WorldWideScience

Sample records for residual lignin determination

  1. Lignin biochemistry and soil N determine crop residue decomposition and soil priming

    Science.gov (United States)

    Cropping history can affect soil properties, including available N, but little is known about the interactive effects of residue biochemistry, temperature and cropping history on residue decomposition. A laboratory incubation examined the role of residue biochemistry and temperature on the decomposi...

  2. Treatment of Lignin and Waste residues by Flash Pyrolysis

    DEFF Research Database (Denmark)

    Jensen, Peter Arendt; Trinh, Ngoc Trung; Dam-Johansen, Kim

    pyrolysis properties were compared with the pyrolysis properti es of wood and straw. The PCR treatment of sewage sludge provides an oil that can be used for energy pur poses and a solid residue rich in in organic nutrients that may be used as fertilizer product. By fast pyroly sis of lignin from the IBUS...... ethanol plant a bio-oil can be produced with oil yields of 36% (daf) and an oil en ergy recovery of 45%. This is a relatively low bio-oil yield compared to other feedstock’s, however, it may increase the value of the lignin residual product, such that the lignin char is used for combustion on the ethanol...... be operated at low rotational speed was constructed. The new rotor systems should make it easier to make an up-scaling of the process....

  3. Evaluating Lignin-Rich Residues from Biochemical Ethanol Production of Wheat Straw and Olive Tree Pruning by FTIR and 2D-NMR

    Directory of Open Access Journals (Sweden)

    José I. Santos

    2015-01-01

    Full Text Available Lignin-rich residues from the cellulose-based industry are traditionally incinerated for internal energy use. The future biorefineries that convert cellulosic biomass into biofuels will generate more lignin than necessary for internal energy use, and therefore value-added products from lignin could be produced. In this context, a good understanding of lignin is necessary prior to its valorization. The present study focused on the characterization of lignin-rich residues from biochemical ethanol production, including steam explosion, saccharification, and fermentation, of wheat straw and olive tree pruning. In addition to the composition and purity, the lignin structures (S/G ratio, interunit linkages were investigated by spectroscopy techniques such as FTIR and 2D-NMR. Together with the high lignin content, both residues contained significant amounts of carbohydrates, mainly glucose and protein. Wheat straw lignin showed a very low S/G ratio associated with p-hydroxycinnamates (p-coumarate and ferulate, whereas a strong predominance of S over G units was observed for olive tree pruning lignin. The main interunit linkages present in both lignins were β-O-4′ ethers followed by resinols and phenylcoumarans. These structural characteristics determine the use of these lignins in respect to their valorization.

  4. Isolation and characterization of lignin from the oak wood bioethanol production residue for adhesives.

    Science.gov (United States)

    Lee, Soo Jung; Kim, Hyun Joo; Cho, Eun Jin; Song, Younho; Bae, Hyeun-Jong

    2015-01-01

    Lignin was isolated from the residue of bioethanol production with oak wood via alkaline and catalyzed organosolv treatments at ambient temperature to improve the purity of lignin for the materials application. The isolated lignins were analyzed for their chemical composition by nitrobenzene oxidation method and their functionality was characterized via wet chemistry method, element analysis, (1)H NMR, GPC and FTIR-ATR. The isolated lignin by acid catalyzed organosolv treatment (Acid-OSL) contained a higher lignin content, aromatic proton, phenolic hydroxyl group and a lower nitrogen content that is more reactive towards chemical modification. The lignin-based adhesives were prepared and the bond strength was measured to evaluate the enhanced reactivity of lignin by the isolation. Two steps of phenolation and methylolation were applied for the modification of the isolated lignins and their tensile strengths were evaluated for the use as an adhesive. The acid catalyzed organosolv lignin-based adhesives had comparable bond strength to phenol-formaldehyde adhesives. The analysis of lignin-based adhesives by FTIR-ATR and TGA showed structural similarity to phenol adhesive. The results demonstrate that the reactivity of lignin was enhanced by isolation from hardwood bioethanol production residues at ambient temperature and it could be used in a value-added application to produce lignin-based adhesives. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Separation and characterisation of sulphur-free lignin from different agricultural residues

