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Minerals 2019, 9, 766 5 of 21 carnallite and kainite. Solution R is saturated with respect to kieserite, carnallite and kainite. Solution Z is saturated with respect to kieserite, carnallite and bischofite (Figure 3). With the exception of seawater and double distilled H2O, the solutions were prepared using pure NaCl (Emsure ACS, ISO for analysis, Merck), KCl (pro analysi, Merck), MgCl2·6H2O (extra pure for table water, Merck) and MgSO4·H2O (Sigma-Aldrich). The first solution used for the experiments was double distilled H2O, representing the largest difference in concentration with an electrical conductivity of 0.055 μS/cm (sample 1). Three pure NaCl solutions were used for the experiments: • 0.42 mol NaCl/kg H2O is a typical NaCl-content of fresh seawater (sample 2); • 4.96 mol NaCl/kg H2O assigns first halite precipitation from evaporating seawater (sample 3); • 5.74 mol NaCl/kg H2O is close to the theoretical halite saturation at 6.11 mol/kg H2O (sample 4) in a pure NaCl solution. Six pure artificial KCl solutions were created: • 0.01 mol KCl/kg H2O represents the KCl content of fresh seawater (sample 5); • 0.02 mol KCl/kg H2O almost corresponds to solution Z at the point of bischofite formation at the end of seawater evaporation (sample 6); • 0.19 mol KCl/kg H2O is typical at halite formation during seawater evaporation (sample 7); • 0.37 mol KCl/kg H2O assigns KCl concentration of evaporating seawater at polyhalite saturation (sample 8); • 0.60 mol KCl/kg H2O represents almost solution Q, equilibrium with sylvite, carnallite and kainite at 25 ◦C (sample 9), and • 4.29 mol KCl/kg H2O at sylvite saturation in a pure KCl solution (sample 10). Four pure MgCl2 solutions were used: • 0.03 mol MgCl2 /kg H2 O, representative for fresh seawater (sample 11); • 3.50 mol MgCl2 /kg H2 O, as in solution Q at 25 ◦ C (sample 12); • 4.26 mol MgCl2 /kg H2 O, as in solution R at 25 ◦ C (sample 13), and • 5.51 mol MgCl2 /kg H2 O near bischofite saturation, almost representing solution Z at 25 ◦ C (sample 14). Sample 15 represents seawater from the North Sea. Additionally, three artificial solutions that correspond approximately to the solutions at the invariant points are Q (sample 16), R (sample 17) and Z (sample 18). All three solutions are comparable to the natural analogue with the exception of the trace components (Br, Rb, Li and Si). The lepidolite samples in the solutions were shaken at a temperature of 22 ◦C to 25 ◦C on a shaking table with a frequency of 150 shakes/min. During the first year, the process was interrupted only shortly after 24 to 26 days for measuring the electrical conductivity. After one year, the solutions were separated from the lepidolite by filtration with Sartorius membrane filters (pore size <0.45 μm and <0.1 μm, Sartorius AG, Göttingen, Germany), washed with double distilled H2O, cleaned with ethanol and dried at room temperature. In a second step, half of the reacted lepidolite and half of the reaction solution were merged again (in the same rock-water-mass-relation of 1(rock):12.5(solution)), and the experiments continued for two more years following the same conditions described above. The entire experiment lasted for ca. three years.PDF Image | Lithium Occurrences in Brines from Two German Salt Deposits
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