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Standard X-Ray Diffraction Powder Patterns

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Standard X-Ray Diffraction Powder Patterns NBS CIRCULAR 539 VOLUME III Standard X-ray Diffraction Powder Patterns UNITED STATES DEPARTMENT OF COMMERCE NATIONAL BUREAU OF STANDARDS Standard X-ray Diffraction Powder Patterns The two 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 I, Standard X-ray Diffraction Powder Patterns (Data for 54 inorganic substances) NBS Circular 539, Volume II, Standard X-ray Diffraction Powder Patterns (Data for 30 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, Ruth K. Fuyat, and George M. Ugrinic National Bureau of Standards Circular 539 Volume III, Issued June 10, 1954 For sale by the Superintendent of Documents, U. S. Government Printing Office, Washington 25, D. C. Price 45 cents , Contents Page Page 1. Introduction 1 2. X-ray data— Con. oxides 2. X-ray data 4 2.5. Multiple 44 Strontium titanate, SrTi0 2.1. Elements 4 3 44 Titanium, Ti 4 Barium titanate, BaTi03 45 Arsenic, As 6 2.6. Halides 47 Rhodium, Rh 9 Sodium bromide, NaBr 47 Cadmium Cd 10 Cesium bromide, CsBr 49 , Cesium dichloroiodide, CsICl 50 Indium, In 12 2 Antimony, Sb 14 2.7. Chlorates 51 Sodium chlorate, NaC10 51 16 3 Iodine, I 2 Hafnium, Hf 18 2.8. Carbonates 53 Bismuth, Bi 20 Calcium carbonate (aragonite), CaC 03 53 2.2. Selenides 23 Strontium carbonate (strontianite) SrC0 Zinc selenide, ZnSe 23 3 56 2.3. Oxides 24 2.9. Nitrates 58 Potassium nitrate (niter), KN0 58 Silicon dioxide (alpha quartz), Si02 24 3 27 2.10. Sulfates and Sulfites 60 Scandium oxide, Sc 2 03 60 Sodium sulfite, Na 2 S03 Yttrium oxide, Y2 03 28 Potassium sulfate (arcanite), K S04 62 Molybdenum trioxide (molybdite), Mo03 30 2 (senarmontite) Sb 0 31 Barium sulfate (barite), BaS04 65 Antimony trioxide , 2 3 oxide, La 0 33 Lead sulfate (anglesite), PbSC>4 67 Lanthanum 2 3 69 Mercury (II) oxide (montroydite) HgO 35 2.11. Phosphates Potassium dihydrogen phosphate, KH P0 69 2.4. Oxide hydrates 38 2 4 Aluminum oxide mono-hydrate, alpha, 2.12. Bromoosmates 71 Ammonium bromodsmate, (NH 0sBr 71 A1 "H 38 4) 2 6 (bohmite), 2 03 2 0 volumes I, II, Aluminum oxide mono-hydrate, beta, (dia- 3. Cumulative index to and III 72 spore), A1 0 *H 0 41 2 3 2 ERRATA Vol. I. Page 64, table 37, Swanson and Tatge pattern. The a value for the d spacing at 2.680 should read 4.642. Vol. II. Page 54, column 1. The a and c values for Bergen should read 4.99003 and 17.0605. II STANDARD X-RAY DIFFRACTION POWDER PATTERNS Vol. Ill — Data for 34 Inorganic Substances 1 Howard E. Swanson, Ruth K. Fuyat , and George M. Ugrinic Data for thirty-two standard X-ray diffraction powder patterns are presented in revision of the eighty-one corresponding patterns in the American Society for Testing Materials card file, a system for the identification of unknown crystalline materials based on the three strongest reflections of each structurally distinct phase. Pat- terns for two compounds not represented in the file are also included. A comparison is made between all powder data available for each of the substances reported. The patterns were made with a geiger counter X-ray spectrometer, using samples of excep- tionally high purity. The d-spacings were assigned Miller indices determined from calculated patterns of theoretical spacings and from space group considerations. The lattice constants and densities were calculated, and the refractive indices were measured whenever possible. Included in this report is X-ray data for the following thirty-four substances: Ti, As, Rh, Cd, In, Sb, I Hf, Bi, ZnSe, Si0 (a-quartz), Sc 0 Y 0 Mo0 (molyb- 2 , 2 2 3 , 2 3 , 3 dite), Sb (senarmontite) La HgO (montroydite) a-Al 'H (bohmite), 2 03 , 2 03 , , 2 0 3 20 /3-Al (diaspore), SrTi0 BaTi0 NaBr, CsBr, CsICl NaC10 CaCo (aragonite), 0 'H 0 , , 2 3 2 3 , 3 , 2 3 3 SrC0 (strontianite) KN0 (niter), Na S0 S0 (arcanite), BaS0 (barite), PbS0 , , K 3 3 2 3 2 4 4 4 (anglesite), KH P0 and (NH ) 0sBr 2 4 , 4 2 6 1. INTRODUCTION The National Bureau of Standards program 3 oxide and ammonium bromoosmate, not repre- for revision and evaluation of published sented in the file, have been added. X-ray data for the American Society for Test- Experimental procedures and the general ing Materials card file presents in this paper plan of these reports are discussed in the a third series 3 of standard powder diffrac- first three papers of this series, two by 4 tion patterns for nine elements and twenty- Swanson and Tatge [1, 2] and one by Swanson three inorganic compounds. These patterns and Fuyat [3]. The significant changes in are recommended to replace eighty- four cards procedure and certain basic data discussed now in the file. Two compounds, scandium below are arranged in the same form as the data for each compound in the body of the re- 3 Fellow at the National Bureau of Standards sponsored port . by the Joint Committee on Chemical Analysis by X-ray Dif- fraction Methods. ASTM Cards. Each section of this paper, devoted to the discussion of X-ray data for 2 This project is sponsored by the Joint Committee on Chemical Analysis by X-ray Diffraction Methods, composed of one substance, contains a table listing old members from American the Society for Testing Materials, and new file card numbers, the ASTM index the American Crystallographic Association, and the British Institute of Physics. Financial support is being given by lines, the radiation used and the literature the National Bureau of Standards and the Flight Research reference for each card. The old card num- Laboratory, Wright Air Development Center, Wright-Patterson bers of these tables to the Air Force Base. refer original 3 The first paper of this series is Standard X-ray Dif- ASTM card file (1939) and the first supple- fraction Powder Patterns, I. Data for 53 Inorganic Sub- ment (1944). The new card numbers are from stances by H. E. Swanson and E. Tatge, and the second is Standard X-ray Diffraction Powder Patterns, II. Data for 4 Figures in brackets indicate the literature refer- 30 Inorganic Compounds by H. E. Swanson and R. K. Fuyat. ences at the end of each section of this paper. 1 the second edition and include the second top. The sample holder was then turned face supplement (1950). up, and the piece of glass removed. This Additional published patterns. Litera- surface was used for exposure to the X-ray ture references and radiation data for pat- beam. For a few powder samples which did not terns that had not been published as ASTM flow readily or were prone to orient badly, cards were listed and the patterns were included 25 to 50 percent finely ground silica-gel was in the tables of d-spacings and intensities. added as a diluent. The intensity values of INBS pattern. The samples used to make each pattern were measured as peak height the NBS patterns were special preparations above background and were expressed as per- of exceptionally high purity obtained or pre- centages of the strongest line. The d-spacing pared only in small quantities. patterns were made with a sample packed into The purity of each sample was determined a shallow sample holder, using approximately by a spectrographic or chemical analysis. A 5 weight percent of tungsten as an internal phase purity check was made on the nonopaque standard, whose lattice constant at 25 °C is materials during the refractive index deter- 3.1648 A, as determined by Jette and Foote mination. Another excellent check on the [ 4 ] . All the NBS patterns were made by using phase purity was provided by the X-ray pat- copper radiation with a wavelength of 1.5405. tern itself, since it was indexed by compari- Interplanar spacings and intensity meas- son with theoretical d-values. However, some urements. Interplanar spacing data presented uncertainty was possible in the unequivocal in the tables were converted to angstrom isolation of the desired isomorphic forms units as internationally defined in 1946 [5], when their d-spacings tended to coincide. from Bragg angle data, from d-spacings in kX The majority of the samples that were in- units or supposed kX units, using the factor itially too coarse for X-ray analysis could 1.00202, or from d-spacings with specifically be reduced to the proper size and then an- stated wavelengths other than kX. In each nealed to remove the lattice distortion case the type of conversion made was indi- caused by grinding. It was found that powder cated. The wavelength values in the tables samples of soluble salts which could not be of d-spacings and intensities are given in annealed successfully or which could not be angstroms; the values listed under the first obtained free from the distortion of grind- section of the reports, ASTM cards, are the ing, could be recrystallized by using a original values taken from the literature. throat aspirator. Particles averaging 15 mi- The tables of patterns contain data from crons were obtained by using an aspirator or the original literature except in those in- a nebulizer in which a concentrated solution stances where there is no reference other of a salt was atomized to form a fine mist.
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