    NARCIS (Netherlands)

    Rossberg, Christine; Bremer, Martina; Machill, Susanne; Koenig, Swetlana; Kerns, Gerhard; Boeriu, Carmen; Windeisen, Elisabeth; Fischer, Steffen

    2015-01-01

    Wheat straw, as one of the most abundant agricultural residues in Europe, was subjected to alkaline pulping, microwave-assisted alkaline pulping and organosolv pulping using formic acid and hydrogen peroxide. The obtained lignins were characterised by means of Klason-lignin, FT-IR spectroscopy,

  6. The distribution of lignin in white birch wood as determined by bromination with TEM-EDXA

    International Nuclear Information System (INIS)

    Saka, S.; Goring, D.A.I.

    1988-01-01

    Ultraviolet absorbance and bromine uptake were measured on various morphological regions of birch wood. To facilitate precise comparison, observations were made on identical locations in successive cross sections. From the data, the concentration of lignin and the ratio of the guaiacyl to syringyl residues were determined. The results obtained were then compared with the previous findings from the use of UV microscopy alone

  7. Assessment of Antioxidant and Antimicrobial Properties of Lignin from Corn Stover Residue Pretreated with Low-Moisture Anhydrous Ammonia and Enzymatic Hydrolysis Process.

    Science.gov (United States)

    Guo, Mingming; Jin, Tony; Nghiem, Nhuan P; Fan, Xuetong; Qi, Phoebe X; Jang, Chan Ho; Shao, Lingxiao; Wu, Changqing

    2018-01-01

    Lignin accounts for 15-35% of dry biomass materials. Therefore, developing value-added co-products from lignin residues is increasingly important to improve the economic viability of biofuel production from biomass resources. The main objective of this work was to study the lignin extracts from corn stover residue obtained from a new and improved process for bioethanol production. Extraction conditions that favored high lignin yield were optimized, and antioxidant and antimicrobial activities of the resulting lignin were investigated. Potential estrogenic toxicity of lignin extracts was also evaluated. The corn stover was pretreated by low-moisture anhydrous ammonia (LMAA) and then subjected to enzymatic hydrolysis using cellulase and hemicellulase. The residues were then added with sodium hydroxide and extracted for different temperatures and times for enhancing lignin yield and the bioactivities. The optimal extraction conditions using 4% (w/v) sodium hydroxide were determined to be 50 °C, 120 min, and 1:8 (w:v), the ratio between corn stover solids and extracting liquid. Under the optimal condition, 33.92 g of lignin yield per 100 g of corn stover residue was obtained. Furthermore, the extracts produced using these conditions showed the highest antioxidant activity by the hydrophilic oxygen radical absorbance capacity (ORAC) assay. The extracts also displayed significant antimicrobial activities against Listeria innocua. Minimal estrogenic impacts were observed for all lignin extracts when tested using the MCF-7 cell proliferation assay. Thus, the lignin extracts could be used for antioxidant and antimicrobial applications, and improve the value of the co-products from the biomass-based biorefinery.

  8. Evaluation of electricity generation from lignin residue and biogas in cellulosic ethanol production.

    Science.gov (United States)

    Liu, Gang; Bao, Jie

    2017-11-01

    This study takes the first insight on the rigorous evaluation of electricity generation based on the experimentally measured higher heating value (HHV) of lignin residue, as well as the chemical oxygen demand (COD) and biological oxygen demand (BOD 5 ) of wastewater. For producing one metric ton of ethanol fuel from five typical lignocellulose substrates, including corn stover, wheat straw, rice straw, sugarcane bagasse and poplar sawdust, 1.26-1.85tons of dry lignin residue is generated from biorefining process and 0.19-0.27tons of biogas is generated from anaerobic digestion of wastewater, equivalent to 4335-5981kWh and 1946-2795kWh of electricity by combustion of the generated lignin residue and biogas, respectively. The electricity generation not only sufficiently meets the electricity needs of process requirement, but also generates more than half of electricity surplus selling to the grid. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Characterisation of Authentic Lignin Biorefinery Samples by Fourier Transform Infrared Spectroscopy and Determination of the Chemical Formula for Lignin

