 only) Randomly oriented powder (samples AMNH 13565, ALB-31i-5^> P-l-M-53, and P-l-P-53, only) Results In figure 1 a comparison is shown "between the X-ray diffractometer patterns of minerals which have "been identified "by chemical and optical Oriented Randomly oriented powders ir\ o 30 20 10 Degrees 20 CuKa radiation Figure 1,—X~ray diffraction patterns of two roscoelite samples methods as roscoelite. Most of the apparent differences in the randomly oriented powder patterns are the result of the much higher degree of pre­ ferred orientation that occurred in the preparation of the mount for sample AMNH 13565" Otherwise both samples exhibit similar patterns except that the peak marked "A" at 33»^° 2© in the randomly oriented powder pattern for sample AMM 135&5 is ncrb evident in ALB»3^-5^ aa& calcite is present in