13 C NMR cross polarization and magic angle spinning (CPMAS) and gas chromatography/mass spectrometry analysis of the products from a soda pulp mill effluent decolourised by two Streptomyces strains

The application of a sugarcane distillery waste known as vinasse to agricultural land has become a common practice in Brazil. The vinasse samples used in this study were collected from several sugarcane distilleries in Northeastern Brazil. These samples were fractionated into dissolved organic carbon (DOC) and particulate organic carbon (POC) fractions. Unfractionated and fractionated vinasse were studied using 13C cross-polarization and magic-angle spinning nuclear magnetic resonance (CP/MAS NMR) spectroscopy as well as diffuse reflectance Fourier-transform infrared (DR-FTIR) spectroscopy. Approximately 79 to 92% of the total unfractionated vinasse dry matter was in the form of DOC fraction. O-alkyl C (42–53% of the total C) and carboxyl C (12–25% of the total C) comprised a significant portion of the 13C NMR spectra of the DOC fraction. The presence of carbohydrates and COOH/COO− was suggested by the DR-FTIR as well. Both 13C NMR and DR-FTIR spectra of this fraction were generally similar to the spectra of the fulvic acid (FA) fraction of soil and sewage sludge. The spectra of DOC differed from the FA fraction in that they showed smaller amounts of aromatic C and had an absence of amide group (bands at 1650 cm−1 and 1540 cm−1). In the POC fraction, O-alkyl (17–52% of the total C) and alkyl C (15–41% of the total C) were the major contributors. The peaks at 62 ppm, 72 ppm, 84 ppm and 105 ppm in the O-alkyl region indicate the presence of cellulose and/or hemicellulose. The alkyl group was comprised mainly of long-chain structures. The total N content in this fraction is ~3–7 times as much as in the DOC fraction. The presence of amino acids in the POC fraction was suggested by both 13C NMR and DR-FTIR spectra. Key words:13C cross-polarization and magic-angle spinning nuclear magnetic resonance, dissolved organic carbon, Fourier-transform infrared, particulate organic carbon, vinasse

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Analysis of lignin and extractives in the oak wood of the 17th century warship Vasa

Holzforschung ◽

10.1515/hf-2013-0067 ◽

2014 ◽

Vol 68 (4) ◽

pp. 419-425 ◽

Cited By ~ 6

Author(s):

Dina Dedic ◽

Teresia Sandberg ◽

Tommy Iversen ◽

Tomas Larsson ◽

Monica Ek

Keyword(s):

Oxidative Degradation ◽

Magic Angle Spinning ◽

Chemical Degradation ◽

Gas Chromatography Mass Spectrometry ◽

Magic Angle ◽

Chemical Mechanisms ◽

Wood Extracts ◽

Cellulose Depolymerization ◽

Angle Spinning ◽

C Nmr

Abstract The wood in the 17th century Swedish warship Vasa is weak. A depolymerization of the wood’s cellulose has been linked to the weakening, but the chemical mechanisms are yet unclear. The objective of this study was to analyze the lignin and tannin moieties of the wood to clarify whether the depolymerization of cellulose via ongoing oxidative mechanisms is indeed the main reason for weakening the wood in the Vasa. Lignin was analyzed by solid-state nuclear magnetic resonance [cross-polarization/magic-angle spinning (CP/MAS) 13C NMR] and by means of wet chemical degradation (thioacidolysis) followed by gas chromatography-mass spectrometry (GC-MS) of the products. No differences could be observed between the Vasa samples and the reference samples that could have been ascribed to extensive lignin degradation. Wood extracts (tannins) were analyzed by matrix-assisted laser desorption ionization (MALDI) combined with time-of-flight (TOF) MS and 13C NMR spectroscopy. The wood of the Vasa contained no discernible amounts of tannins, whereas still-waterlogged Vasa wood contained ellagic acid and traces of castalagin/vescalagin and grandinin. The results indicate that the condition of lignin in the Vasa wood is similar to fresh oak and that potentially harmful tannins are not present in high amounts. Thus, oxidative degradation mechanisms are not supported as a primary route to cellulose depolymerization.

