scholarly journals Optimization of Large Scale Dibuthyldithiocarbamate Synthesis by Experimental Design and Application as Extractant for Gadolinium(III)

The unique physical and chemical properties of Gadolinium (Gd) promote an indispensible number of its application for crucial technologies. In order to satisfy the demands of high purity, the various methods are used to separate Gd from other rare earth elements, in which a solvent extraction provides a simple separation method for these elements. However, an optimization of big scale is consequent for the solvent consumption. To overcome such a problem as a contribution in green chemistry, hereby we study the big scale synthesis optimization of dibuthyldithiocarbamate (DBDTC) by full factorial experimental design and the extraction study for Gd(III). This research start with preparing design of experiment for ligand synthesis, then perform the process of synthesis and extraction of Gd(III) according to the design of experiment. The result of synthesis and extraction were characterized by various spectroscopy methods. The highest Scale up ligand synthesis of DBDTC on this research is 20-fold times with 80.03% yield and 1.25% precision. The result shows that the optimal condition for Gd-DBDTC extraction are at pH 6, the mol ratio of gadolinium and ligand is 1:4, and 60 minutes extraction time with 76.52% yield. Therefore, the synthesis of dibuthyldithiocarbamate ligand based on the experimental design can be developed for optimization of large-scale synthesis with high Gd(III) extraction yield.

2018 ◽  
Vol 14 (1) ◽  
pp. 195
Author(s):  
Diana Hendrati ◽  
Erianti Siska Purnamasari ◽  
Syulastri Effendi ◽  
Santhy Wyantuti

<p>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 <em>contrast agent</em> 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%. Kesimpulan dari penelitian ini bahwa sintesis ligan dibutilditiokarbamat  berdasarkan desain eksperimen dapat dikembangkan untuk sintesis skala besar.</p><p>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<em> </em>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.</p>


2018 ◽  
Vol 14 (2) ◽  
pp. 219
Author(s):  
Diana Hendrati ◽  
Erianti Siska Purnamasari ◽  
Syulastri Effendi ◽  
Santhy Wyantuti

<p>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 <em>contrast agent</em> 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%.</p><p><strong>The Consolidation of Dibutyldithiocarbamate (DBDTC) Synthesis as Gadolinium Metal Extraction Based On Experimental Design. </strong>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<em> </em>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.</p>


2018 ◽  
Vol 14 (1) ◽  
pp. 84
Author(s):  
Diana Hendrati ◽  
Erianti Siska Purnamasari ◽  
Syulastri Effendi ◽  
Santhy Wyantuti

<p>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 <em>contrast agent</em> 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 %. Kesimpulan dari penelitian ini bahwa sintesis ligan dibutilditiokarbamat  berdasarkan desain eksperimen dapat dikembangkan untuk sintesis skala besar.</p><p>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<em> </em>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.</p>


2007 ◽  
Vol 1038 ◽  
Author(s):  
F. P. Doty ◽  
Douglas McGregor ◽  
Mark Harrison ◽  
Kip Findley ◽  
Raulf Polichar ◽  
...  

AbstractCerium and lanthanum tribromides and trichlorides form isomorphous alloys with the hexagonal UCl3 type structure, and have been shown to exhibit high luminosity and proportional response, making them attractive alternatives for room temperature gamma ray spectroscopy. However the fundamental physical and chemical properties of this system introduce challenges for material processing, scale-up, and detector fabrication. In particular, low fracture stress and perfect cleavage along prismatic planes cause profuse cracking during and after crystal growth, impeding efforts to scale this system for production of low cost, large diameter spectrometers. We have reported progress on basic materials science of the lanthanide halides. Studies to date have included thermomechanical and thermogravimetric analyses, hygroscopicity, yield strength, and fracture toughness. The observed mechanical properties pose challenging problems for material production and post processing; therefore, understanding mechanical behavior is key to fabricating large single crystals, and engineering of robust detectors and systems. Analysis of the symmetry and crystal structure of this system, including identification of densely-packed and electrically neutral planes with slip and cleavage, and comparison of relative formation and propagation energies for proposed slip systems, suggest possible mechanisms for deformation and crack initiation under stress. The low c/a ratio and low symmetry relative to traditional scintillators indicate limited and highly anisotropic plasticity cause redistribution of residual process stress to cleavage planes, initiating fracture. Ongoing work to develop fracture resistant lanthanide halides is presented.


