Hybrids Obtained from Monoglyceride of Castor Oil with Hydroxyapatite for Applications in Bioinduction of Bone Tissue: Synthesis and Characterization

2018 ◽  
Vol 930 ◽  
pp. 184-189
Author(s):  
Milton Thélio de Albuquerque Mendes ◽  
Francisco Xavier Nobre ◽  
José Milton Elias de Matos

In this paper, we report the initial research to obtain hybrids (PU@Hap-1%, PU@Hap-2% and PU@Hap-3% compound by hydroxyapatite (Hap) synthesized by coprecipitation (CP) method, with monoglycerides (MG) of castor oil (Ricinus communis) polymerized with hexamethylene diisocyanate (HDI). Hap, was characterized by X-ray diffraction (XRD), Rietveld refinement, Fourier transform infrared (FTIR), RAMAN spectroscopy and X-ray fluorescence (XRF). Hybrids, MG and castor oil, were characterized by Fourier transform infrared (FTIR). XRD patterns and Rietveld refinement analysis confirmed that hexagonal phase for nanostructure for Hap, with average size particles D  12 nm, obtained by Scherrer equation and ration Ca/P = 2.13 (m/m) confirmed that XRF spectroscopy. FTIR and RAMAN spectra exhibited all active modes for vibrational stretches (1, 2, 3 and 4) of the phosphate groups () and vibrational modes of O-H bonds, present in the hexagonal structure for Hap in a ranger from 400 to 4000 cm-1 and 400 to 1100 cm-1, respectively. The conversion of castor oil (triglyceride) to MG, was monitored by FTIR spectroscopy, confirmed that increase of intensity active modes in 3317 cm-1 and 1741 cm-1, corresponding to the vibrations modes of O-H and C=O, respectively. Finally, we observed that all active modes in FTIR spectroscopy, corresponding to the hybrids: PU@Hap-1%, PU@Hap-2% and PU@Hap-3%, and Polyurethanes – PU (standard), confirmed the increase of intensity mode of the phosphate group with the increase of Hap in the polymerization of the mixture MG with HDI.

2021 ◽  
Vol 17 (3) ◽  
pp. 153-165
Author(s):  
Ika Monika ◽  
◽  
Datin Umar ◽  
Arie Hardian ◽  
Rina Astriana ◽  
...  

Karbon aktif dan TiO2 mereduksi SO2 melalui proses adsorpsi dan fotokatalitik. Kedua senyawa ini memiliki efektivitas adsorpsi rendah. Untuk meningkatkan aktivitas adsorpsi dilakukan kombinasi teknik adsorben dan fotokatalitik sehingga adsorpsi dapat optimal. Kombinasi dilakukan dengan membuat komposit karbon aktif/TiO2. Batubara dan semi-kokas dicampur dengan perbandingan 7:3 kemudian TiO2 ditambahkan dengan konsentrasi 1, 3, 6, 9 dan 15%. Karbon aktif/ TiO2 dikarbonisasi pada suhu 600 °C selama 1 jam dan diaktivasi pada suhu 900 °C selama 1 dan 2 jam di bawah aliran gas nitrogen. Hasil analisis fourier-transform infrared (FTIR) spectroscopy menunjukkan intensitas serapan gugus fungsi C=O naik sebesar 49,5% pada karbon aktif/TiO2 6% selama 1 jam dan 33,2% pada karbon aktif/TiO2 3% selama 2 jam. Gugus fungsi basa C=O mereduksi gas SO2 yang bersifat asam. Hasil X-ray diffraction (XRD) ditemukan kristal TiO2 anatas dan rutil. Koeksistensi kristal anatas dan rutil lebih efektif daripada anatas dan rutil fase tunggal. Hasil penelitian ini menunjukkan bahwa karbon aktif/TiO2 meningkatkan aktivitas gugus fungsi permukaan karbon aktif dan membentuk kristal TiO2 anatas dan rutil secara bersama.


2021 ◽  
Vol 33 (1) ◽  
pp. 113-138
Author(s):  
Michael C. Jollands ◽  
Hugh St.C. O'Neill ◽  
Andrew J. Berry ◽  
Charles Le Losq ◽  
Camille Rivard ◽  
...  

