Standard X-ray diffraction powder patterns, HE Swanson, E Tatge, RK Fuyat

Tags: lithiophosphate, Powder Patterns, A. Structural, Bondareva, Mighell, H. Swanson, lithium sulfate, monohydrate, Chemical analysis, Z. Krist, R. Bechmann, L. K. Frevel, J. D. Hanawalt, F. Mauer, Powder data, UNITED STATES DEPARTMENT OF COMMERCE, Lithium Phosphate, Eloise H. Evans National Bureau of Standards, Marlene C. Morris, Howard E. Swanson, A. V. Astin, Secretary NATIONAL BUREAU OF STANDARDS, National Bureau of Standards, E. Swanson, A. Mighell, John T. Connor, C. Keffer
Content: United States Department of Commerce. John T. Connor, Secretary NATIONAL BUREAU OF STANDARDS. A. V. Astin, Director Standard X-ray Diffraction Powder Patterns Howard E. Swanson, Marlene C. Morris, and Eloise H. Evans National Bureau of Standards Monograph 25 - Section 4 Issued June 28, 1966 For sale by the Superintendent of Documents, U.S. Government Printing Office Washington, D.C., 20402 - Price 55 cents
Lithium Phosphate, low form (lithiophosphate), LiaP04 (orthorhombic) revised
This compound was described in earlier work [1] from this laboratory. Recently the structure of the low form was determined by Keffer, Mighell, Mauer, Swanson, and Block [2]. The following pattern is intended to replace the earlier one in Monograph 25, Section 3. Powder data card. No. 12-230, Fisher [3] 1958. Additional published patterns. Matias and Bondareva [4] 1957 and National Bureau of Standards [1] 1964. NBS sample. The samJ?le of lithium phosphate was obtained from the CIty Chemical Co., New York, N.Y. Spectrographic anal)Jis showed the following major impurities: 0.1 to 1.0 percent calcium; 0.01 to 0.1 percent each of aluminum, sodium, and strontium; and 0.001 to 0.01 percent each of barium, iron, magnesium, and silicon. The sample was colorless. Two indices of refraction are Na=1.550 and N'Y=1.538. It is optically negative with a large 2V. N~ could not be determined because of the crystal shape. The d-values of the three strongest lines are 3.973, 3.797, and 2.640 A. Structural data. Keffer, Swanson, Mighell, Mauer, and Block [2] in 1964 determined that low form lithium phosphate has the space group Civ-Pmn2] (No. 31) and 2(Li3P04) per Unit Cell. References [I] H. E. Swanson, M. C. Morris, E. H. Evans, and L. Ulmer, Standard X-ray Diffraction Powder Patterns, NBS Mono. 25, Sec. 3, 38 (1964). [2] C. Keffer, A. Mighell, F. Mauer, H. Swanson, and S. Block, The crystal structure of low temperature lithium phosphate (to be published in Inorg. Chern.). t3] D. J. Fisher, Note on lithiophosphate, Am. Mineralogist 43, 761-2 (1958). [4] V. V. Matias and A. M. Bondareva, Lithiophosphate, a new mineral, Dokl. Akad. Nauk SSSR 112, 124-6 (1957); an English abstract exists in Am. Mineralogist 42, 585 (1957). [5] F. Zambonini and F. Laves, tJber die Kristallstruktur des LigPO. und seine Beziehung Zum Strukturtyp des Olivin, Z. Krist. 83, 26-28 (1932).
hkl 010 110 101 011 111 200 210 020 002 211 021 012 121 112 310,202 301 221 212 311 122 130 031 320 131 103 013 400 230 113 410 411 213 123 420 040 402 232 331 303 412 223 240 510 501 241 422 430 323 340
Internal Standard Ag, a=4.0861 1; temp. 25°C Cu A 1.54051
d
I
.1 5. 232 3. 973 3. 797 3. 554 3. (}71 3. 059 2. 640 2. 616 2. 423 2.318 2. 303 2. 199 2.155 2. 070 1. 899 1. 879 1. 839 1. 785 1. 769 1. 7074 1. 6777 1. 6415 1. 6083 1.5855 1. 5616 1. 5431 1.5287 1. 5152 1. 4959 1. 4675 1. 4043 1. 3776 1. 3409 1. 3203 1.3078 1. 2931 1.2848 1. 2788 1. 2656 1. 2550 1. 2533 1. 2027 1. 1909 1.1860 1. 1676 1. 1591 1. 1498 1. 1394 1. 1014
34 100 98 56 } 26 64 36 47 } 31 <1 4 3 1 2 4 14 9 1 2 1 3 2 4 3 11 16 1 1 2 14 2 2 <1 4 8 4 2 1 1 <1 2 2 3 2 <1 <1 2
21 794-239 0 - 66 - 4
Lattice COWJtant8
1932 1965
a ----- A Zambonini and Laves [5]- ________ 6.08 National Bureau of Standards, sample at 25 °C. ______________ 6.1155 ±0.0004
b A 10.28 5.2340 ±0.0005
c A 4.87 4. 8452 ±0.0005
The density of lithium phosphate, low form, calculated from the NBS lattice constants is 2.479 g/cm3 at 25 °0.
Lithium Sulfate Monohydrate, Li2S04 · H 20 (monoclinic)
Powder data card. No. 1-0425, Hanawalt, Rinn, and Frevel [1]1938. Additional published patterns. None. NBS sample. The sample of lithium sulfate monohydrate was prepared at NBS from lithium metal and sulfuric acid, using enough heat to fume off the excess acid. Spectrographic analysis showed the following major impurities: 0.01 to 0.1 percent each of silver, calcium, sodium, and tungsten; and 0.001 to 0.01 percent each of aluminum, barium, iron, potassium, magnesium, silicon, and strontium.
The sample was colorless and optically negative. The indices of refraction are Na =1.460, N,,= 1.477, and N y =1.487; 2V is large. The d-values of the three strongest lines are 5.084, 4.133, and 3.559 1. Structural data. Ziegler [2] in 1934 determined that lithium sulfate monohydrate has the space group 0~-P21 (No.4) with 2(Li2S04 ·H20) per unit cell.
Lattice Constants
a
1934 1952 1954 1965
Ziegler [2] _________________________________ Bechmann [3]- _____________________________ Larson and Helmholz [4]-------------------National Bureau of Standards, sample at 25 °e_
A 5. 44 5. 45 5.430 5. 4518 ±0.0005
b A 4.84 4.87 4. 836 4. 8707 ±0.0004
c A 8. 16 8. 18 8. 140 8. 175 ±0.001
{3 107°35' 107°18' 107°14' 107°19. 8' ±0.4'
The density of lithium sulfate monohydrate calculated from the NBS lattice constants is 1.939 g/cm3 at 25° O.
References [1] J. D. Hanawalt, H. W. Rinn, and L. K. Frevel, Chemical analysis by x-ray diffraction, Anal. Chem. 10, 457-512 (1938). [2] G. E. Ziegler, The crystal structure of lithium sulphate monohydrate, Li2S04·H20, Z. Krist. 89, 456-459 (1934) . [3] R. Bechmann, Elastic and piezoelectric coefficients of lithium sulphate monohydrate, Proc. Phys. Soc. GliB, 375-77 (1952). [4] A. C. Larson and L. Helmholz, Redetermination of the crystal structure of lithium sulfate monohydrate, Li2S04·H20, J. Chem. Phys. 22, 2049-2050 (1954).
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HE Swanson, E Tatge, RK Fuyat

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