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Section 9—Data for 63 Substances

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Section 9—Data for 63 Substances iL BUREAU OF STANDARDS DEC 2 1971 Y\jCi"<- act (^t\00 UNITED STATES DEPARTMENT OF COMMERCE • Maurice H. Stans, Secretary 'OS'^io NATIONAL BUREAU OF STANDARDS • Lewis M. Branscomb, Director Standard X-ray Diffraction Powder Patterns Section 9—Data for 63 Substances Howard E. Swanson, Howard F. McMurdie, Marlene C. Morris Eloise H. Evans, and Boris Paretzkin Assisted by Johan H. DeGroot and Simon J. Carmel Institute for Materials Research National Bureau of Standards Washington, D.C. 20234 National Bureau of Standards Monograph 25—Section 9 Nat. Bur. Stand. (U.S.), Monogr. 25—Section 9, 128 pages (Dec. 1971) CODEN: NBSMA Issued December 1971 For sale by the Superintendent of Documents, U.S. Government Printing Office, Washington, D.C. 20402 (Order by SD Catalog No. C13.44:25/Sec. 9), Price Sl.25. Library of Congress Catalog Card Number: 53-61386 CONTENTS Page Page Introduction 1 Sodium Chromium Oxide Hydrate, Reference intensity values 4 Na^CrO^iH^O 50 Experimental patterns: Sodium Hydrogen Sulfate Hydrate, Ammonium Aluminum Fluoride, (NH^)2AIFg 5 NaHSO^-H^O 52 Ammonium Aluminum Selenate Hydrate, Sodium Iron Fluoride, Na^FeFg 54 NH^AI(SeO^)2-12H20 6 Sodium Selenate, Na^SeO^ 55 Ammonium Copper Chloride Hydrate, Tin Sulfide (berndtite), beta, SnS^ 57 (NH^)2CuCl4-2H20 8 Vanadium, V 58 Zinc Chromium Oxide, ZnCr^O^ Ammonium Iron Fluoride, (NH^)3FeFg 9 59 Zinc Iron Oxide Barium Calcium Tungsten Oxide, (franklinite), ZnFejO^ 60 Calculated patterns: Ba^CaWOg 10 Aluminum Chloride, AICI^ 61 Barium Chloride, BaCI^, (orthorhombic) 11 Barium Oxide, BaO 63 Barium Chloride, BaCI^, (cubic) 13 Beryllium, alpha, Be Barium Titanium Silicate (fresnoite), 64 Beryllium Lanthanum Oxide, Be^La^O^ BaJiSi^Og 14 65 Calcium, Ca 68 Cadmium Iron Oxide, CdFe^O^ 16 Cesium Beryllium Fluoride, CsBeF^ Calcium Titanium Oxide (perovskite), 69 Hydrogen Borate, beta, HBO^ CaTiOj 17 71 Magnesium Phosphate, alpha, Calcium Tungsten Oxide, Ca^WO^ 19 Mg^p^o^ 73 Manganese Cobalt Chromium Oxide, CoCr^O^ 21 Vanadium Oxide, Mn^V^O-, 75 Methanesulfonanilide, Cobalt Iron Oxide, CoFe^O^ 22 CgHj-NH-SO^CHj 78 Nickel Chloride, NiCI^ Lithium Sodium Aluminum Fluoride, 81 Nickel Phosphide, Ni^^P^ cryolithionite, LijNajAI^Fj^ 23 83 Phosphorus Oxide (stable form I), Magnesium Aluminum Oxide (spinel), P^Oj, (orthorhombic) 86 MgAI^O^ (revised) 25 Phosphorus Oxide (stable form II), Magnesium Sulfite Hydrate, P2O5, (orthorhombic) MgSOj-GH^O 26 88 Phosphorus Oxide (metastable form), Manganese Chloride Hydrate, MnCl2"4H20 28 P^Ojg, (rhombohedral) 91 Manganese Cobalt Oxide, MnCo^O^ 30 Potassium Aluminum Sulfate, KAKSO^)^ 31 Potassium Hydrogen Diformate, Potassium Barium Nickel Nitrite, KH(HC00)2 93 K2BaNi(N02)g 32 Potassium Oxalate Perhydrate, Potassium Calcium Nickel Nitrite, ^f^O^^^O^ 96 K2CaNi(N02)6 33 Potassium Sulfate, ^28,20^ 99 Potassium Copper Chloride Hydrate Rubidium Oxalate Perhydrate, (mitscherlichite), K2CuCI^'2H20 34 ^\i^C^O^-H^O^ 102 Potassium Iron Cyanide, K3Fe(CN)g 35 Sodium, Na 105 Potassium Iron Fluoride, K^FeFg 37 Sodium Calcium Carbonate Hydrate, Potassium Nitrite, KNO^ 38 Potassium Oxalate Hydrate, \{f,^0^-H^O 39 pirssonite, Na2Ca(C03)2-2H20 106 Potassium Selenate, K^SeO^ 41 Sodium Molybdenum Oxide, Na^Mo^O^ 110 Potassium Sodium Aluminum Fluoride Trimethylammon4um Chloride, (elpasolite), K^NaAIFg 43 (CH3)3NHCI 113 Rubidium Selenate, Rb^SeO^ 44 Cumulative index to Circular 539, Silver Cyanide, AgCN 46 Volumes 1 through 10, and Monagraph 25, Silver Oxalate, Ag^C^O^ 47 Sections 1 through 9 115 Sodium Chromium Oxiae, Na CrO, 48 Cumulative mineral index 125 iii ) Errata Monograph 25 Section 8, pg. 12; N„ should be 1.486 p Section 8, pgs. 36, 37, 46, 47, 58, 76. Data in the table headings should read: a=3. 16516 and A=l. 54056 Section 8, pg. 68; should be 1.6217 and N should be 1.6330 and N^=l .6435'^as given by Tutton Section 8, pg. 129; both tables are for hexagonal HaH^ and should appear on page 130. Section 8, pgs. 130-131; both tables are for monoclinic HaH^ and should appear on page 129 STANDARD X-RAY DIFFRACTION POWDER PATTERNS NBS Monograph 25, Sections 1, 2, 3 and NBS Circular 539, Volumes 1 thru 10 may be obtained from Mr. Howard E. Swanson, Room A221 , Materials Building, National Bureau of Standards. The following five volumes in this series are available from the Superintendent of Documents, U.S. Government Printing Office, Washington, D.C. , 20402, as follows: NBS Monograph 25, Section 4, 55 cents; Section 5, 55 cents; Section 6, 60 cents; Section 7, $1.50; Section 8, $1.50. (Order by SD Catalog No. C 13.44:25/Sec.