2021 ◽  
Vol 09 ◽  
Author(s):  
Sarvat Zafar ◽  
Aiman Zafar ◽  
Fakhra Jabeen ◽  
Miad Ali Siddiq

: Nanotechnology studies the various phenomena of physio-chemical procedures and biological properties for the generation of nanosized particles, and their rising challenges in the various sectors, like medicine, engineering, agriculture, electronic, and environmental studies. The nanosized particles exhibit good anti-microbial, anti-inflammatory, cytotoxic, drug delivery, anti-parasitic, anti-coagulant and catalytic properties because of their unique dimensions with large surface area, chemical stability and higher binding density for the accumulation of various bio-constituents on their surfaces. Biological approaches for the synthesis of silver nanoparticles (AgNPs) have been reviewed because it is an easy and single-step protocol and a viable substitute for the synthetic chemical-based procedures. Physical and chemical approaches for the production of AgNPs are also mentioned herein. Biological synthesis has drawn attention because it is cost-effective, faster, non-pathogenic, environment-friendly, easy to scale-up for large-scale synthesis, and having no demand for usage of high pressure, energy, temperature, or noxious chemical ingredients, and safe for human therapeutic use. Therefore, the collaboration of nanomaterials with bio-green approaches could extend the utilization of biological and cytological properties compatible with AgNPs. In this perspective, there is an immediate need to develop ecofriendly and biocompatible techniques, which strengthen efficacy against microbes and minimize toxicity for human cells. The present study introduces the biological synthesis of silver nanoparticles, and their potential biomedical applications have also been reviewed.


Nanophotonics ◽  
2018 ◽  
Vol 7 (8) ◽  
pp. 1387-1422 ◽  
Author(s):  
Stefano L. Oscurato ◽  
Marcella Salvatore ◽  
Pasqualino Maddalena ◽  
Antonio Ambrosio

AbstractThe illumination of azobenzene molecules with UV/visible light efficiently converts the molecules between trans and cis isomerization states. Isomerization is accompanied by a large photo-induced molecular motion, which is able to significantly affect the physical and chemical properties of the materials in which they are incorporated. In some material systems, the nanoscopic structural movement of the isomerizing azobenzene molecules can be even propagated at macroscopic spatial scales. Reversible large-scale superficial photo-patterning and mechanical photo-actuation are efficiently achieved in azobenzene-containing glassy materials and liquid crystalline elastomers, respectively. This review covers several aspects related to the phenomenology and the applications of the light-driven macroscopic effects observed in these two classes of azomaterials, highlighting many of the possibilities they offer in different fields of science, like photonics, biology, surface engineering and robotics.


2020 ◽  
Vol 32 (6) ◽  
pp. 1433-1436 ◽  
Author(s):  
Tran Thi Kim Ngan ◽  
Nguyen Van Muoi ◽  
Pham Minh Quan ◽  
Mai Huynh Cang

This study attempted the extraction of essential oils from the peels of pomelo (Citrus grandis L.) grown in Ben Tre province, Vietnam through hydrodistillation method. In addition, the chemical composition and physio-chemical properties of the essential oils were reported. The results showed that the extraction yield of the extraction process achieved about 1.67%. The physico-chemical index of essential oils is determined by specific gravity (0.8572 g/cm3), acid index (0.3556 mg KOH/g), ester index (2.4216 mg KOH/g), and refractive index (1.476). The GC-MS analyses of the oil indicated the component with highest content in the oil was α-limonene (96.491%), followed by α-pinene (0.686%), β-pinene (0.248%), β-myrcene (1.644%), α-phellandrene (0.793%) and β-cis-ocimene (0.138%). These results suggested that wastes from fruit peeling process can be converted into a new material source with great potential for industrial use.


