scholarly journals [FeII(L•)2][TCNQF4•−]2: A Redox-Active Double Radical Salt

2019 ◽  
Vol 72 (10) ◽  
pp. 769 ◽  
Author(s):  
Ian A. Gass ◽  
Jinzhen Lu ◽  
Ruchika Ojha ◽  
Mousa Asadi ◽  
David W. Lupton ◽  
...  

The reaction of [FeII(L•)2][BF4]2 with LiTCNQF4 results in the formation of [FeII(L•)2][TCNQF4•−]2·2CH3CN (1) (L• is the neutral aminoxyl radical ligand 4,4-dimethyl-2,2-di(2-pyridyl)oxazolidine-N-oxide; TCNQF4 is 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane). Single-crystal X-ray diffraction; Raman, Fourier-transform infrared (FTIR) and ultraviolet–visible spectroscopies; and electrochemical studies are all consistent with the presence of a low-spin FeII ion, the neutral radical form (L•) of the ligand, and the radical anion TCNQF4•−. 1 is largely diamagnetic and the electrochemistry shows five well-resolved, diffusion-controlled, reversible one-electron processes.

Author(s):  
John A. Sutliff

Near-eutectic Pb-Sn alloys are important solders used by the electronics industry. In these solders, the eutectic mixture, which solidifies last, is the important microstructural consituent. The orientation relation (OR) between the eutectic phases has previously been determined for directionally solidified (DS) eutectic alloys using x-ray diffraction or electron chanelling techniques. In the present investigation the microstructure of a conventionally cast, hyper-eutectic Pb-Sn alloy was examined by transmission electron microscopy (TEM) and the OR between the eutectic phases was determined by electron diffraction. Precipitates of Sn in Pb were also observed and the OR determined. The same OR was found in both the eutectic and precipitation reacted materials. While the precipitation of Sn in Pb was previously shown to occur by a discontinuous precipitation reaction,3 the present work confirms a recent finding that volume diffusion controlled precipitation can also occur.Samples that are representative of the solder's cast microstructure are difficult to prepare for TEM because the alloy is multiphase and the phases are soft.


Arena Tekstil ◽  
2013 ◽  
Vol 28 (1) ◽  
Author(s):  
Maya Komalasari ◽  
Bambang Sunendar

Partikel nano TiO2 berbasis air dengan pH basa telah berhasil disintesis dengan menggunakan metode sol-gel dan diimobilisasi pada kain kapas dengan menggunakan kitosan sebagai zat pengikat silang. Sintesis dilakukan  dengan prekursor TiCl4 pada konsentrasi 0,3 M, 0,5 M dan 1 M, dan menggunakan templat kanji dengan proses kalsinasi pada suhu 500˚C selama 2 jam. Partikel nano TiO2 diaplikasikan ke kain kapas dengan metoda pad-dry-cure dan menggunakan kitosan sebagai crosslinking agent. Berdasarkan hasil Scanning Electron Microscope (SEM),diketahui bahwa morfologi partikel TiO2 berbentuk spherical dengan ukuran nano (kurang dari 100 nm). Karakterisasi X-Ray Diffraction (XRD) menunjukkan adanya tiga tipe struktur kristal utama, yaitu (100), (101) dan (102) dengan fasa kristal yang terbentuk adalah anatase dan rutile. Pada karakterisasi menggunakan SEM terhadap serbuk dari TiO2 yang telah diaplikasikan ke permukaan kain kapas, terlihat adanya imobilisasi partikel nano TiO2 melalui ikatan hidrogen silang dengan kitosan pada kain kapas. Hasil analisa tersebut kemudian dikonfirmasi dengan FTIR (Fourier Transform Infra Red) yang hasilnya memperlihatkan puncak serapan pada bilangan gelombang 3495 cm-1, 2546 cm-1, dan 511 cm-1,  yang masing-masing diasumsikan sebagai adanya vibrasi gugus fungsi O-H, N-H dan Ti-O-Ti. Hasil SEM menunjukkan pula bahwa kristal nano yang terbentuk diantaranya adalah fasa rutile , yang berdasarkan literatur terbukti dapatberfungsi sebagai anti UV.