    DEFF Research Database (Denmark)

    Le, Duy Michael; Damgaard Nielsen, Anders; Sørensen, Hanne

    2017-01-01

    samples in situ with no prior purification and minimal sample preparation. Lignin chemical formulas and lignin Fourier transform infrared (FTIR) spectra were extracted from mixed spectra by filtering out signals from residual carbohydrates and minerals. From estimations of C, H and O and adjustment...... for cellulose and hemicelluloses contents, the average chemical formula of lignin was found to be C9H10.2O3.4 with slight variations depending on the biomass feedstock and processing conditions (between C9H9.5O2.8 and C9H11.1O3.6). Extracted FTIR lignin spectra showed many of the same characteristic peaks...... as organosolv and kraft lignin used as benchmark samples. Some variations in the lignin spectra of biorefinery lignin residue samples were found depending on biomass feedstock (wheat straw, corn stover or poplar) and on pretreatment severity, especially in the absorbance of bands at 1267 and 1032 cm−1 relative...

  10. Fate of Residual Lignin during Delignification of Kraft Pulp by Trametes versicolor

    Science.gov (United States)

    Reid, Ian D.

    1998-01-01

    The fungus Trametes versicolor can delignify and brighten kraft pulps. To better understand the mechanism of this biological bleaching and the by-products formed, I traced the transformation of pulp lignin during treatment with the fungus. Hardwood and softwood kraft pulps containing 14C-labelled residual lignin were prepared by laboratory pulping of lignin-labelled aspen and spruce wood and then incubated with T. versicolor. After initially polymerizing the lignin, the fungus depolymerized it to alkali-extractable forms and then to soluble forms. Most of the labelled carbon accumulated in the water-soluble pool. The extractable and soluble products were oligomeric; single-ring aromatic products were not detected. The mineralization of the lignin carbon to CO2 varied between experiments, up to 22% in the most vigorous cultures. The activities of the known enzymes laccase and manganese peroxidase did not account for all of the lignin degradation that took place in the T. versicolor cultures. This fungus may produce additional enzymes that could be useful in enzyme bleaching systems. PMID:9603823

  11. Litter decay rates are determined by lignin chemistry

    Science.gov (United States)

    Jennifer M. Talbot; Daniel J. Yelle; James Nowick; Kathleen K. Treseder

    2011-01-01

    Litter decay rates are often correlated with the initial lignin:N or lignin:cellulose content of litter, suggesting that interactions between lignin and more labile compounds are important controls over litter decomposition. The chemical composition of lignin may influence these interactions, if lignin physically or chemically protects labile components from microbial...

  12. Steam gasification of a thermally pretreated high lignin corn stover simultaneous saccharification and fermentation digester residue

    Energy Technology Data Exchange (ETDEWEB)

    Howe, Daniel T.; Taasevigen, Danny; Garcia-Perez, Manuel; McDonald, Armando G.; Li, Guosheng; Wolcott, Michael

    2017-01-01

    Efficient conversion of all components in lignocellulosic biomass is essential to realizing economic feasibility of biorefineries. However, when utilizing biochemical pathways, lignin cannot be fermented. Furthermore, the high lignin and high ash residue resulting from simultaneous saccharification and fermentation (SSF) reactors is difficult to thermochemically process due to feed line plugging and bed agglomeration. In this study a corn stover SSF digester residue was thermally pretreated at 300°C for 22.5 minutes (min) and then gasified in a bubbling fluidized bed gasifier to study the effect of thermal pretreatment on its processing behavior. Untreated, pelletized SSF residue was gasified at the same conditions to establish the baseline processing behavior. Results indicate that the thermal pretreatment process removes a substantial portion of the polar and non-polar extractives, with a resultant increase in the concentration of lignin, cellulose, and ash. Feed line plugging was not observed, although bed agglomeration was occurring at similar rates for both feedstocks, suggesting that overall ash content is the most important factor affecting bed agglomeration. Benzene, phenol, and polyaromatic hydrocarbons in the tar were present at higher concentrations in the treated material, with higher tar loading in the product gas. Total product gas generation is lower for the treated material, although the overall gas composition does not change.