Abstract. Single crystals of synthetic Cr-doped forsterite (Cr:Mg2SiO4) containing both Cr3+ and Cr4+ were partially hydroxylated in piston-cylinder apparatuses at 750–1300 ∘C and pressures from 0.5 to 2.5 GPa, with p(H2O) ≈Ptotal. The oxygen fugacity (fO2) was buffered by graphite-water, Ni–NiO, Re–ReO2, Fe2O3–Fe3O4 or Ag–Ag2O, and the silica activity (aSiO2) was buffered by powdered forsterite plus either enstatite (Mg2Si2O6), periclase (MgO) or zircon–baddeleyite (ZrSiO4–ZrO2). Profiles of OH content versus distance from the crystal edge were determined using Fourier transform infrared (FTIR) spectroscopy, and profiles of the oxidation state and coordination geometry of Cr were obtained, at the same positions, using K-edge X-ray absorption near-edge structure (XANES) spectroscopy. The techniques are complementary – FTIR spectroscopy images the concentration and nature of O–H bonds, where Cr K-edge XANES spectroscopy shows the effect of the added H on the speciation of Cr already present in the lattice. Profiles of defect-specific absorbance derived from FTIR spectra were fitted to solutions of Fick's second law to derive diffusion coefficients, which yield the Arrhenius relationship for H diffusion in forsterite: log⁡10D̃[001]=-2.5±0.6+-(224±12+4.0±2.0P)2.303RT, where D̃ is the measured diffusion coefficient in m2 s−1, valid for diffusion parallel to [001] and calibrated between 1000 and 750 ∘C, P and T are in GPa and K, and R is 0.008314 kJK−1 mol−1. Diffusivity parallel to [100] is around 1 order of magnitude lower. This is consistent with previous determinations of H diffusion associated with M-site vacancies. The FTIR spectra represent a variety of Cr-bearing hydrous defects, along with defects associated with the pure Mg–Si–O–H system. It is proposed that all of the defects can form by interaction between the dry lattice, including Cr3+ and Cr4+, and fully hydroxylated M-site vacancies. The initial diffusive wave of hydroxylation is associated with neither reduction nor oxidation of Cr but with Cr4+ changing from tetrahedral to octahedral coordination. Superimposed on the H diffusion and concomitant change in Cr4+ site occupancy, but at a slower rate, producing shorter profiles, is reduction of Cr4+ to Cr3+ and potentially of Cr4+ and Cr3+ to Cr2+. In addition, by comparing FTIR data to trace element contents measured by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), constraints can be placed on absorption coefficients used for converting absorbance to H2O contents – our data support either wavenumber- or defect-dependent values of absorption coefficients. We estimate absorption coefficients of between 60 200 and 68 200 L mol−1 cm−1 for OH− associated with octahedral Cr3+ and an M-site vacancy and 18 700 to 24 900 L mol−1 cm−1 for two OH− associated with octahedrally coordinated Cr4+ and a Si vacancy (i.e. a “clinohumite-type” point defect).


SPAFA Journal ◽  
2021 ◽  
Vol 5 ◽  
Author(s):  
Jan-Michael Cayme

Countries in Southeast Asia have a unique and diverse culture due to its varied ethnic groups having different traditions and beliefs. The process of manufacturing building materials such as brick masonry is one aspect where this distinctiveness is manifested. This study provides a general analytical chemistry method that will estimate the original firing temperature of a historical brick material from a convent in Milaor, Camarines Sur, Philippines. Different instrumental techniques were utilized namely the Energy Dispersive X-ray Fluorescence (EDXRF), Fourier Transform Infrared (FTIR) Spectroscopy and Scanning Electron Microscopy with Energy Dispersive X-ray (SEM-EDX). From these techniques, the chemical and mineralogical composition of the brick was reported. The clay mixture used in the production of the brick is known to be non-calcareous and low refractory, that was fired in an oxidizing atmosphere. The brick’s microstructure is classified within the initial vitrification stage based on the features of the mineral transformations. The results of this study point to an estimated firing temperature range of 650°C to 850°C. An emphasis on the importance of chemical analysis in studying cultural heritage materials in the Southeast Asian region is also highlighted on this paper.  Ang mga bansa sa Timog-Silangang Asya ay may natatangi at magkakaibang kultura sanhi ng iba’t ibang mga pangkat etniko na may magkakaibang tradisyon at paniniwala. Ang pamamaraan ng paggawa sa mga materyales ng lumang gusali tulad ng ladrilyo ay isang aspeto kung saan naipapamalas ang pagkakaiba-iba nito. Ang pagaaral na ito ay nagbibigay ng isang pangkalahatang pamamaraan ng mapanuring-kimika para tantyahin ang orihinal na temperatura ng paggawa sa lumang ladrilyo mula sa isang kumbento ng Milaor, Camarines Sur, Pilipinas. Iba’t ibang mga instrumento ang ginamit tulad ng Energy Dispersive X-ray Fluorescence (EDXRF), Fourier Transform Infrared (FTIR) Spectroscopy at ang Scanning Electron Microscopy na nakakabit sa Energy Dispersive X-ray (SEM-EDX). Mula sa mga intrumentong ito, ang kemikal at mineral na komposisyon ng ladrilyo ay iniulat. Ang mga pinaghalong luad na ginamit sa paggawa ng ladrilyo ay masaasabing hindi gaanong madami ang bilang ng kalsiyo at mababang refractory, na sinunog sa isang kapaligiran na sagana sa hangin. Ang mga pinaka-maliliit na istruktura ng ladrilyo ay masasabing nasa paunang yugto ng pagtunaw ng mga mineral sa luad, batay sa mga pagbabagong anyo ng mga ito. Sa mga resulta ng pagaaral, masasabi na ang tantyang temperatura ng pagsunog ay nasa 650°C hanggang 850°C. Binibigyan ng diin ang kahalagahan ng pagsusuri ng kimika sa pagaaral ng mga materyales na pamanang kultura sa rehiyon ng Timog-Silangang Asya ay naitala din sa pagaaral na ito.