— Send orders with remittance for the above five Monographs to Superintendent of Documents, U.S. Government Printing Office, Washington, D.C, 20402. Remittance from foreign countries should include an additional one-fourth of the purchase price for postage. Those wishing to be notified of future issues should send mailing address to the Government Printing Office. iv STANDARD X-RAY DIFFRACTION POWDER PATTERNS Section 9 - Data for 63 substances Howard E. Swanson, Howard F. McMurdie,' Marlene C. Morris/ Eloise H. Evans,^ and Boris Paretzkin^ Assisted by Johan H. deGroot^ and Simon J. Carmel standard x-ray diffraction patterns are presented for 63 substances. Forty of ttiese patterns represent experimental data and 23 are calculated. The experimental x-ray powder diffraction patterns were obtained with an x-ray diffractometer. All d-values were assigned Miller indices determined by comparison with computer interplanar spacings consistent with space group extinctions. The densities and lattice constants were calculated, and the refractive indices were measured whenever possible. The calculated x-ray powder diffraction patterns were computed from published crystal structure data. Both peak height and integrated intensities are reported for the calculated patterns. Key words: Crystal structure; integrated intensities; lattice constants; peak intensities; powder patterns; reference intensities; standard; x-ray diffraction. INTRODUCTION Optical data, color. A microscopic inspection for phase purity was also made on the non-opaque materials during the refractive index determination. The latter was done by grain-immersion methods in white light, with oils The Powder Diffraction File is a compilation of diffraction standardized patterns, gathered from many sources, produced, and published in sodium light, in the refractive index range 1.40 to 2.1. by the Joint Committee on Powder Diffraction Standards.^ The [Hartshorne and Stuart, I960]. The names of the File is used for identification of crystalline materials by sample colors were selected from the matching d-spacings and diffraction intensity measurements. ISCC-NBS Centroid Color Charts. Under the partial sponsorship of the Joint Committee, our program at the National Bureau of Standards contributes new Structure, lattice constants. The space groups data to this File. Our work also aids in the evaluation and are listed with short Hermann-Mauguin symbols as well as the revision of published x-ray data and in the development of space group numbers given in the International Tables for report presents information for diffraction techniques. This 63 X-ray Crystallography Vol. I [1952j. compounds (40 experimental and 23 calculated patterns), and Orthorhombic cell dimensions were arranged according to is the nineteenth of the series of "Standard X-ray Diffraction the Dana convention b>a>c [Palache et al., 1944]. Powder Patterns".* A computer program [Evans et al., 1963] assigned hke's and refined the lattice constants. Cell refinement was based EXPERIMENTAL POWDER PATTERNS only upon le values which could be indexed without ambi- guity. In indexing cubic patterns, multiple hkx's were not Sample. The samples used to make NBS patterns were reported; instead, we chose the single appropriate index obtained from a variety of sources or were prepared in small having the largest h. The number of significant figures reported quantities in our laboratory. Appropriate annealing, recrystal- for d-values varied with the symmetry and crystallinity of each lizing, or heating in hydrothermal bombs improved the quality sample. Unit cell constants and their standard errors were' of most of the patterns. A check of phase purity was usually based on least-squares refinement of the variance-covariance provided by indexing the x-ray pattern. matrix derived from the unweighted residuals. Densities. These were calculated from the NBS lattice constants, the Avogadro number (6.06252 x 10^^), and atomic Consultant and Research Associates, respectively, of the Joint Committee on weights based on carbon 12 [International Union, 1961]. Powder Diffraction Standards Associateship at the National Bureau of Standards. Interplanar spacings. For spacing determinations, a Joint Committee on Powder Diffraction Standards, 1601 Park Lane ,Swarthmore, shallow holder was packed with a sample mixed with an Pa. 19081. This Pennsylvania non-profit corporation functions in cooperation with the American Society for Testing and Materials, the American Crystallo- internal standard (approximately 5 wt. percent tungsten graphic Association, The Institute of Physics, the National Association of powder). When tungsten lines were found to interfere, approxi- Corrosion Engineers, the American Ceramic Society, the Mineralogical Society mately 25 wt. percent powdered silver was used in place of of America, and the Canadian Mineralogical Society. tungsten. If the internal standard correction varied along the length of the pattern, linear interpolations were used. To avoid 'See previous page for listing of other published volumes. aberrations at the very top of the peak, the reading of le was taken at a position about 20 percent of the way down from the top, and in the center of the peak width. The internal standard powder did not flow readily, or was prone to orient ex- correction appropriate to each region was then applied to the cessively, approximately 50 volume percent of finely ground measured value of le. We have reported all data as K^j peaks silica-gel was added as a diluent.
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