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Comparisons of lipid dynamics and packing in fully interdigitated monoarachidoylphosphatidylcholine and non-interdigitated dipalmitoylphosphatidylcholine bilayers: cross polarization/magic angle spinning 13+C-NMR studies

Biochimica et Biophysica Acta (BBA) - Biomembranes ◽

10.1016/0005-2736(90)90068-y ◽

1990 ◽

Vol 1026 (2) ◽

pp. 225-235 ◽

Cited By ~ 21

Author(s):

Wen-guey Wu ◽

Lang-Ming Chi

Keyword(s):

Magic Angle Spinning ◽

Magic Angle ◽

Cross Polarization ◽

Nmr Studies ◽

Lipid Dynamics ◽

Angle Spinning ◽

C Nmr

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Azo pigments and their intermediates. A reinvestigation of the tetrazotization of 1,4-diaminoanthraquinone

Canadian Journal of Chemistry ◽

10.1139/v91-176 ◽

1991 ◽

Vol 69 (8) ◽

pp. 1183-1188 ◽

Cited By ~ 3

Author(s):

Kock-Yee Law ◽

Ihor W. Tarnawskyj ◽

Samuel Kaplan

Keyword(s):

Acetic Acid ◽

Acetic Acid Solution ◽

Magic Angle Spinning ◽

Magic Angle ◽

Cross Polarization ◽

Fluoboric Acid ◽

Angle Spinning ◽

C Nmr ◽

Nitrosylsulfuric Acid ◽

Brown Precipitate

The azotization of 1,4-diaminoanthraquinone (1) by n-amyl nitrite in glacial acetic was reinvestigated. The structure of a red-brown precipitate, which was previously identified as anthraquinone-1,4-tetrazonium dichloride (3) by Schaarschmidt, was found to be incorrect. In this work, we have identified the red-brown solid as 4-aminoanthraquinone-1-diazonium chloride (2), a diazotized product of 1. The yield of 2 was 80%. The tetrazonium dichloride 3 was actually formed in minute quantity and is soluble in acetic acid. The tetrazonium product of 1 can be isolated as tetrafluoroborate salt 4 in 3.4% yield by adding fluoboric acid into the acetic acid solution. The structure 4 was confirmed by IR and cross-polarization magic angle spinning13C NMR spectroscopy. Further investigations showed that 1 can be quantitatively tetrazotized by nitrosylsulfuric acid in 78% sulfuric acid. The tetrazonium product was isolated as 4 in 74% yield. Key words: 1,4-diaminoanthraquinone, diazotization, tetrazotization, azo pigments.

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13C CP/MAS nuclear magnetic resonance of crystalline methylxylopyranosides

Canadian Journal of Chemistry ◽

10.1139/v85-044 ◽

1985 ◽

Vol 63 (1) ◽

pp. 270-273 ◽

Cited By ~ 10

Author(s):

Michael G. Taylor ◽

Robert H. Marchessault ◽

Serge Perez ◽

Peter J. Stephenson ◽

Colin A. Fyfe

Keyword(s):

Nuclear Magnetic Resonance ◽

Magnetic Resonance ◽

Nmr Spectra ◽

Magic Angle Spinning ◽

Magic Angle ◽

Cross Polarization ◽

Asymmetric Unit ◽

Angle Spinning ◽

Detailed Nature ◽

C Nmr

The 13C nmr spectra of solids, acquired using the Cross Polarization/Magic Angle Spinning (CP/MAS) technique, are very sensitive to the detailed nature of crystalline packing. These effects are illustrated in the CP/MAS spectra of the α and β anomers of methyl-D-xylopyranoside. In the spectrum of the α anomer, which crystallizes with two molecules per unit cell, individual spectra can be resolved for the two molecules in the asymmetric unit of this crystal.

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