Elkawnie ◽  
2020 ◽  
Vol 6 (1) ◽  
pp. 85
Author(s):  
Saharman Gea ◽  
Agus Haryono ◽  
Andriayani Andriayani ◽  
Junifa Layla Sihombing ◽  
Ahmad Nasir Pulungan ◽  
...  

Abstract : Material characteristics analysis of Sarulla natural zeolite (SNZ) with base activation has been carried out. The base used was NaOH at various concentrations; 0.2 M, 0.5 M, and 2 M. Base activated catalysts were characterized by X-ray Fluorescence (XRF), X-ray diffractometer (XRD), Fourier-transform Infrared (FTIR) Spectroscopy, Scanning Electron Microscopy (SEM) and gas adsorption analysis using BET method. The procedures applied have caused differences in adsorption and desorption rates as well as the crystallinity values of the catalytic materials. Moreover, the ratio of Si/Al contents has also changed at the lowest concentration. On the other hand, the crystallinity of catalysts has decreased at the highest concentration of base applied. The results are reinforced in FTIR characterization which shows the changes of silanol bonds to become silicate and aluminate. Furthermore, morphological analysis of the catalysts shows that homogenous surface was obtained at low concentration, while rough/lumpy surfaces was obtained at higher concentration.Abstrak : Analisis terhadap karakteristik material dari zeolit alam Sarulla (SNZ) dengan metode aktivasi basa telah dilakukan. Basa yang digunakan ialah NaOH dengan berbagai konsentrasi; 0,2 M; 0,5 M, dan 2 M. Katalis yang telah diaktivasi dengan basa kemudian dikarakterisasi dengan Analisis X-ray Fluorescence (XRF), X-ray diffractometer (XRD), Fourier-transform Infrared (FTIR) Spectroscopy, Scanning Electron Microscopy (SEM) dan Gas Adsorption menggunakan metode BET. Dari hasil penelitian, ditemukan perbedaan pada tingkat adsorpsi dan desorpsi, begitu juga dengan kristalinitas pada material katalis. Lebih jauh, rasio konten Si/Al juga berubah pada basa dengan konsentrasi terendah. Di sisi lain, tingkat kristalinitas dari katalis mengalami penurunan pada basa dengan konsentrasi tertinggi. Hasil ini diperkuat dengan data FTIR yang menunjukkan perubahan ikatan silanol menjadi silikat dan aluminat. Lebih jauh, analisis morfologi pada katalis menunjukkan bahwa permukaan yang homogen didapatkan dari penggunaan basa dengan konsentrasi rendah. Sebaliknya, basa dengan konsentrasi tinggi memberikan bentuk permukaan katalis yang tidak homogen serta kasar.


2020 ◽  
Vol 851 ◽  
pp. 220-227
Author(s):  
Sukarni Sukarni ◽  
Lukman Arifianto Andi Saputra

The availability of synthetic waste (SW) continuously increases, but on the contrary fossil fuels resources always decrease. The potential of SW for alternative fuel is critical to investigate for overcoming the problem generated from its overabundance and to provide its value-added. In this study, the changes of the macromolecular and the mineralogical during the SW combustion processes were investigated by Fourier Transform Infrared (FTIR) spectroscopy and x-ray diffraction (XRD), respectively. The combustion has been performed by using thermogravimetric analyzer (TGA) at a heating rate of 10 °C/min, from 25 to 1000 °C, with 100 ml/min constant flowrate of air atmosphere. According to the TGA results, the decomposition stage of the sample can be identified as a function of temperature and time. From ambient temperatures to 293 °C the sample experienced the first decomposition process that was correlated with the moisture losses and light volatile release. Macromolecular changes occurred at the temperature 293 °C where functional group of C–H in methylene was decomposed due to the removal of volatile matter. From the temperature of 293 to 485 °C the sample underwent the second stage of decomposition. The XRD result showed that mineral changes occurred at the temperature of 485 °C where the KCl compound was formed. In line with the escalating temperature, SiO2 was decomposed at a temperature of 590 °C. The final stage occurred at the temperature 625 to 1000 °C indicated by constant of TG line. At 625 °C, XRD result indicated the significant increasing of the CaCO3 compound.


