Search results for "Carbon-13 NMR"
showing 10 items of 262 documents
Humic Substances for Agricultural Applications: Properties and Challenges
2021
Nowadays, humic substances, the main organic components of soils and many fossil sediments, are becoming a material of wide application in agriculture and many technologies. Elemental, functional and spectral (UV, fluorescence, FTIR, 13C NMR spectra) analysis of industrially produced, as well as reference humic substances demonstrate significant differences in properties of humic substances depending on their origin, and thus, their potential application in agriculture. For authentication of humic substances’ origin, their elemental composition, as well as stable isotope (δC, δN, δO) ratios can be used.
Synthesis and structure verification of two previously uncharacterized pentachlorobiphenyls: PCB 108 and PCB 127
1992
Abstract The synthesis and structure verification of two previously uncharacterized polychlorinated biphenyl (PCB) congeners mono- ortho -substituted 2,3,3′,4,5′-pentachlorobiphenyl (PCB 108) and non- ortho -substituted 3,3′,4,5,5′-pentachlorobiphenyl (PCB 127) is described. The synthesis was done by the method of aromatic arylation in the presence of isopentyl nitrite. The purification and separation of the compounds was done by flash-chromatography on Al2O3- and charcoal columns. The structures were verified by 1H NMR, 13C NMR, IR and mass spectroscopy.
Model compounds of spent bleach liquor: 2,3,6-trichloro-p-cymenene and 2,3,5-trichloro-p-cymenene
1991
Abstract 2,3,6-Trichloro-p-cymene (1) was synthesized by chlorination of p-cymene. A reaction mixture was distilled in a Fischer-Spaltrohr distilling apparatus. One fraction contained small quantities of chlorinated cymenenes (two isomers) which were concentrated by preparative gas chromatography. Their FTIR and mass spectra were recorded. In earlier paper the structures of 2,3,6-trichloro-p-cymenene were verified by means of its coupled 13C NMR and mass spectra. In the present work the mass and FTIR spectral data of 2,3,5-trichloro-p-cymenene and 2,3,6-trichloro-p-cymenene are published.
Characterization of Hardwood Soda-AQ Lignins Precipitated from Black Liquor through Selective Acidification
2016
In the development of integrated biorefinery process alternatives to produce value-added by-products, various black liquors from sulfur-free pulping processes offer potential feedstocks for recovering their main chemical constituents, lignin and aliphatic carboxylic acids. In this study, lignin fractions were obtained from silver birch (Betula pendula) soda-anthraquinone black liquor by carbonation (pH to about 8.5) or by acidification (pH to about 2) with H2SO4 after carbonation or directly. These fractions were characterized by Fourier transform infrared (FTIR), ultraviolet (UV), energy dispersive X-ray fluorescence (ED XRF), and 13C nuclear magnetic resonance (13C NMR) spectroscopy. In a…
Secondary structure of peptides. 4:13C-Nmr CP/MAS investigation of solid oligo- and poly(L-alanines)
1983
Primary and tertiary amine-initiated polymerizations of L-alanine-N-carboxyanhydride (L-Ala-NCA) were conducted at 20 or 100°C in a variety of solvents. The 75.5-MHz 13C-nmr CP/MAS spectra of the resulting poly(L-alanines) revealed that all samples contain both α-helix and pleated-sheet structures. Depending on the reaction conditions the α-helix content varied between ca. 1 and 99%. Reprecipitation from aprotic nonsolvents does not change the α-helix/β-sheet ratio, indicating that this ratio is thermodynamically controlled. Since relatively large amounts of oligopeptides of degree of polymerization (DP) 4–6 can be extracted by means of acetic acid, it is concluded that (a) most poly(L-alan…
Synthesis, molecular structure and stability of fused bicyclic Δ4-1,2,4-oxadiazoline Pt(II) complexes
2015