  13. Determination of ethylenic residues in wood and TMP of spruce by FT-Raman spectroscopy

    Science.gov (United States)

    Umesh P. Agarwal; Sally A. Ralph

    2008-01-01

    A method based on FT-Raman spectroscopy is proposed for determining in situ concentrations of ethylenic residues in softwood lignin. Raman contributions at 1133 and 1654 cm-1, representing coniferaldehyde and coniferyl alcohol structures, respectively, were used in quantifying these units in spruce wood with subsequent conversion to concentrations in lignin. For...

  14. Rapid and accurate determination of the lignin content of lignocellulosic biomass by solid-state NMR.

    Science.gov (United States)

    Fu, Li; McCallum, Scott A; Miao, Jianjun; Hart, Courtney; Tudryn, Gregory J; Zhang, Fuming; Linhardt, Robert J

    2015-02-01

    Biofuels and biomaterials, produced from lignocellulosic feedstock, require facile access to cellulose and hemicellulose to be competitive with petroleum processing and sugar-based fermentation. Physical-chemical barriers resulting from lignin complicates the hydrolysis biomass into fermentable sugars. Thus, the amount of lignin within a substrate is critical in determining biomass processing. The application of 13 C cross-polarization, magic-angle spinning, and solid-state nuclear magnetic resonance for the direct quantification of lignin content in biomass is examined. Using a standard curve constructed from pristine lignin and cellulose, the lignin content of a biomass sample is accurately determined through direct measurement without chemical or enzymatic pre-treatment.

  15. Catalytic Hydrothermal Gasification of Lignin-Rich Biorefinery Residues and Algae Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Elliott, Douglas C.; Neuenschwander, Gary G.; Hart, Todd R.; Rotness, Leslie J.; Zacher, Alan H.; Santosa, Daniel M.; Valkenburt, Corinne; Jones, Susanne B.; Tjokro Rahardjo, Sandra A.

    2009-11-03

    This report describes the results of the work performed by PNNL using feedstock materials provided by the National Renewable Energy Laboratory, KL Energy and Lignol lignocellulosic ethanol pilot plants. Test results with algae feedstocks provided by Genifuel, which provided in-kind cost share to the project, are also included. The work conducted during this project involved developing and demonstrating on the bench-scale process technology at PNNL for catalytic hydrothermal gasification of lignin-rich biorefinery residues and algae. A technoeconomic assessment evaluated the use of the technology for energy recovery in a lignocellulosic ethanol plant.

  16. Microwave Assisted Hydrolysis of Holocellulose Catalyzed with Sulfonated Char Derived from Lignin-Rich Residue

    Directory of Open Access Journals (Sweden)

    Kui Wang

    2015-01-01

    Full Text Available A microwave assisted green process has been developed for production of sugars through liquefying holocellulose catalyzed with sulfonated char derived from the lignin-rich residue produced during pretreatment of lignocellulose. Various reaction parameters including the hydrolysis temperature, hydrolysis time, catalyst content, and the ratio of water to feedstock were evaluated. The maximum sugars yield of 82.6% (based on the dry mass of holocellulose was obtained under the optimum reaction conditions. The sulfonated char showed superior catalytic performance to that of dilute sulfuric acid in converting holocellulose into sugars under microwave irradiation.

  17. Benefits of weakening in thermogravimetric signals of hemicellulose and lignin for producing briquettes from soybean crop residue

    International Nuclear Information System (INIS)

    Gangil, Sandip

    2015-01-01

    Thermogravimetric signals of hemicellulose and lignin were found to subside due to the binderless briquetting of soybean crop residue. Minor but distinct thermogravimetric signals of secondary charring reactions were observed in raw crop residue and its briquetted biofuel. The bio-component related kinetics was evaluated using the Kissinger method. Activation energy level of intrinsic cellulosic biopolymer was found higher in briquette than that level in crop residue. The activation energy profile with respect to conversion fraction for raw residue and its briquette was analyzed by the Kissinger–Akahira–Sunose method. The activation energy profile of briquette was superior to raw residue of soybean crop showing the better thermal stability in briquetted biofuel, highlighting the benefits of briquetting process. In addition to the physico-chemical transformations occurred in lignin, the hemicellulose and cellulose related transitions were also expected to play positive role for briquetting. - Highlights: • Briquette of soybean-crop-residue showed weak TG-signals of hemicellulose & lignin. • Activation energy profile of briquette was superior to raw crop residues. • Thermal stability of different constituents due to briquetting was explained. • Hemicellulose and cellulose played positive role for briquetting along with lignin

