scholarly journals Synthesis and Characterization of Caprolactam- based Ionic Liquids as Green Solvents

Author(s):  
Rania A. Naiyl ◽  
Fredrick O. Kengara ◽  
Kirimi H. Kiriamiti ◽  
Yousif A. Ragab

Aims: To synthesize and characterize six caprolactam-based ionic liquids (CPILs) by combination of caprolactam with different organic and inorganic Brønsted acids that can be utilized for lipid extraction from microalgae. Study design:  Experimental design include quantitative and qualitative. Place and duration of study: The study was done at Department of Chemistry & Biochemistry, School of Sciences and Aerospace Studies, Moi University (Kenya) between November 2020 and May 2021. Methodology: Six CPILs were prepared through a  simple neutralization reaction between Caprolactam and Brønsted acids such as Hydrochloric acid (HCl), Methane sulphonic acid (CH3SO3H), Trifluoromethanesulphonic acid (CF3SO3H), Acetic acid (CH3CO2H), Trifluoroacetic acid (CF3CO2H), and Sulfuric acid (H2SO4). The first three acids were used in the synthesis of CPILs for the first time. The chemical structures of the synthesized CPILs were characterized by Fourier transform infrared and Raman spectroscopy. The densities and viscosities were measured at 20 oC using the weight (pycnometer) and capillary viscometer (Oswald) methods, respectively. Results: All the CPILs were insoluble in hexane and had high miscibility with water and methanol. Fourier transform infrared and Raman spectra of the CPILs were compared with that of free Caprolactam. The characteristic absorption bands of the synthesized compounds showed a big shift in position and/or intensity (compared to caprolactam), indicating the formation of the CPILs. The results showed that both the density and viscosity increased with the molecular weight of the anion - except in Caprolactamium hydrogen sulphate (CPSA)- which could be due to the strong interactions between the cation and anion resulting from the dimerization between hydrogen sulphate anions.   Conclusion: The hydrophilic nature of the CPILs indicated by high miscibility with polar solvents (water and methanol) indicates that they are suitable for the dissolution of cellulose of microalgae cell wall and thus could result in high lipid extraction efficiency. Further studies should therefore utilize the synthesized CPILs in lipid extraction from microalgae.

2019 ◽  
Vol 1 (2) ◽  
pp. 1-7
Author(s):  
O.O. Shonekan ◽  
◽  
A.C. Otuka ◽  
D.K. Adeyemi ◽  
O.T. Fatunsin ◽  
...  

Background: Syzygium guineenses, (the most common and abundant specie in Nigeria) is a medicinal plant used by traditional practitioners in northern Nigeria for a variety of healing purposes. Objective: The main objective of this project was to carry out a comparison of antioxidant activities and Fourier Transform Infrared Spectrophotometric (FTIR) analysis on both methanol and hexane leaf extracts of S. guineenses. Methods: Phytochemical screening, Semi-quantitative DPPH (1,1-diphenyl-2-picrylhydrazyl)- dot blot assay and FTIR analysis were performed on both extracts to determine antioxidant activity and identify the functional groups present. Results: Phytochemicals tested for, were observed to be more prominent in the methanol extract than hexane. The in vitro antioxidant assay also revealed a more intense yellow colour of inhibition in methanol extract than the hexane extract. The FTIR spectra revealed different characteristic peak values with various functional compounds in both extracts. The methanol extract displayed major peaks of absorption at 3341 cm-1 (-OH) for alcohol, 1736 cm-1 (C=O) carbonyl group, 1161.83 cm-1, 1036.49 cm-1 (C-O) of esters. Other absorption bands like 1452.25 cm-1 and 1612.20 cm-1 for alkenes were present in both extracts. Conclusion: This result shows that the methanol extract of S. guineenseshas a higher potential of phytochemicals, antioxidants and functional groups than the hexane extract.


1996 ◽  
Vol 79 (5) ◽  
pp. 1116-1123 ◽  
Author(s):  
Magdi M Mossoba ◽  
Sarah Adams ◽  
John A G Roach ◽  
Mary W Trucksess

Abstract Gas chromatography/matrix isolation/Fourier transform infrared (GC/MI/FTIR) spectroscopy and GC/mass spectrometry (MS) were used to confirm the identities of trimethylsilyl (TMS) derivatives of trichothecene mycotoxins in naturally contaminated grains. Infrared spectral bands observed in the fingerprint region were unique for 10 trichothecene standards. Characteristic absorption bands were observed for the ester (near 1750 cm-1) and ketone (near 1700 cm-1) carbonyl stretching vibrations, the acetate CH3 symmetric bend (1370 cm-1), the epoxide ring (1262 cm-1), the trimethylsilyl CH3 in-plane deformation (1253 cm-1), the ester (O)C-O asymmetric stretching vibration (near 1244 cm-1), and several other bands including intense features due to the TMS function. Infrared bands observed under cryogenic matrix isolation conditions were compared with those found at room temperature in a potassium bromide matrix for 5 of these standards. Identities of deoxynivalenol (DON) from barley and mixed feed, nivalenol from wheat and barley, and DON and fusarenon-x from sweet corn were confirmed by comparison of their infrared spectral bands with those of standards. The identity of DON in the same test samples of sweet corn was confirmed further by GC/MS. GC/MS was also used to quantitate the levels of DON (67-455 ppm) in sweet corn test samples.