Abstract The reaction of trans -[PtCl 2 (NCR) 2 ] (R 1 = CH 2 CO 2 Me ( 1a ), R 2 = CH 2 Cl ( 1b )) with pyrroline N -oxide − O + N CHCH 2 CH 2 C Me 2 ( 4 ), at room temperature for 15 min, furnishes via [3+2] cycloaddition the fused bicyclic Δ 4 -1,2,4-oxadiazoline Pt(II) complexes trans- [PtCl 2 { N C(R)O N C(H)CH 2 CH 2 C Me 2 } 2 ] (R 1 = CH 2 CO 2 Me ( 5a ), R 2 = CH 2 Cl ( 5b )). Compounds 5a and 5b were refluxed in CH 2 Cl 2 for 1 week to afford the derived ketoimine Pt(II) complexes trans- [PtCl 2 {N(C( O)(R)) C CH 2 CH 2 C(Me 2 ) N H} 2 ] (R 1 = CH 2 CO 2 Me ( 6a ), R 2 = CH 2 Cl ( 6b )), respectively, as a result of the N–O bond cleavage of the oxadiazoline ring in 5 . The c…
Effect of RF Field Inhomogeneity and Sample Restriction on Spectral Resolution of CP/MAS-13C NMR Spectra of Natural Organic Matter
2010
It is well known that the induced B1 magnetic field in an NMR coil is inhomogeneously distributed. However, this issue has so far received little attention in the field of environmental NMR. As this research field often aims at quanti- tative results as well as relaxation phenomena, the repercussions of such inhomogeneity on peak integrals and relaxation times need to be taken into account. The objective of the present study was to test standard recording conditions on different sample positions in an NMR coil in order to determine the effect of the RF field inhomogeneity on the spectrum of a molecularly complex humic material and on some standard molecules of known structure and conformati…
Pairwise effects of chlorine substituents on the13C NMR chemical shifts of dichlorobicyclo[2.2.1]heptanes (norbornanes)
1984
The 13C NMR spectra of nine dichlorinated bicyclo[2.2.1]heptanes (norbornanes) have been measured and assigned. The pairwise effects of chlorine substituents which cause deviations from the additivity of single-substituent effects were investigated and are discussed. The largest effect found is the high-field shift of carbons bearing vicinal cis substituents. In the case of geminal substitution deviations from additivity were found to be to low field and large in the γ, smaller in the β and negligible in the α chemical shifts. The observed deviations for 1,3-disubstituted cases vary from −3.2 to +1.1 ppm at different carbons, allowing no simple explanation. Replacement of α-hydrogen in a di…
Interaction of metal ions with N-glycosylamines: isolation and characterization of the products of 4,6-O-benzylidene-N-(o-carboxyphenyl)-β-D-glucopyr…
2001
Metal-ion complexes of Li+, Na+, K+, Mg2+, Ca2+, Ba2+, Pb2+, Cd2+, Hg2+ with 4,6–O–benzylidene–N–(o–carboxyphenyl)–β–D–glucopyranosylamine were synthesized and isolated as solid products and characterized by analytical means as well as by spectral techniques, such as, 1H and 13C NMR, FTIR, absorption, FAB mass spectrometry, optical rotation and CD. While the alkali metal ions formed ML type of complexes, the other metal ions formed ML2 type complexes. Molecular weights of the complexes of Li+, Na+ and K+ were established based on the molecular-ion peaks in the FAB mass spectra. The saccharide portion remians in the β-anomeric form even after the complexation. The spectral data, as well as t…
Synthesis and spectroscopic characterization of dimethyl-, di-n-butyl-, di-t-butyl-and diphenyl-tin(iv) derivatives of dipeptides: Crystal and molecu…
1992
The dipeptide complexes R2SnL listed below have been synthesized: (a) Me2SnL; H2L = glycylalanine (H2GlyAla), glycylvaline (H2GlyVal), glycylmethionine (H2GlyMet), glycyltryptophan (H2GlyTrp), glycyltyrosine (H2GlyTyr); (b) nBu2SnL; H2L = H2GlyAla, H2GlyVal; (c) nBu2SnL.H2O; H2L = glycylglycine (H2GlyGly), H2GlyAla; (d) tBu2SnL; H2L = H2GlyAla, H2GlyVal; (e) tBu2SnGlyGly. H2O; (f) Ph2SnL; H2L = H2GlyAla, H2GlyVal, H2GlyTyr, H2GlyTrp; (g) Ph2Sn(HGlyVal)2. The crystal and molecular structures of nBu2SnGl Val have been determined by single-crystal X-ray diffraction. The polyhedron around tin is a distorted trigonal bipyramid, analogous to that of Et2SnGlyTyr (see Vornefeld et al., Appl. Organo…