  18. Coprocessing of fossil fuels with biomass Pt. 1. Vacuum residue with wood or lignin; Coprocessing von fossilen Rohstoffen mit Biomasse T. 1. Erdoelvakuumrueckstand mit Holz oder Lignin

    Energy Technology Data Exchange (ETDEWEB)

    Krey, F. [Technische Univ. Clausthal, Clausthal-Zellerfeld (Germany). Inst. fuer Technische Chemie; Oelert, H.H. [Technische Univ. Clausthal, Clausthal-Zellerfeld (Germany). Inst. fuer Technische Chemie

    1995-09-01

    The hydrogenation of vacuum residue with beechwood and eucalyptus lignin had been investigated. The experiments were done in an autoclav with 6 to 12 MPa hydrogen, at 380 to 440 C and a resistence time of 0 to 60 minutes. The results were evaluated over fractionation in several product fractions and over the analytical characterisation of some of these fractions. There was been found synergetic effects between the residue and the biomass. They result in higher yield of oils and in lower molecular weight of oils. The reasons can be found in the higher thermal sensibility of biomass which bonds are split at lower temperatures than the bonds of the vacuum residue. So the biomass builds radicals which act as initiator for the reactions of the vacuum residue. (orig.) [Deutsch] Es werden Untersuchungen zu der gemeinsamen hydrierenden Umsetzung von Erdoelvakuumrueckstand mit Buchenholz oder Eukalyptus-Lignin dargestellt. Die Versuche wurden in einem Autoklaven unter 6 bis 12 MPa Wasserstoffkaltdruck, bei 380 bis 440 C und 0 bis 60 Minuten Verweilzeit durchgefuehrt. Es findet eine Bewertung der Ergebnisse ueber die Trennung in verschiedene Produktfraktionen sowie ueber die analytische Charakterisierung einzelner Fraktionen statt. Es tritt eine synergistische Wechselwirkung zwischen dem Erdoelvakuumrueckstand und der Biomasse auf. Diese wirkt sich vor allem auf die oelfoermigen Produkte sowohl in ihrer Menge als auch in ihrer Charakterisierung aus. Die Wechselwirkung beruht vor allem auf der groesseren thermischen Empfindlichkeit der Biomasse, wodurch diese wie ein Initiator auf die Reaktionen des Vakuumrueckstandes wirkt und diesen zu verstaerkten Reaktionen anregt. (orig.)

  19. Pyrolysis characteristics and kinetics of lignin derived from enzymatic hydrolysis residue of bamboo pretreated with white-rot fungus.

    Science.gov (United States)

    Yan, Keliang; Liu, Fang; Chen, Qing; Ke, Ming; Huang, Xin; Hu, Weiyao; Zhou, Bo; Zhang, Xiaoyu; Yu, Hongbo

