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Infrared Spectra of the Hydrated Borates

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Infrared Spectra of the Hydrated Borates JOURNAL OF RESEARCH of the National Bureau of Standards-A. Physics and Chemistry Vol. lOA. No.2. March- April 1966 Infrared Spectra of the Hydrated Borates C. E. Weir Institute for Materials Research, Nationa l Bureau of Standards, Washington, D.C. (November 4, ]965) Infrared absorption spectra of 42 different hydrated borates were obtained in the 2000-300 em- I range. A few spectra were obtained between 4000 a nd 2000 em- I. Most spectra are complex and cannot be interpreted sati sfactorily except in the case of the simplest anions. Many correlatIOns between spectra are possible, however, and possible anion types have been deduced. Differentiation between triangular and tetrahedral boron is possible on the basis of the spectra but IS less certain than in the case of the anhydrous borates. Key Words: Hydrated borates. infrared spect ra, absorption spectra, borates, boron coordination, borate ani ons 1. Introduction In the present study, infrared spectra were obtained [or 42 different hydrated borates. Most specimens A comprehensive survey of the infrared spectra of were natural minerals but in many instances synthetic the crystalline anhydrous inorganic borates was re­ materials were also available. Approximately 63 ported recently [1].1 The spectra were correlated different specimens were studied so that it was pos­ with known structures and predictions of unknown sible to determine the reproducibility of the spectra structures were made on the basis of the observed [or materials o[ different origin - a question of i mpor­ spectra. Two of the predicted anion structures have tance for natural minerals which may contain infrared been verified by subsequent x-ray crystallographic active impurities. studies [2, 3]. The obvious extension of the studies to include the hydrated borates is the s ubject o[ this 2. Experimental Method and Apparatus report. The hydrated borates have been subjected to a more Experimental techniques and equipment were sim­ systematic study than the anhydrous materials, largely ilar to those described previously for the anhydrous as a consequence of their mineralogical occurrence. borates [1]. A double-beam grating spectrometer Miller and Wilkins [4] reported data on eight hydrated was used to cover the range 4000-200 em- I. This borates obtained by the mull technique. Several range was covered in two steps, 4000- 400 em- I and years later, Takeuchi [5] studied the spectra of 17 2000-200 cm - I. In each case the lower frequency borates of which 12 were hydrated. Takeuchi also limit imposed by the available energy was higher than used the mull technique of sample preparation. the limits given. Most spectra were obtained only Moenke and his coworkers, in a series of papers, [6-13] in the range 2000-300 em- I because the fundamentals have presented spectra obtained on approximately of the borate anions were known to occur in this range. 17 hydrated borates using the KBr pellet technique. For these studies powdered films deposited on CsBr Akhamanova [14] has reported on seven hydrated plates from a volatile liquid were used. A few spec­ borates and Plyusnina and Kharitonov [15] have tra in the higher frequency range were obtained to studied six, with spectra in both cases being obtained locate the OR fundamental stretching modes. For using films deposited from isopropyl alcohol on alkali these studi es the spectra were obtained using a mull halide plates. The early work by Miller and Wilkins with perfluorokerosene as the suspending medium. [4] and that of Takeuchi [5] had a lower frequency In both cases a blank cell was placed in the reference limit of about 600 em- I which is too high to obtain some beam of the spectrometer. The possibility of dehy­ of the known fundamental vibrations of the borate drating the specimens precluded using dry air in the anion. All the more recent studies, however, extend instrument and considerable care was exercised in as far as e m- I. 400 the 500-300 cm-1 • region. In this range only those bands were considered to originate in the specimen which were not obtained on a comparison spectrum 1 Figures in brackets indicate the lite rat ure references at the e nd of this paper. run with no specimen in the beam. 153 TABLE 1. Description of samples studied 3. Samples The samples studied are listed in table 1. Column 1 Material Empirical formula Origin of specimen a of this table lists the mineral or chemical name, column 2, the empirical formula, and column 3, the Hambcrgile 4BeO . B,O, . H,O C 4744 Bandylilc CuO · CuCI,· B,O,,· 4H,0 103459. source of the material. Throughout this paper, sam­ Teepleite Na,O· 2NaCI . B,O,,· 4H,0 102798. Pinnoite MgO . B,O" . 