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Making Solid Solutions with Alkali Halides (And Breaking Them)

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Making Solid Solutions with Alkali Halides (And Breaking Them) MAKING SOLID SOLUTIONS WITH ALKALI HALIDES (AND BREAKING THEM) INTRODUCTION When two cations have the same charge and a similar radius, a mineral that contains one of the cations may contain the other as well, thus forming a solid solution. Common examples include Mg+2 and Fe+2 as in olivine, Na+1 and K+1 as in alkali feldspar, Al+3 and Fe+3 as in garnet. Some solid solutions are complete, so minerals may occur with the similar cations present in any proportion (e.g. olivine). In other cases, the solid solution is limited (e.g. alkali feldspar) so that some intermediate compositions cannot be formed, at least at low temperatures. Solid solutions are important because the physical properties and behavior of a mineral depend on its chemical composition. In this exercise, the class will grow a variety of crystals of the same mineral, but with different chemical compositions. These crystals will be made from mixtures of halite (NaCl) and sylvite (KCl). Because K+1 is significantly larger than Na+1, the unit cell is larger in sylvite than in halite. Intermediate compositions have intermediate unit cell sizes. Thus, a measurement of the lattice spacing of the crystalline products of your experiments can be used to determine their chemical composition. The principle goal of these experiments is to demonstrate that solid solutions do occur and that their physical properties vary with their chemical composition. An additional is to see the process of exsolution as a function of temperature. SAMPLE PREPARATION • The class should work together in small groups to prepare a series of ten-gram mixtures of NaCl and KCl in simple molar proportions, say 10, 30, 50, 70, and 90 mole percent KCl. Ten grams is much more sample than you will need, but the reagents are inexpensive and weighing larger quantities will improve the accuracy of the resulting mixes (Why?). Because the gram formula weights of these compounds differ (NaCl = 58.4428 g/mole, KCl = 74.555 g/mole), some calculation is required to determine the appropriate mass proportions. Both NaCl and KCl are hygroscopic, so for the most accurate results you should use dry reagents that have been heated above 100°C and cooled shortly before weighing. • Be sure to record your calculations and reagent weights in your lab notebook. • Mix the measured NaCl and KCl thoroughly by grinding with a mortar and pestle. PART I. MAKING SOLID SOLUTIONS BY HEATING • Use the hydraulic press to create a pellet from a modest amount (1-2 grams) of your mixture. • Place your pellet in an inexpensive porcelain crucible with a shiny glazed finish. • Heat your pellet at 600°C for at least 30 minutes. • Collect a powder x-ray pattern for your pellet (25°-35° 2 theta). Do not grind the sample! Be sure to use the sample height alignment before collecting data. • Heat your pellet at 400°C for at least 30 minutes. • Collect a powder x-ray pattern for your sample (25°-35° 2 theta). Do not grind the sample! Be sure to use the sample height alignment before collecting data. 1 DATA ANALYSIS • Measure or look up the position of the (200) peak on diffraction patterns for pure halite and pure sylvite. • Draw a graph with d-values on the y-axis and molar composition (from NaCl to KCl) on the x- axis. • Plot d(200) for halite and sylvite on this graph. Connect the d(200) values for pure halite and pure sylvite with a straight line. • Plot d(200) for each sample at the appropriate composition on this graph. • Interpret your results. 2 05-0628 Quality: Quality Data Na Cl Sodium Chloride Halite, Syn Rad:CuKa1 Lambda:1.5405 Filter:Beta filter used d sp: Cutoff: Int: I/Icor:4.4 Ref:Swanson, Fuyat., 2 41, (1953) Sys:Cubic S.G.:Fm 3 m a:5.6402 b: c: α: β : γ: Z:4 mp Ref2 Dx:2.164 Dm:2.163 SS/FOM: F17=92.7(0.0108,17) Volume[CD]:179.43 εα: ηωβ :1.542 εγ: Sign : 2V: Ref3 Color:Colorless An ACS reagent grade sample recrystallized twice from hydrochloric acid. X-ray pattern at 26 C. Merck Index, 8th Ed., p. 956. 804$DE 17 reflections in pattern. 2 θ Int. h k l 2 θ Int. h k l 2 θ Int. h k l 2 θ Int. h k l 27.3345 13 1 1 1 101.1897 2 4 4 0 31.6920 100 2 0 0 107.8049 1 5 3 1 45.4489 55 2 2 0 110.0417 3 6 0 0 53.8521 2 3 1 1 119.4997 4 6 2 0 56.4774 15 2 2 2 127.1639 1 5 3 3 66.2269 6 4 0 0 129.8877 3 6 2 2 73.0639 1 3 3 1 142.2317 2 4 4 4 75.3019 11 4 2 0 83.9702 7 4 2 2 90.4063 1 5 1 1 41-1476 Quality: Quality Data K Cl Potassium Chloride Sy lv it e, Sy n Rad:CuKa1 Lambda:1.54056 Filter:Monochromator crystal used d sp:Diffractometer Cutoff: Int:Diffractometer I/Icor: Ref:Welton, J., McCarthy, G., North Dakota StateUniversity, Fargo, North Dakota, USA.Copper, M., Rouse, K.Winchell, A., Win Sys:Cubic S.G.:Fm 3 m a:6.2917±0.0003 b: c: α: β : γ: Z:4 mp Ref2 Dx:1.988 Dm:1.988 SS/FOM: F15=87.7(0.0086,20) Volume[CD]:249.06 εα: ηωβ :1.4904 εγ: Sign : 2V: Ref3 Color:White Sample from Mallinckrodt. Lot analysis showed sample as 99.9+% pure. Sample recrystallized from 50/50 ethanol water solvent system and heated at 600 C for 72 hours. 790 C Merck Index, 8th Ed., p. 853. To replace 4-587, and validated by calculated patterns 26-920 and 26-921. 15 reflections in pattern. 2 θ Int. h k l 2 θ Int. h k l 2 θ Int. h k l 2 θ Int. h k l 24.4819 1 1 1 1 101.4846 2 6 2 0 28.3453 100 2 0 0 108.6041 1 6 2 2 40.5075 37 2 2 0 116.0401 1 4 4 4 47.9088 1 3 1 1 123.9746 1 6 4 0 50.1689 10 2 2 2 132.7331 1 6 4 2 58.6403 5 4 0 0 66.3810 9 4 2 0 73.7332 5 4 2 2 87.6783 1 4 4 0 94.5554 2 6 0 0.
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