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Standard X-Ray Diffraction Powder Patterns

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Standard X-Ray Diffraction Powder Patterns ^356 OCT 3 NBS CIRCULAR ;r\f tn '- ‘ 08y KH J i. u VOLUME 6 a ,, arv. Standard X-ray Diffraction Powder Patterns UNITED STATES DEPARTMENT OF COMMERCE NATIONAL BUREAU OF STANDARDS Standard X-ray Diffraction Powder Patterns The five previously issued volumes in this series are avail- able from the Superintendent of Documents, U. S. Govern- ment Printing Office, Washington 25, D. C., as follows: NBS Circular 539, Volume 1, Standard X-ray Diffraction Powder Patterns (Data for 54 inorganic substances) NBS Circular 539, Volume 2, Standard X-ray Diffraction Powder Patterns (Data for 30 inorganic substances) NBS Circular 539, Volume 3, Standard X-ray Diffraction Powder Patterns (Data for 34 inorganic substances) NBS Circular 539, Volume 4, Standard X-ray Diffraction Powder Patterns (Data for 42 inorganic substances) NBS Circular 539, Volume 5, Standard X-ray Diffraction Powder Patterns (Data for 45 inorganic substances) The price of each volume is 45 cents. Send orders with remittance to: Superintendent of Documents, Government Printing Office, Washington 25, D. C. UNITED STATES DEPARTMENT OF COMMERCE . Sinclair Weeks, Secretary NATIONAL BUREAU OF STANDARDS • A. V. Astin, Director Standard X-ray Diffraction Powder Patterns Howard E. Swanson, Nancy T. Gilfrich, and Marlene I. Cook National Bureau of Standards Circular 5^ Volume 6, Issued September 26, 1956 For sale by the Superintendent of Documents, U. S. Government Printing Office, Washington 25, D, C. Price 40 cents Contents Page Page Introduction 1 Standard X-ray powder patterns—Continued Standard X-ray powder patterns: Potassium aluminum sulfate dodecahydrate, Ammonium aluminum sulfate dodecahydrate, - KA1 (S0 4) 2 1 2H 2 0 36 3 NH 4 A1(S0 4) 2 -12H 2 0 Potassium chlorostannate, K 2 SnCl8 38 Ammonium chloropalladite, (NH 4 ) 2 PdCl 4 6 Potassium chromium sulfate dodecahydrate, chromium sulfate dodecahydrate, Ammonium KCr(S0 4) 2 -12H 2 0 39 -12H 7 NH 4 Cr(S04) 2 2 0 Potassium fiuogermanate, K2 GeF6 41 fiuogermanate, 8 Ammonium (NH 4 ) 2 GeF6 Potassium fluoplatinate, Iv2 PtF 6 42 gallium sulfate dodecahydrate, Ammonium Potassium perchlorate, KC10 4 43 -12H 9 NH 4 Ga(S0 4) 2 2 0 Rubidium aluminum sulfate dodecahydrate, Ammonium iron sulfate dodecahydrate, NH 4 Fe RbAl(S0 4) 2 -12H 20 44 (S04 ) 2 -12H 2 0 10 Rubidium chlorostannate, Rb2 SnCle 46 Ammonium sulfate (mascagnite) (NH 4 ) 2 S0 4 __ 12 , Rubidium chromium sulfate dodecahydrate, Ammonium zirconium fluoride, (NH 4) 3 ZrF7 14 RbCr(S0 4) 2 -12H 2 0 47 Antimony(III) iodide, Sbl 3 16 Rubidium fluoplatinate, Rb 2 PtF6 48 Arsenic (III) iodide, Asl 3 17 Rubidium fluosilicate, Rb 2 SiF 6 49 Barium peroxide, Ba0 2 18 Sodium nitrate (soda-niter), NaN03 50 Bismuth (III) iodide, Bil 3 20 Strontium peroxide, Sr0 2 52 molybdate, 21 Cadmium CdMo0 4 Thallium aluminum sulfate dodecahydrate, Calcium molybdate (powellite), CaMo0 4 22 T1A1(S0 4 ) 2 -12H 2 0 53 Calcium tungstate (scheelite), CaW0 4 23 Thallium chlorostannate, Tl2 SnCl6 54 sulfate dodecahydrate, Cesium aluminum Thallium chromium sulfate dodecahydrate, CsA1(S0 4 ) 2 -12H 2 0 25 TlCr(S0 4 ) 2 -12H 2 0 55 Cesium fluoplatinate, Cs 2 PtF6 27 Thallium fluosilicate, Tl 2 SiF6 56 iron sulfate dodecahydrate, CsFe Cesium Thallium gallium sulfate dodecahydrate, (S0 4 ) 2 -12H 2 0 28 TlGa(S0 4 ) 2 -12H 2 0 57 Chromium silicide, Cr3 Si 29 Thallium (I) nitrate, T1N0 58 Gallium antimonide, GaSb 30 3 Thallium (I) sulfate, T1 2 S0 4 59 Magnesium hydroxide (brucite), Mg(OH) 2 30 Zinc fluoride, ZnF2 60 Magnesium silicate (enstatite), MgSi0 3 32 Mercury(II) cyanide, Hg(CN) 2 35 Cumulative index to volumes 1, 2, 3, 4, 5, and 6 61 ERRATA Vol. 1. Page 24, last sentence should read, ... a body centered lattice with four atoms in the unit cell. Page 35, table 17, column 1, line 13, the hkl 620 should read 600. The following hkl’s should be deleted: 533, 622, and 444. Page 41, table 20, the Clark Pattern, Mo 0.7093 A, should read Co 1.7889 A. ” Vol. 2. Page 20, the space group under “lattice constant^ listed as D-R3c, should read Dgd R3c. Page 47, the space group under “lattice constants” should read D^-Pnma. Vol. 5. Page 11, the hkl 400 should be 440. Page 24, the data given for Copper(II) Fluoride, CuF 2 (cubic) should be deleted. Page 25, the three strongest lines tabulated for the NBS pattern should read 222, 400, and 440. Page 25, the missing hkl in the GeB table for d-value 1.5047 is 800. Page 30, the d-value 1.1448 for the NBS pattern should read 1.4448. STANDARD X-RAY DIFFRACTION POWDER PATTERNS Vol. 6—Data for 44 Inorganic Substances 1 1 Howard E. Swanson, Nancy T. Gilfrich , and Marlene I. Cook Forty-four standard X-ray