3H,0 C 4488: synthetic ples will be referred to by the mineral names and syn­ Mgo . B,O, . 3H,0 (R. C. Erd). thetic samples will be designated by their composition Inyoilc 2CaO . 3B,0" . 13H,0 114260: Pacific Coast Borax open pit. 80ron, Calif. unless it is known that the synthetic and natural Mcycrhofferite 2CaO 3B,0,,· 7H,0 96072: Gower Gulch. Death Valley Nat. Monume nt. minerals are equivalent- In the latter case the mineral Colemanite 2CaO . 3B,0,,· 5H,0 %445: Pacific Coast Borax name will be used. Samples were obtained generally open pit, Boron, Calif. Inderite 2MgO . 3B,0" . 15H,0 11462: Pacific Coasl Borax from two sources, the mineralogical collection of the open pit , Boron, Calif. Smithsonian Institution and the U.S_ Geological Kurnakovite 2MgO· 3B,0,,· 15H,0 R 11023: Pacific Coast Borax open pit, Boron, Calif. Survey. In column 3, designations denoted by num­ Inderborit e MgO . CaO . 3B,0,,· II H,O Inder region, USSR. Hydroboracite MgO· CaO . 3B,0,,· 6H,0 Inder region , USSR (R. C. bers correspond to catalog numbers in the Smith­ E rd via H. B. Mason). sonian collection. Origins of specimens obtained Synthetic 2SrO . 3B,0" . SH,O Synthetic strontium cole­ manite (R. C. Erd via C. R. from the U.S_ Geological Survey are listed in column 3. Parkerson). Tunellite SrO· 3B,0" . 4H,0 Pacific Coast Borax open The total number of samples of each mineral type pit, Boron, Calif.: sy nthetic studied is indicated by the number of listings in .unelli.e (R. C. Erd). Noble it e CaO ·3B,0" 4H,0 115278: N. of DeBely mine, column 3 separated by semicolons. The order in Death Valley Nat. Monume nt: synthetic nobleite (R. C. Erd). which the samples are listed in table 1 corresponds to Gowerit e CaO . 3B,0" . SH,O 11 5277: Hard Scramble C laim. the order followed in the discussion. Death Valley Nat. Monument: synthetic gowerile (R. C. Erd). Veatchile SrO . 3B,0" . 2H,0 11 7214: synthetic veatchit e (c. R. Parkerson via R. C. Erd). Synthetic CaO· 3B,0,,· 2H,0 Syntheti c calc ium veatchite (c. R. Parkerson via R. C. Erd). Synthetic MgO . 3B,0,,· 7t H,O Synthet ic rnacallistcrite 4. Results and Discussion (R. C. Erd ). Synthetic MgO . 3B,0,,· SH,o Synthetic aksaitc (H. A. Lehmann via R. C. Erd). Synthetic SrO . 3B,0" . 4H,0' Synthet ic (c. R. Parkerson 4.1. Presentation of Data via R. C. Erd), possibly a di­ morph of tunellite but degree of hydration uncertain. Data will be presented here as in the previous Ginorite 2CaO· 7B,o,,· 8H,0 112966: synthe ti c ginorite (R. C. Erd). report [1]. Compounds are grouped according to Stronlian Ginorite 2SrO . 7B,o,,· 8H,0 Natural mineral via R. C. Erd. Syntheti c 2SrO . 78,0,,· 8H,0 Synthetic volkovite [?J the anion type expected based on the ideas presented (R. C. Erd). by Christ [16]. For each compound, observed bands Priceitc 4CaO . 5B,0" . 7H,0 Death Valley Nat. Monu­ ment O. F. McAllister via are tabulated with the type of band designated by the R. C. Erd). Pandermite 4CaO . 58,0,,· 7H,0 Panderma, Asia Minor (W. T. usual abbreviations_2 Typical spectra are shown only Schaller via R. C. Erd). for a few of the materials and only for the range 1800 Tertschite 4CaO· 5B,0,,· 20 H,0['J Kurtpinari mine, Bigadic district, Turkey (H. Meixner via cm-1 to approximately 300 cm-1_ R. C. Erd). Preobrazhenskite 3MgO . 5B,Q, . 4t H,O['J Inder region, USSR (M. E. Mrose via R. C. Erd). Ulexile Na,O . 2CaO . SB,O,,· 16H,0 96994: Pacific Coast Borax open pit , Boron, Calif.; Mudd­ 4.2. Borates With Simple Anions mine, Boron, Calif. Probt!TtiLe Na,O . 2CaO . 5B,.o" . IOH ,O 96077: Mudd mine, Boron, Calif.: Harmony Borax Works. In order to assess the extent to which analyses of Death Valley Nat. Monume nt. Kaliborite K,O . 4MgO . II B,O" . 9H,0 R 5844. the spectra of the hydrated borates can be pursued, Parahilgardite 6CaO . 2CaCI, . 9B,0" . 4H,0 105822. Kernite N a,O . 2B,0" . 4H,0 95737: Mudd mine, Boron, Cal. it is instructive to consider first the spectra of ham­ Tincalconite Na,O . 2B,0,,· SH,O 107397. bergite, bandylite, teepleite, and pinnoite. These Synthetic Na,O . 28,0,,· 10H,0 Synthetic borax, reagent grade. materials have known structures with relatively simple Synthetic K,O . 28,0" . 4H,0 Reagent grade. anions. Hambergite contains unhydrated planar BO:;-3 Synthetic Na,O ·58,0,,· IOH,O Synthetic (V. Morgan via R. C. Erd). groups [17 , 18] and the formula Be2(OH)BO:; repre­ Larderellile NH,· 5B,0,,· 4H ,0 C 4481. Ammonioborite NH,· 5B,0" ·S'/3ii,O R 6167. sents the structure. Both bandylite and teepleite Ezcurrite 2Na,.o ·58,0,,· 7H,0 Tinealayu. Argentina.
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