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Download PDF (402K) Geochemical Journal, Vol. 41, pp. 149 to 163, 2007 Boron isotope fractionation accompanying formation of potassium, sodium and lithium borates from boron-bearing solutions MAMORU YAMAHIRA, YOSHIKAZU KIKAWADA* and TAKAO OI Department of Chemistry, Sophia University, 7-1 Kioi-cho, Chiyoda-ku, Tokyo 102-8854, Japan (Received March 18, 2006; Accepted June 22, 2006) A series of experiments was conducted in which boron minerals were precipitated by water evaporation from solutions containing boron and potassium, sodium or lithium at 25°C, and boron isotope fractionation accompanying such mineral precipitation was investigated. In the boron-potassium ion system, K2[B4O5(OH)4]·2H2O, santite (K[B5O6(OH)4]·2H2O), KBO2·1.33H2O, KBO2·1.25H2O and sassolite (B(OH)3) were found deposited as boron minerals. Borax (Na2[B4O5(OH)4·8H2O) was found deposited in the boron-sodium ion system, and Li2B2O4·16H2O, Li2B4O7·5H2O, Li2B10O16·10H2O, LiB2O3(OH)·H2O and sassolite in the boron-lithium ion system. The boron isotopic analysis was con- 11 10 ducted for santite, K2[B4O5(OH)4]·2H2O, borax and Li2B2O4·16H2O. The separation factor, S, defined as the B/ B isotopic ratio of the precipitate divided by that of the solution, ranged from 0.991 to 1.012. Computer simulations for modeling boron mineral formations, in which polyborates were decomposed into three coor- dinated BO3 unit and four coordinated BO4 unit for the purpose of calculation of their boron isotopic reduced partition function ratios, were attempted to estimate the equilibrium constant, KB, of the boron isotope exchange between the boric – acid molecule (B(OH)3) and the monoborate anion (B(OH)4 ). As a result, the KB value of 1.015 to 1.029 was obtained. The simulations indicated that the KB value might be dependent on the kind of boron minerals, which qualitatively agreed with molecular orbital calculations independently carried out. Keywords: boron isotopes, boron minerals, boron isotope fractionation, separation factor, reduced partition function ratio INTRODUCTION et al., 1993; Palmer et al., 1998; Honisch et al., 2004; Pagani et al., 2005). The usefulness of the method, how- Boron has two stable isotopes, 10B and 11B, and their ever, is still in dispute. To use the boron isotopic ratio as relative abundances are approximately 20 and 80%, re- a geochemical tracer, the knowledge on the accurate equi- spectively. The variation in the boron isotopic composi- librium constants of boron isotope exchange reactions tion of natural samples is large. As summarized by Palmer between two boron species in equilibrium is essential. and Swihart (1996), it is about 100‰ (permil) in the δ Boron atom is always bonded to oxygen atoms, in the expression defined as, trigonal form or in the tetrahedral form, except for some rare cases. The most important boron isotope exchange δ11 11 10 11 10 × B = {( B/ B)sample/( B/ B)standard – 1} 1000, (1) reaction is that between the boric acid molecule (B(OH)3) – 11 10 11 10 and the monoborate anion (B(OH)4 ): where ( B/ B)sample denotes the B-to- B boron iso- topic ratio of the sample and (11B/10B) that of a standard 10B(OH) + 11B(OH) – = 11B(OH) + 10B(OH) –. (2) standard. The standard used in most studies is NBS SRM 3 4 3 4 951 boric acid (Cantanzaro et al., 1970). The equilibrium constant (K ) of Reaction (2) is larger Due mainly to this large variation, boron isotopic com- B than unity, which means the heavier isotope is preferen- position has been applied to many areas of earth sciences tially fractionated into the trigonal boric acid and the and has provided valuable findings on fundamental proc- lighter one into the borate anion. The theoretical value esses in natural circumstances. One of the recent and im- based on the molecular vibrational analysis was first ob- portant applications is to estimate the ancient ocean pH tained to be 1.0194 at 25°C (Kakihana and Kotaka, 1977), using the boron isotopic composition of natural carbon- but there are experiments and observations that require ates (for instance, Hemming and Hanson, 1992; Spivack larger KB values (Vengosh et al., 1991; Palmer et al., 1987; Nomura et al., 1990). Other theoretical methods includ- ing those based on molecular orbital calculations (Oi, *Corresponding author (e-mail: [email protected]) 2000a; Zeebe, 2005) also suggest KB should be larger than Copyright © 2007 by The Geochemical Society of Japan. 1.0194 (Kakihana and Kotaka, 1977). 