2016 ◽  
Vol 5 (1) ◽  
pp. 6
Author(s):  
Budi Setiawan ◽  
Erizal Zaini ◽  
Salman Umar

Sebuah penelitian tentang sistem dispersi padat dari asiklovir dengan poloxamer 188 telah dilakukan formulasi dengan pencampuran secara fisika dengan rasio 1 : 1, 1 : 3, 1 : 5 dan dispersi padat 1 : 1, 1 : 3, 1 : 5 dan penggilingan 1:1 sebagai pembanding. Dispersi padat dibuat menggunakan metode pencairan (fusi), yang digabung dengan poloxamer 188 pada hotplate kemudian asiklovir dimasukkan ke dalam hasil poloxamer 188 lalu di kocok hingga membentuk masa homogen. Semua formula yang terbentuk termasuk asiklovir poloxamer 188 murni dianalisis karakterisasinya dengan Differential Thermal Analysis (DTA), X-ray Diffraction, Scanning Electron Microscopy (SEM), dan Fourier Transform Infrared (FTIR), kemudian pengambilan dilakukan  (penentuan kadar) mengunakan spektrofotometer UV pada panjang gelombang 257,08 nm dan uji laju disolusi dengan aquadest bebas CO2 menggunakan metode dayung. Hasil pengambilan  (penentuan kadar) menunjukkan bahwa semua formula memenuhi persyaratan farmakope Amerika edisi 30 dan farmakope Indonesia edisi 4 yaitu 95-110%. Sedangkan hasil uji laju disolusi untuk campuran fisik 1: 1, dan dispersi padat 1: 1, dan penggilingan 1: 1 menunjukkan peningkatan yang nyata dibandingkan asiklovir murni. Hal ini juga dapat dilihat dari hasil perhitungan statistik  menggunakan analisis varian satu arah  SPSS 17.


2021 ◽  
Vol 317 ◽  
pp. 426-433
Author(s):  
Siti Nurhaziqah Abd Majid ◽  
Afiqah Qayyum Ishak ◽  
Nik Aziz Nik Ali ◽  
Muhamad Zalani Daud ◽  
Hasiah Salleh

The development of biopolymer electrolytes based on methylcellulose (MC) has been accomplished by incorporating ammonium bromide (NB) to the polymer-salt system. The biopolymer electrolytes were prepared via solution-casting method. The conductivity and permittivity characteristics of the material were studied. The biopolymer-salt complex formation have been analysed through Fourier Transform Infrared (FTIR) spectroscopy and X-ray diffraction (XRD). The conductivity of the sample was measured by EIS HIOKI. Upon addition of 20 wt.% of NB, highest conductivity of 3.25×10-4 μScm-1 was achieved at ambient temperature. The temperature dependence of the biopolymer electrolytes exhibit Arrhenius behaviour. This result had been further proven in FTIR study.


2012 ◽  
Vol 476-478 ◽  
pp. 2059-2062
Author(s):  
Chen Wang ◽  
Ya Dong Li ◽  
Gu Qiao Ding

Tributyl borate was first adopted for the introduction of boron in the preparation of bioactive borosilicate xerogel by sol-gel method. The xerogel reacted continuously in 0.25M K2HPO4 solution with a starting pH value of 7.0 at 37 °C for 1day. The structural, morphologies and compositional changes resulting from the conversion were characterized using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy. The results indicated that speed of formation of HA was cut way back on the time with the addition of boron and the induction period for the HA nucleation on the surface of the borosilicate xerogel was short than 1 days. The conversion mechanism of the borosilicate xerogels to hydroxyapaptite was also discussed.


Author(s):  
Alaa Mohamed Elsafi ◽  
Vinotha Krishnasamy ◽  
Karthik Kannan ◽  
John-John Cabibihan ◽  
Abdulaziz Khalid AlAli ◽  
...  

High levels of glucose or acetone in breath confirms diabetes disease. One of the analytical devices that detect changes in breath is the electrochemical sensor having high selectivity, easy to use and being able to meet diabetic patient’s needs. In this study, sensors were made by fabricating metal oxide coated glassy carbon electrodes and using nafion as a proton conductor. Characterization methods such as X-ray diffraction, FTIR and morphological analysis have been performed for metal oxides to characterize their atomic arrangement and composition. In addition, electrochemical studies were done using Gamry instrument and curves plotted as current in amperes versus voltage to test the coated electrodes conductivity. High selectivity sensors provide promising applications in any field.


2020 ◽  
Vol 16 (2) ◽  
pp. 12
Author(s):  
Solihudin Solihudin ◽  
Haryono Haryono ◽  
Atiek Rostika Noviyanti ◽  
Muhammad Rizky Ridwansyah

