PEMBUATAN DAN SERTIFIKASI CRM-INHOUSE ZIRKONIL KLORIDA HASIL PROSES MINERAL ZIRKON

PEMBUATAN DAN SERTIFIKASI CRM-INHOUSE ZIRKONIL KLORIDA HASIL PROSES MINERAL ZIRKON. Telah dilakukan pembuatan dan sertifikasi bahan acuan bersertifikat (CRM) zirkonil klorida hasil proses mineral zirkon Kalimantan. Mineral zirkon diproses dalam Feeder dengan kecepatan 17 kg/jam, maka diperoleh konsentrat zirkon. Konsentrat zirkon dicampur dengan NaOH, NaF, Na2CO3 dan H2O. Campuran dilebur dalam Furnace pada suhu 750 oC selama 2 jam. Leburan dilindi menggunakan aquadest. Hasil pelindian dilakukan pengenapan selama 24 jam . Padatan dipisahkan dari filtratnya dan kemudian dikeringkan dalam oven pada suhu 105 o C selama 3 jam dan diperoleh natrium zirkonat. Natrium zirkonat dilakukan pelindian dengan HCl, diperoleh larutan zirkonil klorida, dan kemudian diuapkan, sehingga diperoleh larutan zirkonil klorida pekat. Larutan ini dilakukan kristalisasi maka diperoleh kristal zirkonil klorida. Kristal zirkonil klorida dicuci dengan etanol sehingga diperoleh kristal zirkonil klorida berwarna putih. Kristal ini dikeringkan dalam oven pada suhu 90oC, digerus dengan stainless steel, diayak lolos 100 mesh, dihomogenkan dengan homogenizer dan dilakukan uji homogenasi dan stabilisasi dengan metode statistik. Kristal zirkonil klorida distandardisasi dengan menggunakan standar ZrOCl2 8 H2O buatan E.Merck, meliputi uji senyawa kimia dengan Spektrometri XRD, uji komposisi, kadar air Kristal dan uji berat jenis. Berdasarkan evaluasi data uji homogenasi dan stabilisasi, kandidat CRM Zirkonil klorida sudah homogen, stabil dan memenuhi syarat sebagai CRM. Dibandingkan dengan standar zirkonil klorida, ZrOCl2 8 H2O, CRM kristal zirkonil klorida mempunyai komposisi kimia (96,263 %), kadar air kristal (98,625 %) dan berat jenis (97,190 %) mirip sama. Sertifikat parameter uji dalam CRM zirkonil klorida dari 7 laboratorium terakreditasi dengan metode statistik diperoleh konsentrasi Zr : (27,357 ± 0,007) %, Hf : (0,625 ± 0,0006 %, Ti : (0,005 ± 0,00006) %, Si : (0,071 ± 0,0009) %, Cl : (22,442 ± 0,186) %, Mg : (0,097 ± 0,0156) %, Na : (0,072 ± 0,0002) %, Mo : (0,012 ± 0,0001) %, dan H2O : (44,716 ± 0,199 ) %.

Kata Kunci : Sertifikasi, CRM-Inhouse, zirkonil klorida, mineral zirkon.

THE PREPARATION AND CERTIFICATION OF ZIRCONYL CHLORIDE CRM-INHOUSE FROM PROCESS RESULT OF ZIRCON MINERAL. The preparation and certification of the zirconyl chloride certified reference material (CRM) has been carried out from the row material of the zircon mineral. The zircon mineral was processing in the Feeder with the velocity of 17 kg/hour and producted the zircon concentrate. The zircon concentrate was mixed with NaOH, NaF, Na2CO3 and H2O. The mixture was melted in the Furnace at 750 oC for 2 hours. The results of molten was pressed with aquadest and then was precipated for 24 hours. The solid was separated from the filtrate, and then it was dried in the Oven at 105 oC for 3 hours, those result was called sodium zirconate. Sodium zirconate was leaching with HCl, it was found the zirconyl chloride solution and then was evaporated it was found the zirconyl chloride concentrated solution. This solution was crystallized, then obtained the zirconyl chloride crystal. It was washed with ethanol, so retrieved the crystal white zirconyl chloride. The crystal white zirconyl chloride was dried in the Oven at 90 oC, it was crushed with stainless steel pounder and sieved to 200 mesh of the particle size. The crystal white zirconyl chloride was stirred up to homogenous in the Homogenizer. Next was treated the homogenezation and the stabilitation testing with statistically method. Zirkonyl chloride crystals was standardized by using standard ZrOCl2 8 H2O made in E. Merck. were include the chemical compounds test with XRD Spectrometry, the composition the content of crystals and the specific grasvuty.. From the evaluation of the homogenezation and stabilitation testing, the crystal zirconyl chloride was homogen, stable and it was fulfil to physically behavior as CRM. Compared with the standard zirkonyl chloride, ZrOCl2 8 H2O, the XRD spectra and chemical composition (96,263%), the content of crystals (98,625%) .and specific gravity ( 97,190 %) of the zirkonyl chloride crystal were neraly same respectively. Certificate of the parameters testing results in the CRM the zirconyl chloride crystal from 7 acredited Laboratories with statistically method were resulted 10 parameters are the concentration of Zr : (27,357 ± 0,007) %, Hf : (0,625 ± 0,0006 %, Ti : (0,005 ± 0,00006) %, Si : (0,071 ± 0,0009) %, Cl : (22,442 ± 0,186) %, Mg : (0,097 ± 0,0156) %, Na : (0,072 ± 0,0002) %, Mo : (0,012 ± 0,0001) %, and H2O : (44,716 ± 0,199 ) %

Keywords : Certification,CRM-Inhouse zirconyl chloride, zircon mineral