Erianti Siska Purnamasari
Department Of Chemistry, Faculty Of Mathematics And Natural Sciences, Universitas Padjadjaran, Jl. Raya Bandung-Sumedang Km 21, Jatinangor 45363, West Java, Indonesia

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Pemantapan Proses Sintesis Ligan Dibutilditiokarbamat (DBDTK) Sebagai Pengekstrak Logam Tanah Jarang Berdasarkan Desain Eksperimen Diana Hendrati; Erianti Siska Purnamasari; Syulastri Effendi; Santhy Wyantuti
ALCHEMY Jurnal Penelitian Kimia Vol 14, No 2 (2018): September
Publisher : UNIVERSITAS SEBELAS MARET (UNS)

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.20961/alchemy.14.2.15006.219-235

Abstract

Gadolinium (Gd) merupakan salah satu logam tanah jarang, dimana logam tanah jarang dapat diekstrak dari mineral salah satunya mineral monasit. Logam Gd biasanya digunakan sebagai bahan dasar contrast agent dalam dunia kesehatan. Ligan dibutilditiokarbamat mampu membentuk senyawa kompleks dengan cara mengikat logam sehingga membentuk khelat yang dapat digunakan untuk ekstraksi. Tujuan dari penelitian ini adalah memantapkan sintesis ligan dibutilditiokarbamat berdasarkan desain eksperimen dan karakterisasi kompleks antara Gd(III) dengan ligan dibutilditiokarbamat hasil sintesis. Penelitian ini diawali dengan pembuatan desain eksperimen untuk sintesis ligan dan ekstraksi Gd(III) dengan ligan, kemudian proses sintesis dan ekstraksi dilakukan sesuai dengan desain eksperimen, hasil sintesis dan ekstraksi dikarakterisasi menggunakan metode spektroskopi serta diuji kelarutannya dalam pelarut organik. Data yang diperoleh menunjukkan bahwa sintesis ligan dibutilditiokarbamat optimal pada suhu 4 °C, perbandingan dibutilamin dan karbondisulfida yaitu 1 : 3 dengan perbandingan mol ammonia terhadap dibutilamin yaitu 1 : 4, sedangkan kondisi optimal untuk ekstraksi Gd(III) dengan ligan yaitu pada pH 6, dengan perbandingan mol Gd(III) dan ligan yaitu 1 : 4 dan lama ekstraksi 60 menit. Oleh karena itu ligan dibutilditiokarbamat hasil sintesis berpotensi digunakan sebagai ekstraktan untuk ekstraksi Gd(III). Hasil prediksi ligan berdasarkan desain eksperimen yaitu sebesar 56,12% sedangkan prediksi ekstraksi Gd(III) dengan ligan hasil sintesis diperoleh sebesar 78,41%.The Consolidation of Dibutyldithiocarbamate (DBDTC) Synthesis as Gadolinium Metal Extraction Based On Experimental Design. Gadolinium (Gd) is one of the rare-earth elements, whereas rare-earth elements can be extracted from monazite. Gd is usually used as raw material for synthesizing contrast agent in medicine field. Dibuthyldithiocarbamate ligand can form a complex compound with metal. This ligand will bind a metal and then forming chelate which is used for extraction. The purpose of this research is to ensure procedure of dibuthyldithiocarbamate ligand synthesis based on the design of experiment and to study the characterization of reaction result between Gd(III) and dibuthyldithiocarbamate ligand which this ligand is synthesis result. This research begins with making design of experiment for ligand synthesis and Gd(III) extraction with ligand, then perform the process of synthesis and extraction according to the design of experiment, the result of synthesis and extraction were characterized by spectroscopy method and solubility tested in organic solvent. The data was collected indicate that the optimal condition of dibuthyldithiocarbamate ligan synthesis at 4 °C (temperature), the ratio of di-n-butylamine and carbon disulphide is 1:3 with the mole ratio of ammonia to the di-n-butylamine 1:4, while the optimal conditions for gadolinium extraction with ligand at pH 6, the mol ratio of gadolinium and ligand is 1:4 and 60 minutes extraction time. Hence, dibuthyldithiocarbamate ligand can be used as extractan for extracting Gd(III). The prediction of ligand based on the experimental design is 56.12% while the prediction of Gd(III) extraction with ligand of the synthesis result is obtained equal to 78.41%. The conclusion of this research is that the synthesis of dibuthyldithiocarbamate ligand based on the experimental design can be developed for large-scale synthesis.
Selection of the Parameters in the Synthesis of Ethylenediamine-Folate Using the Plackett Burman Design Erianti Siska Purnamasari; Linda Septiana; Ari Hardianto; Ukun Mochammad Syukur Soedjanaatmadja; Anni Anggraeni; Husein Hernadi Bahti
Indonesian Journal of Chemistry Vol 22, No 3 (2022)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.22146/ijc.68313

Abstract

This study is concerned with synthesizing ethylenediamine-folate (EDA-Folate), which will then be used as a precursor in synthesizing Gd-PEG-DOTA-Folate, a novel targeted-contrast agent for the diagnosis of cancer, employing the Magnetic Resonance Imaging method. This study aims to determine all the parameters affecting the synthesis of EDA-Folate using the Plackett Burman design. The synthesis method included activation of folic acid using dicyclohexylcarbodiimide and N-Hydroxysuccinimide to result in NHS-Folate, followed by conjugation of ethylenediamine with NHS-Folate to produce EDA-Folate. Analysis of the reaction product confirmed that the reaction product was EDA-Folate. From the resulted data, it can also be concluded that there were four significant parameters (out of the ten parameters studied) in the synthesis of EDA-Folate (with its value presented in the bracket), i.e., time inactivation of NHS-Folate (24 h), stirring rate inactivation of NHS-Folate (300 rpm), the mole of EDA (12 moles), and time of EDA-Folate (12 h). Moreover, the value or desirability of the experimental design was found to be 0.875 (which is < 1.0), meaning that the design will produce optimal conditions and thus the optimal yield of the reaction.