1980 ◽  
Vol 34 (1) ◽  
pp. 7-14 ◽  
Author(s):  
R. C. Wieboldt ◽  
B. A. Hohne ◽  
T. L. Isenhour

A method is presented for the direct analysis of interferometric data from gas chromatography Fourier transform infrared spectroscopy (GC/FTIR). A synthetic interferogram is initially produced which represents the characteristic absorption features of a particular functional group or compound class. A zero displacement correlation is performed between this test interferogram and each sample interferogram from the GC data. The presence of the desired functionality in the GC effluent is indicated by a small value of the resulting cumulative sum. A “correlogram” which emulates the response from a chemically specific GC detector is obtained by plotting the cumulative sum from each sample correlation. Synthetic interferograms representing infrared absorption bands which are truly specific for a particular functionality yield the best results.


Author(s):  
Maria Grazia Bridelli ◽  
Chiaramaria Stani ◽  
Roberta Bedotti

The two main ageing-inducing events in the collagenous tissues are the water loss and the formation of intermolecular crosslinks based on the reaction of collagen with matrix carbohydrates, following a mechanism known as non-enzymatic-glycation. With the aim to mimic the two deleterious processes for the protein structure, rat-tail collagen was submitted to hydration changes and allowed to interact with two sugars characterized by different reducing properties, D-glucose and D-ribose. Fourier transform infrared (FTIR) spectroscopy was employed to investigate the conformational changes induced in the protein by the two treatments by analyzing the subsequent spectra modifications. FTIR spectra monitored: i) the amplitude and position changes of the two characteristic absorption bands OH stretching and Amide I, in dependence on the humidity level: a significant hysteresis effect in the ν(OH) band (ν~3400 cm–1) amplitude of the protein dehydrated and then rehydrated to the initial relative humidity (aw=0.92- 0.06) may be related to the enhancement of the β-sheet fraction in the protein structure as revealed by the parallel modification in the Amide I band (ν~1650 cm–1); ii) the area of the carbohydrate double band peaking at 1080 cm–1 and 1031 cm–1, associated to the accumulation of the glycation products, depending on the sugar concentration and incubation time. The association of both sugars to collagen only minimally affects the protein secondary structure as revealed by Amide I band Gaussian analysis. The whole set of results suggests hints to hypothesize a self-assembly model for collagen molecules induced by ageing.


1988 ◽  
Vol 42 (1) ◽  
pp. 108-113 ◽  
Author(s):  
W. M. Coleman ◽  
Bert M. Gordon

A series of lactones and lactams have been examined by matrix isolation Fourier transform infrared spectrometry. The values for the carbonyl absorption bands fall between those reported for the same compounds in the vapor phase and solid state. Multiple absorption bands are found in the region of carbonyl absorption for compounds examined under the matrix isolation phase. Ring strain has a dramatic effect on simplifying the complexity of the spectra. Little or no aggregation effects are observed for either the lactones or lactams under accepted operating parameters. The effects of substituents on these systems are comparable to those found in the vapor-phase and solid-state data.


2009 ◽  
Vol 23 (3-4) ◽  
pp. 175-189 ◽  
Author(s):  
Iram Liaqat

Fourier transform-infrared (FT-IR) spectroscopy has become an important tool for rapid analysis of complex biological samples. The infrared absorbance spectrum could be regarded as a “fingerprint” which is a feature of biochemical substances. The FT-IR spectra of fresh and stored dried samples of six bacterial isolates (Klebsiellasp.,Bacillus cereus, Bacillus subtilis, Pseudomonas aeruginosa, Achromobacter xylosoxidans and Achromobactersp.) were observed by variation in sample preparation. The results indicated that variation in sample preparation did not affect the spectra of isolates. However, less promiment/absence of a small shoulder peak at 1738 cm−1was evident in fresh dried samples ofAchromobactersp. and A.xylosoxidanscompared to prominent and broad shoulder band at 1724 cm−1in stored dried samples of these two isolates. In addition to the established KBr pellet technique, attenuated total reflectance (ATR) spectroscopy was used to analyse the spectra of planktonic growth (−80°C liquid cultures) and biofilm growth of six isolates. ATR spectroscopy of −80°C planktonic and biofilm growth showed variation in absorption spectra in fingerprint (1200−900 cm−1) region. Two clear absorption bands were prominent in biofilm at 1175 and 1143 cm−1whereas, one prominent broad band at 1075 cm−1resulting from the overlapping of two band was noted in planktonic cultures. Biofilm forming capability of the six isolates was also determined by acridine orange staining method. The microscopic analysis of biofilms formed on glass slides revealed the presence of a matrix of exopolysaccharides and microcolonies typical of biofilm architecture. Maximum biofilm formation was observed after 175 h inP. aeruginosaandKlebsiellasp.


2008 ◽  
Vol 112 (34) ◽  
pp. 7816-7824 ◽  
Author(s):  
Steven D. Chambreau ◽  
Stefan Schneider ◽  
Michael Rosander ◽  
Tom Hawkins ◽  
Christopher J. Gallegos ◽  
...  

2016 ◽  
Vol 869 ◽  
pp. 283-287 ◽  
Author(s):  
Isabela Leão Amaral da Silva ◽  
Alice Barreto Bevitori ◽  
Lazaro Araújo Rohen ◽  
Frederico Muylaert Margem ◽  
Fabio de Oliveira Braga ◽  
...  

The world is ever more demanding materials that are not only less intensive in terms of processing energy but also environmentally friendly. Presently, issues like generalized pollution and global warming are renewing the interest of natural materials in substitution for synthetic ones. In fact, natural lignocellulosic fibers are today the subject of a growing number of studies. In particular, the jute fiber, has been investigated by various mechanical and thermal analyses. With the intention to further characterize this fiber, a specific method was considered in this work, the infrared spectroscopy. The Fourier Transform Infrared (FTIR) was used to reveal the most typical absorption bands of specific molecular components of jute fibers, in order to understand the interaction that occurs between the jute fiber and a polymer matrix.


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