2017 ◽  
Vol 43 (5) ◽  
pp. 2752 ◽  
Author(s):  
E. Theodosoglou ◽  
A. Koroneos ◽  
T. Soldatos ◽  
T. Zorba ◽  
K. M. Paraskevopoulos

Natural K-feldspars from igneous rocks have been examined by means of X-ray powder diffraction(XRPD) and Fourier transform infrared (FTIR) spectroscopy in the spectral range 400-1400 cm-1,where the Si-Al-O bonds exhibit the dominant vibrations. From the XRPD analysis three specieshave been distinguished, i.e. microclines (3 samples), orthoclases (4 samples) and sanidines (3 samples);their unit cell parameters were calculated. The FTIR transmittance spectra of all sampleshave common bands at 426, 463, 584, 604, 726 and 772 cm-1 and some additional features. The spectraof sanidine and orthoclase exhibit fewer and broader bands than the microclines’, especially inthe area 1000-1200 cm-1. The differences in their spectra are located in four bands. The bands ataround 536-538 and 646-648 cm-1 in the spectrum of microcline, are shifted at around 542-544 and640-642 cm-1 in the spectrum of orthoclase and at around 546 and 636 cm-1 in the spectrum of sanidine.Four bands at 1010, 1050, 1090 and 1136 cm-1 in the spectra of microcline are substitutedwith two quite broad bands at about 1030 and 1125 cm-1 in the spectra of orthoclase and sanidine.These differences are attributed to different degree of Al-Si ordering in the structure of K-feldspars.


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.


2019 ◽  
Vol 70 (8) ◽  
pp. 2747-2752
Author(s):  
Constantin Marutoiu ◽  
Ioan Bratu ◽  
Mircea Gelu Buta ◽  
Olivia Florena Nemes ◽  
Sergiu Petru Timbus(Monk Siluan) ◽  
...  

A two-sided wooden icon from a monastery in Transylvania was submitted for multidisciplinary investigations involving X-Ray Fluorescence, Radiographic Photographyand Fourier Transform Infrared Spectroscopy. The most important part of the icon is St. Nicholas wooden icon, painted over forty years ago. The spectroscopic methods used revealed the painting materials composition, the status of the wooden stage, and the presence of resins as varnish (Fourier Transform Infrared Spectroscopy). On one side, the St Nicholasicon was painted over an old icon, St. Arch. Michael, which was evidenced by X-Ray Photography. The obtained data can serve for the preservation and the restoration of these wooden icons.


2021 ◽  
pp. 002580242110109
Author(s):  
Sweety Sharma ◽  
Rito Chophi ◽  
Jaskirandeep Kaur Jossan ◽  
Rajinder Singh

The most important task in a criminal investigation is to detect and identify the recovered biological stains beyond reasonable scientific doubt and preserve the sample for further DNA analysis. In the light of this fact, many presumptive and confirmatory tests are routinely employed in the forensic laboratories to determine the type of body fluid. However, the currently used techniques are specific to one type of body fluid and hence it cannot be utilized to differentiate multiple body fluids. Moreover, these tests consume the samples in due process, and thus it becomes a great limitation especially considering the fact that samples are recovered in minute quantity in forensic cases. Therefore, such limitations necessitate the use of non-destructive techniques that can be applied simultaneously to all types of bodily fluids and allow sample preservation for further analysis. In the current work, attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy has been used to circumvent the aforementioned limitations. The important factors which could influence the detection of blood such as the effect of substrates, washing/chemical treatment, ageing, and dilution limits on the analysis of blood have been analysed. In addition, blood discrimination from non-blood substance (biological and non-biological in nature) has also been studied. Chemometric technique that is PCA–LDA has been used to discriminate blood from other body fluids and it resulted in 100% accurate classification. Furthermore, blood and non-blood substances including fake blood have also been classified into separate clusters with a 100% accuracy, sensitivity, and specificity. All-inclusive, this preliminary study substantiates the potential application of ATR-FTIR spectroscopy for the non-destructive identification of blood traces in simulated forensic casework conditions with 0% rate of false classification.


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