Chemosensors ◽  
2019 ◽  
Vol 7 (3) ◽  
pp. 33 ◽  
Author(s):  
Saylan ◽  
Erdem ◽  
Cihangir ◽  
Denizli

Human fecal contamination is a crucial threat that results in difficulties in access to clean water. Enterococcus faecalis is a bacteria which is utilized as an indicator in polluted water. Nevertheless, existing strategies face several challenges, including low affinity and the need for labelling, which limit their access to large scale applications. Herein, a label-free fingerprint of the surface proteins of waterborne bacteria on a sensor was demonstrated for real-time bacteria detection from aqueous and water samples. The kinetic performance of the sensor was evaluated and shown to have a range of detection that spanned five orders of magnitude, having a low detection limit (3.4 × 104 cfu/mL) and a high correlation coefficient (R2 = 0.9957). The sensor also designated a high selectivity while other competitor bacteria were employed. The capability for multiple usage and long shelf-life are superior to other modalities. This is an impressive surface modification method that uses the target itself as a recognition element, ensuring a broad range of variability to replicate others with different structure, size and physical and chemical properties.


2021 ◽  
Vol 12 ◽  
Author(s):  
Fangfang Chen ◽  
Zhihong Liu ◽  
Fan Jiang

Since December 2019, the SARS-CoV-2 has erupted on a large scale worldwide and spread rapidly. Passive immunization of antibody-related molecules provides opportunities for prevention and treatment of high-risk patients and children. Nanobodies (Nbs) have many strong physical and chemical properties. They can be atomized, administered by inhalation, and can be directly applied to the infected site, with fast onset, high local drug concentration/high bioavailability, and high patient compliance (no needles). It has very attractive potential in the treatment of respiratory viruses. Rapid and low-cost development of Nbs targeting SARS-CoV-2 can quickly be achieved. Nbs against SARS-CoV-2 mutant strains also can be utilized quickly to prevent the virus from escaping. It provides important technical supports for the treatment of the SARS-CoV-2 and has the potential to become an essential medicine in the toolbox against the SARS-CoV-2.


2022 ◽  
Vol 8 ◽  
Author(s):  
Sophie Clayton ◽  
Harriet Alexander ◽  
Jason R. Graff ◽  
Nicole J. Poulton ◽  
Luke R. Thompson ◽  
...  

In this article, we present Bio-GO-SHIP, a new ocean observing program that will incorporate sustained and consistent global biological ocean observations into the Global Ocean Ship-based Hydrographic Investigations Program (GO-SHIP). The goal of Bio-GO-SHIP is to produce systematic and consistent biological observations during global ocean repeat hydrographic surveys, with a particular focus on the planktonic ecosystem. Ocean plankton are an essential component of the earth climate system, form the base of the oceanic food web and thereby play an important role in influencing food security and contributing to the Blue Economy. Despite its importance, ocean biology is largely under-sampled in time and space compared to physical and chemical properties. This lack of information hampers our ability to understand the role of plankton in regulating biogeochemical processes and fueling higher trophic levels, now and in future ocean conditions. Traditionally, many of the methods used to quantify biological and ecosystem essential ocean variables (EOVs), measures that provide valuable information on the ecosystem, have been expensive and labor- and time-intensive, limiting their large-scale deployment. In the last two decades, new technologies have been developed and matured, making it possible to greatly expand our biological ocean observing capacity. These technologies, including cell imaging, bio-optical sensors and 'omic tools, can be combined to provide overlapping measurements of key biological and ecosystem EOVs. New developments in data management and open sharing can facilitate meaningful synthesis and integration with concurrent physical and chemical data. Here we outline how Bio-GO-SHIP leverages these technological advances to greatly expand our knowledge and understanding of the constituents and function of the global ocean plankton ecosystem.


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