diffraction powder patterns are presented. Twenty-three are to replace thirty-three patterns already represented in the ASTM card file, and twenty- one are for substances not previously represented. The ASTM card file is a compilation of diffraction patterns from all sources and is used for the identification of unknown crystalline materials by matching spacing and intensity measurements. In this Circular, comparison is made of all powder diffraction data available for each of the substances reported. The patterns were made with a Geiger counter X-ray diffractometer, using samples of high purity. The d-values were assigned Miller indices determined by comparison with calculated inter- planar spacings and from space group considerations. The densities and lattice constants were calculated, and the refractive indices were measured whenever possible. Included are X-ray data for the following fortv-four substances: NH 4 A1(S04)2T2H 2 0, (NH 4 ) PdCl Cr(S0 -12H (NH GeF -12H NPI Fe(S0 4 -12H 2 4 , NH 4 4 ) 2 2 4 NH 4 Ga(S0 4) 2 4 ) 2 2 0, 0, ) 2 6 , 2 0, (NH 4) S04 (mascagnite), (NH 4)3ZrF Sbl ASI3, Ba0 Bil 4 4 (scheelite), 2 7 , 3 , 2 3 CdMo0 CaW0 , , , CsA1(S0 4 ) -12H Cs,PtF 6 CsFe(S04) -12H,0, Cr3 Si, GaSb, Mg(OH) (brucite), MgSiOa 2 2 0, , 2 2 (enstatite), -12 HoO, Iv>SnCl -12H,0, K,PtF RbAl Hg(CN) KA1(S0 KCr(S0 ) , KC10 2 , 4 ) 2 6 , 4 2 6 4 , (S04 -12H,0, Rb SnCl ) -12H,0, PtF Rb,SiF (soda-niter), Sr0 2 RbCr(S0 4 Rb , 2 ) 2 6 2 2 , 6 NaN03 , , 6 T1A1(S0 4 2 -12H Tl SnCl TlCr(S0 -12H Tl SiF Tl'Ga(S04 -12H T1N0 T12 S04 ) 2 0, 2 6 , 4) 2 2 0, 2 6 , ) 2 2 0, 3 , , and ZnF2 . INTRODUCTION The National Bureau of Standards in its pro- for each card. The card numbers are as revised gram 2 for the revision and evaluation of publish- in the second edition. This volume of Circular ed X-ray data for the American Society for Test- 539 includes the sixth set of ASTM cards. ing Materials card file presents in this paper, the Additional published patterns. Literature refer- sixth of this series, 3 data for 44 inorganic com- ences and radiation data for patterns that had not pounds. Twenty-three of these patterns are been published as ASTM cards are listed, and the recommended to replace 33 cards now in the file. patterns are included in the tables of d-values and The patterns for 21 compounds not represented in intensities. the file have been added. These compounds are NBS sample. Many of the samples used to ammonium chloropalladite, ammonium fiuoger- make the NBS patterns are special preparations manate, ammonium gallium sulfate dodecaliy- (of exceptionally high purity) obtained or prepared drate, cadmium molybdate, calcium molybdate, only in small quantities. The purity of each cesium fluoplatinate, cesium iron sulfate dodeca- sample was determined by spectroscopic or hydrate, chromium silicide, gallium antimonide, chemical analysis. The limit of detection for the potassium chlorostannate, potassium fluoplatinate, alkali elements is 0.05 percent for the NBS rubidium chlorostannate, rubidium fluoplatinate, spectrographic analysis. Unless otherwise noted, rubidium fluosilicate, thallium aluminum sulfate the spectrographic analysis was done at the NBS. dodecahydrate, thallium chlorostannate, thallium A phase-purity check was made of the nonopaque chromium sulfate dodecahydrate, and thallium (I) materials during the refractive index determina- nitrate. tion. Another excellent check of phase-purity was The experimental procedure and general plan of provided by the indexing of the X-ray pattern. these reports have not changed from that of the Treating the sample by appropriate annealing, previous volumes of this NBS Circular. The basic recrystallizing, or heating in a hydrothermal bomb technique is included and discussed in the same improved the quality of most of the patterns. order that is followed in presenting the data for At least two intensity patterns were prepared to each compound in the body of this volume. check reproducibility of measured values. Sam- ASTM cards. Each section of this Circular ples that gave satisfactory intensity patterns contains a table listing the file card numbers, the showed a particle size average well within the ASTM index lines in order of decreasing intensity, range of 5 to 10 microns as was suggested by the radiation used, and the literature references Alexander, Ivlug, and Kummer [l]. 4 A special cell with one open end is used for making intensity 1 Fellow at the National Bureau of Standards sponsored by the Joint Com- measurements. An intensity sample was prepared mittee on Chemical Analysis by Powder Diffraction Methods. by clamping a flat piece of glass temporarily over 2 This project is sponsored by the Joint Committee on Chemical Analysis by Powder Diffraction Methods.
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