Pengaruh Tri-n-Oktil Posfin Oksida dan Tingkat Ekstraksi pada Pemurnian Konsentrat Thorium

Telah dilakukan ekstraksi konsentrat thorium oksalat hasil olah monasit memakai ekstraktan Tri – n - Oktil Posfin Oksida (TOPO). Pengotor yang paling banyak terkandung dalam konsentrat thorium oksalat adalah cerium (Ce) dan lantanum (La). Tujuan penelitian ini adalah untuk memurnikan thorium (Th) dengan memisahkan Ce dan La dengan cara ekstraksi. Ekstraksi dilakukan secara batch dan bertingkat. Larutan umpan atau fase air adalah 10 gram konsentrat Th oksalat yang dilarutkan dalam 10,08 M HNO3 sehingga volume menjadi 100 mL dan fase organik adalah TOPO dalam kerosen. Stripping setiap tingkat ekstraksi dilakukan tiga kali, yaitu stripping pertama memakai air, stripping kedua memakai asam oksalat 5%, dan stripping ketiga memakai air. Waktu ekstraksi setiap tingkat 15 menit dan waktu stripping setiap tingkat 5 menit dengan perbandingan fase air dengan fase organik adalah 1 berbanding 1. Parameter yang diteliti adalah persentase TOPO dalam kerosen dan jumlah tingkat ekstraksi. Pemakaian TOPO dalam kerosen yang optimum 5% dan jumah tingkat ekstraksi 3. Pada ekstraksi I diperoleh konsentrat Ce dan pada tingkat ekstraksi II dan III diperoleh Th. Efisiensi ekstraksi Th tingkat II sebesar 39,76% dan efisiensi ekstraksi Th tingkat III 26,33%. Koefisien distribusi (Kd) Th tingkat ekstraksi II adalah 0,7587 dan Kd Th tingkat ekstraksi III 1,0096. Efisiensi ekstraksi Th total adalah 80,08 %, efisiensi ekstraksi Ce total 56,12%, efisiensi ekstraksi La total 1,54. Faktor pisah (FP) Th – Ce pada ekstraksi I adalah 1,00, FP Th – La pada ekstraksi I 92,07, FP Th – Ce pada ekstraksi II adalah 250,24 dan FP Th – La pada ekstraksi II adalah ∞, FP Th – Ce pada ekstraksi III 124,22 dan FP Th – La pada ekstraksi III adalah ∞. Faktor pisah total Th – Ce sebesar 1,4270 dan Faktor pisah total Th – La 47,0459. Kadar Th oksalat pada ekstraksi II sebesar 97,06%, kadar Th oksalat pada ekstraksi III 98,00 %. The extraction of thorium oxalate concentrate as processing product of monazite using Tri Octyl Posfine Oxide (TOPO) has been done. The most impurities contained in thorium oxalate concentrate are Ce (cerium) and La (lanthanum). The purpose of this study is to purify Th by separating Ce and La using extraction process. The extraction is done by bacth and multistage. The solution of feed or water phase is 10 grams of Th oxalate concentrate dissolved in 10.08 M HNO3 so that the volume becomes 100 mL and the organic phase is TOPO in kerosene. Stripping in each stage conducted three times, first stripping use water, second stripping use 5 % oxalic acid and the third stripping use water. Extraction time at every stage is 15 minutes and stripping time at every stage is 5 minutes with ratio of aqueous phase to organic phase = 1 : 1 . The parameters were studied % TOPO - kerosene and number of extraction stage. The optimum usage of TOPO in kerosene is 5 %. On extraction I obtained Ce concentrate and on extraction II and III obtained Th concentrates. The extraction II efficiency of Th is 39.76 % and extraction III efficiency of Th is 26.33 % . Coefficient of distribution (Kd) of Th in stage II is 0.7587 and Kd of Th in stage III is 1.0096. Total extraction efficiency of Th is 80.08 %, total extraction efficiency of Ce is 56.12 %, and total extraction efficiency of La is 1.54 %. The separation factor of Th – Ce in extraction I is 1.00 and separation factor of Th – La in extraction I is 92.0, separation factor of Th – Ce in extraction II is 250.24, and separation factor of Th – La in extraction II is ∞. Separation factor of Th – Ce in extraction III is 124.22 and separation factor of Th – La in extraction III is ∞. Total separation factor of Th – Ce is 1.4270 and total separation factor of Th – La is 4.0459. The content of Th oxalate in stripping product from the extraction II is 97.06 % and in stripping product from the extraction III is 98.00%.

Novel synthesis and characterization of nanocrystalline thoria from oxalate precursor via reverse micellar route

Nanoparticles of thorium oxalate were synthesized by the reaction of thorium nitrate and ammonium oxalate by the microemulsion method. The Th02 nanoparticles were obtained by heating thorium oxalate nanoparticles at 500 °C in air. The oxalate and oxide nanoparticles of thorium were characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), thermogravimetric analysis (TGA) and selected area electron diffraction (SAED). X-ray diffraction studies showed the mono-phasic nature of the powder thoria. The particle size was obtained from X-ray line broadening (~l0 nm) and transmission electron microscopy (~l0 nm). Dynamic light scattering (DLS) was used to calculate the average grain size of the particles. SAED confirmed the nanocrystalline nature of thoria particles. High resolution transmission electron microscopy (HRTEM) was also carried out to understand the morphology of the system. The monodisperse nanoparticles of thoria are promising for future reactor technologies.