<p>Komposit forsterit-karbon merupakan salah satu material modifikasi dari forsterit yang berpotensi memiliki sifat isolator panas baik. Karbon dalam komposit dapat mengisi cacat titik pada kristal forsterit. Arang sekam padi (residu gasifikasi) mengandung SiO2 amorf dan karbon yang tinggi. Penelitian ini bertujuan menentukan pengaruh suhu kalsinasi dalam medium gas inert (dengan pengaliran gas argon) terhadap karakteristik komposit forsterit-karbon dari arang sekam padi dan magnesium karbonat. Metode penelitian meliputi preparasi arang sekam padi hasil gasifikasi, dan sintesis forsterit-karbon. Proses sintesis komposit forsterit karbon dilakukan dengan cara mencampurkan arang sekam padi dengan kalium karbonat pada rasio mol magmesium terhadap silikon sebesar 2 : 1 kemudian dikalsinasi dengan suhu divariasikan (700, 800, 900, dan 1000 oC). Selanjutnya sampel hasil sintesis dikarakterisasi dengan Fourier-transform infrared (FTIR), X-ray diffraction (XRD), dan scanning electron microscope-energy dispersive spectroscopy (SEM-EDS). Hasil karakterisasi dengan FTIR dan XRD diperoleh kesimpulan bahwa forsterit mulai terbentuk pada suhu kalisiasi 800 oC dan sempurna pada suhu 1000 oC, karenanya komposit yang terbentuk pada 1000 oC dimungkinkan sebagai forsterit-karbon, di mana unsur-unsur yang terkandung ditunjukkan oleh SEM-EDS.</p><p> </p><p><strong>The Effect of Calcination Temperature on the Characteristics of Forsterite-Carbon Composites Synthesized in Argon Gas Medium</strong>. Forsterite-carbon composite is one of the material modifications of forsterite, which potentially has a good heat insulation property. Carbon in composites can fill point defects in forsterite crystals. Rice husk charcoal, as gasification residues, contains high amorphous SiO2 and carbon. This study aims to determine the effect of temperature on the calcination of a mixture of rice husk charcoal and magnesium carbonate under an inert gas (argon gas) on the characteristics of the forsterite-carbon composite produced. The experimental research performed includes the preparation of gasified rice husk charcoal and the synthesis of the carbon-forsterite composite. The synthesis process of the carbon-forsterite composites was carried out by mixing rice husk charcoal with potassium carbonate at a mole ratio of magnesium to silicon of 2 : 1. The mixture was then calcined with varying temperatures (700, 800, 900, and 1000 °C). Furthermore, the synthesized sample was characterized by Fourier-transform infrared (FTIR), X-ray diffraction (XRD), and scanning electron microscope-energy dispersive spectroscopy (SEM-EDS). The FTIR and XRD analysis show that the forsterites began to form at a calcination temperature of 800 °C and perfectly formed at a temperature of 1000 °C; therefore, the composite formed at 1000 °C is possible as forsterite-carbon, in which the contained elements were indicated by SEM-EDS.</p>


2019 ◽  
Vol 29 (2) ◽  
Author(s):  
Mutia Dewi Yuniati ◽  
Feronika Cinthya Mawarni Putri Wawuru ◽  
Anggoro Tri Mursito ◽  
Iwan Setiawan ◽  
Lediyantje Lintjewas

Magnesite (MgCO3) is the main source for production of magnesium and its compound. In Indonesia, magnesite is quite rare and can be only found in limited amount in Padamarang Island, Southeast Sulawesi Provence. Thus the properties of magnesite and the reactivity degree of the obtained product are of technological importance. The aim of this work was to analyze the characteristics of Padamarang magnesite under calcination and hydrothermal treatment processes. The processes were carried out at various temperatures with range of 150-900°C for 30 minutes. The solids were characterized with respect to their chemical and physical properties by using scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX), Fourier-transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). SEM image indicates that magnesite was formed from thin and flat hexagon sheets. The FTIR and XRD analysis disclose that MgO formed at temperature above 300°C, where as the magnesite sample also lost its mass around 50%. These results demonstrate that Padamarang magnesite decomposes to magnesium oxide and carbon dioxide at high temperature.Magnesit (MgCO3) merupakan sumber utama untuk produksi magnesium dan senyawa-senyawanya. Di Indonesia, magnesit cukup jarang dan hanya dapat ditemukan dalam jumlah yang terbatas di Pulau Padamarang, Propinsi Sulawesi Tenggara. Oleh karena itu sifat magnesit dan derajat reaktivitas dari produk-produk magnesit penting untuk diketahui. Penelitian ini bertujuan untuk menganalisis karakteristik magnesit Padamarang dengan perlakuan kalsinasi dan hidrothermal.  Proses dilakukan pada temperatur yang bervariasi dari 150-900°C selama 30 menit. Sifat kimia dan fisika dari magnesit dikarakterisasi dengan menggunakan scanning electron microscopy dengan energy-dispersive X-ray spectroscopy (SEM-EDX), Fourier-transform infrared spectroscopy (FTIR), dan X-ray diffraction (XRD). Gambar dari analisis SEM menunjukkan bahwa magnesit terbentuk dari lembaran-lembaran heksagonal yang tipis dan datar. Hasil analisis dengan FTIR dan XRD menunjukkan bahwa MgO terbentuk pada temperatur diatas 300°C, dimana sampel magnesit juga kehilangan massanya sekitar 50% pada suhu tersebut. Hal ini menunjukkan bahwa Magnesit Padamarang terdekomposisi menjadi magnesium oksida dan karbon dioksida pada temperatur tinggi.


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