149 An application of the boron isotopic composition is The 95% confidence limit is typically about ±0.2%. Each to the elucidation of the origin and alteration of borate sample was measured at least twice and the arithmetic deposits (Peng and Palmer, 1995; Swihart et al., 1996). mean was taken as the isotopic ratio of the sample. To quantitatively discuss such problems, the knowledge on the exact degrees of boron isotope fractionations ac- RESULTS companying boron mineral formation from boron- bearing solutions is certainly required. To the best our Table 1 summarizes the initial solution conditions and knowledge, our previous paper (Oi et al., 1991) is only the final results of the solution and the solid phases, ex- one that reported laboratory experiments in which boron cept for the isotopic data. Many runs are omitted from minerals were precipitated from boric acid solutions and the table in which solution became mucilaginous without boron isotope fractionation upon precipitation was mea- producing precipitate by water evaporation, only a very sured. Unfortunately, the counterion was limited to the small volume of solution remained with a very large sodium ion. Precipitation experiments were then extended amount of precipitate, or while separating the precipitate to include the potassium and lithium ions. In this paper, from solution by filtration, new precipitate formed, and we report the results of boron isotope fractionations ac- so forth. In most cases, the solution and the solid (pre- companying boron mineral formations from aqueous so- cipitate) phases were separated by filtration as soon as lutions of boric acid containing potassium, sodium or we noticed the formation of precipitates. It was often very lithium ion as the counterion. difficult to determine accurately the ratio of the amount of boron precipitated to that in the initial solution. EXPERIMENTAL Precipitates obtained An aqueous solution, in which boron concentration Potassium borate system The boron concentration, pH was about 0.3 M (1 M = 1 mol/dm3) to 1.0 M and that of and the mole ratio of potassium to boron of initial solu- the cation (K+, Na+ or Li+ ion) was about 0.2 M to 3.2 M, tion ranged from 0.61 to 1.0 M, 0.36 to 14.3 and 0.41 to was first prepared by dissolving boric acid and metal hy- 2.30, respectively. The time elapsed between the start of droxide or metal chloride into distilled water. The pH was the run and the start of separation of the solid and solu- adjusted with 5.0 M sodium hydroxide solution or conc. tion phases (deposition time) was from 4 hours to 34 days. hydrochloric acid. This pH adjusted solution was used as It must have depended on many factors such as the chemi- the stock solution of the initial solution of each run. A cal composition of the initial solution and the evapora- beaker containing 200 cm3 of this initial solution was tion speed of water. The major boron minerals identified placed in a water bath, the temperature of which was con- by XRD analysis were sassolite (B(OH)3; JCPDS No. 30- ± ° trolled at 25.0 0.2 C. (In some cases, the volumes of 0199), santite (K[B5O6(OH)4]·2H2O; JCPDS No. 25- 3 the initial solutions other than 200 cm were adopted.) 0624) and K2[B4O5(OH)4]·2H2O (JCPDS No. 29-0987; No stirring of the solution or shaking the beaker was no mineral name given; designated hereafter as K2B4O7). practiced while the beaker was kept placed in the water KBO2·1.333H2O (JCPDS No. 18-1039) and bath. No artificial manipulation such as adding a seed KBO2·1.25H2O (JCPDS No. 19-0980) were also identi- crystal to the solution was attempted to promote the pre- fied as minor boron minerals. Minerals without boron cipitation, either. A precipitate was formed from the so- component identified included KCl and K2CO3. Exam- lution by concentration of the solution due to water evapo- ples of XRD patterns of K2B4O7 and santite obtained ration. Upon precipitation, the solid and the solution are shown in Figs. 1(a) and (b), respectively. They are phases were separated by sucking filtration. The solution compared with the ones in the JCPDS files. Figure 2 shows phase was analyzed for its pH and concentrations of bo- the solution conditions (the mole ratio of potassium to ron and the cation. The precipitate was air-dried and the boron and pH of the final solution) under which minerals mineral phase was identified by X-ray powder diffrac- are supposed to have been formed. As is seen, the pH tion (XRD) analysis with a Rigaku RINT 2100V/P X-ray value of solution seems the most influential to determine spectrometer. The amount of boron in the precipitate was which mineral is formed, and the kind of mineral formed determined by measuring the boron content of the solu- is almost independent of the K/B mole ratio. Admittedly tion that was prepared by dissolving an aliquot of the pre- roughly, sassolite is deposited in the low pH region. Be- cipitate into a certain volume of distilled water. tween pH about 4.5 and about 9, the main borate depos- The boron isotopic ratios of solutions and minerals ited is santite.
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