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Materials 2021, 14, 6843 5 of 15 12 M (37%) HCl solution (FUJIFILM Wako Pure Chemical Corporation, Osaka, Japan, Wako Grade 1 087–01071) was used to prepare 1.5 M, 3 M, and 6 M HCl solutions by diluting with ultrapure water. To each container, a HCl solution of the desired concentration (10 mL) was added. These containers were then covered and placed in a pressure-resistant stainless-steel outer cylinder, which was then placed in an oven (ADVANTEC, DRN320DD). The oven temperature was raised to 40 ◦C at a rate of 10 ◦C/min, maintained for 5 min, then further increased to 180 ◦C, and maintained at this temperature for 2 h. Subsequently, the inside of the oven was cooled to <100 ◦C under a flow of air prior to the removal of the reaction container. To suppress the reaction, the reaction container was rapidly cooled in a vat containing ice-water. The inside of the PTFE container was then washed with ultrapure water, and the solids were separated by filtering the reaction solution through a 0.2 μm PTFE membrane filter under reduced pressure. The filtrate volume was made up to 100 mL with a 2.5 % HCl solution to provide the leachate. The solid residues were then leached using aqua regia (see Section 2.3.2). 2.3.2. Aqua Regia A sample of the spent autocatalyst (1.0 g) and aqua regia (30 mL) were added to three tall beakers, and the beakers were heated on a hot plate at 150 ◦C for 1.5 h. After cooling, the solids were separated by filtering the solutions through a PTFE membrane filter (pore size = 0.2 μm) under reduced pressure. The leachate was made by diluting the filtrate volume to 100 mL using a 2.5% HCl solution. The solid residue was put into the beaker again to leach out the metals under the same leaching procedure. The leachate obtained after repeating this process five times was used for analysis. 2.4. Characterization 2.4.1. Thermogravimetric–Differential Thermal Analysis Thermogravimetric–differential thermal analysis (TG–DTA) measurements of the samples were performed using a TG/DTA6300 instrument (Hitachi High-Tech Science Corporation, Tokyo, Japan). The desired sample (10 mg) was charged to a ∅5 mm alumina cell and heated to 1000 ◦C at a rate of 10 ◦C/min under a 300 mL/min flow of air. As a reference sample, α-Al2O3 powder was used. 2.4.2. Elemental Analysis The concentrations of the metals (Pt, Rh, Pd, and Li) in the leachate were quantified using inductively coupled plasma mass spectrometry (ICP-MS, ELEMENT 2, Thermo Fisher Scientific, Waltham, MA, USA) or inductively coupled plasma atomic emission spectroscopy (ICP-AES, SPECTRO ARCOS, SPECTRO Analytical Instruments, Kleve, Germany). The amount of each leached metal was calculated using Equation (1). The quantities of the PGMs in the solid sample were calculated on the basis of the concentrations of the elements detected in the spent autocatalyst (see Table 1). Leached metal amount [%] = Quantity of metal in leachate × 100. (1) Quantity of metal in solid sample 2.4.3. XRD Analysis The crystalline phase of the sample was identified by powder X-ray diffraction (XRD) analysis (Bruker Co., Ltd., Karlsruhe, Germany, D8 ADVANCE/L, USA). Measurements were taken at a voltage of 40 kV, a current of 40 mA, and 2θ values of 10–80◦ with a step width of 0.02◦ and a counting time of 1 s/step. 3. Results and Discussion 3.1. Calcination and Influence of Li2CO3 Addition Figure 3 shows the TG–DTA curves obtained for the spent autocatalyst alone and a mixture of the spent autocatalyst and Li2CO3. In Figure 3a, which shows the resultsPDF Image | Recovery of Platinum Group Metals from Auto Catalysts
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