    2016-01-01

    The lignocellulose biorefinery based on the sugar platform usually focuses on polysaccharide bioconversion, while lignin is only burned for energy recovery. Pyrolysis can provide a novel route for the efficient utilization of residual lignin obtained from the enzymatic hydrolysis of lignocellulose. The pyrolysis characteristics of residual lignin are usually significantly affected by the pretreatment process because of structural alteration of lignin during pretreatment. In recent years, biological pretreatment using white-rot fungi has attracted extensive attention, but there are only few reports on thermal conversion of lignin derived from enzymatic hydrolysis residue (EHRL) of the bio-pretreated lignocellulose. Therefore, the study investigated the pyrolysis characteristics and kinetics of EHRL obtained from bamboo pretreated with Echinodontium taxodii in order to evaluate the potential of thermal conversion processes of EHRL. Fourier transform infrared spectroscopy spectra showed that EHRL of bamboo treated with E. taxodii had the typical lignin structure, but aromatic skeletal carbon and side chain of lignin were partially altered by the fungus. Thermogravimetric analysis indicated that EHRL pyrolysis at different heating rates could be divided into two depolymerization stages and covered a wide temperature range from 500 to 900 K. The thermal decomposition reaction can be well described by two third-order reactions. The kinetics study indicated that the EHRL of bamboo treated with white-rot fungus had lower apparent activation energies, lower peak temperatures of pyrolysis reaction, and higher char residue than the EHRL of raw bamboo. Pyrolysis-gas chromatography-mass spectrometry (Py-GC/MS) was applied to characterize the fast pyrolysis products of EHRL at 600 ℃. The ratios of guaiacyl-type to syringyl-type derivatives yield (G/S) and guaiacyl-type to p-hydroxy-phenylpropane-type derivatives yield (G/H) for the treated sample were increased by 33.18 and

  20. Understanding the Nonproductive Enzyme Adsorption and Physicochemical Properties of Residual Lignins in Moso Bamboo Pretreated with Sulfuric Acid and Kraft Pulping.

    Science.gov (United States)

    Huang, Caoxing; He, Juan; Min, Douyong; Lai, Chenhuan; Yong, Qiang

    2016-12-01

    In this work, to elucidate why the acid-pretreated bamboo shows disappointingly low enzymatic digestibility comparing to the alkali-pretreated bamboo, residual lignins in acid-pretreated and kraft pulped bamboo were isolated and analyzed by adsorption isotherm to evaluate their extents of nonproductive enzyme adsorption. Meanwhile, physicochemical properties of the isolated lignins were analyzed and a relationship was established with non-productive adsorption. Results showed that the adsorption affinity and binding strength of cellulase on acid-pretreated bamboo lignin (MWLa) was significantly higher than that on residual lignin in pulped bamboo (MWLp). The maximum adsorption capacity of cellulase on MWLp was 129.49 mg/g lignin, which was lower than that on MWLa (160.25 mg/g lignin). When isolated lignins were added into the Avicel hydrolysis solution, the inhibitory effect on enzymatic hydrolysis efficiency of MWLa was found to be considerably stronger than that with MWLp. The cellulase adsorption on isolated lignins was correlated positively with hydrophobicity, phenolic hydroxyl group, and degree of condensation but negatively with surface charges and aliphatic hydroxyl group. These results suggest that the higher nonproductive cellulase adsorption and physicochemical properties of residual lignin in acid-pretreated bamboo may be responsible for its disappointingly low enzymatic digestibility.

  1. Suitability of steam exploded residual softwood for the production of binderless panels. Effect of the pre-treatment severity and lignin addition

    Energy Technology Data Exchange (ETDEWEB)

    Angles, M.N.; Ferrando, F.; Farriol, X.; Salvado, J. [Universitat Rovira i Virgili, Tarragona (Spain). Escola Tecnica Superior d' Enginyeria

    2001-07-01

    A steam explosion pre-treatment was applied at various severities to softwood residual substrate to determine the most suitable pre-treatment for the manufacture of binderless panels. The effect of adding acid to the pre-treatment of fibres was also evaluated. The changes in the chemical composition and morphology of the original material were investigated by fractionation analyses and scanning electron micrographs. High severities caused defibrillation of the material allowing to build links to form the panels. Prehydrolysis with acid had a great effect of the structure of the material even at low acid concentration, The physical and mechanical properties of the panel improved with as the severity of the pre-treatment increased up to a point where mechanical properties deteriorated. The composites with highest internal bond had a high cellulose content and a medium lignin content, All these factors suggested that steamed pre-treated residual could be improved by adding a natural binder to produce the panels. A test of producing panels with addition of several kinds of lignin (up to 20%) was performed. With no significant changes in density, water stability (thickness swelling and water absorption) internal bond and mechanical properties were greatly improved., Results after accelerated ageing test were also enhanced. (Author)

  2. Polyoxometalate delignification of birch kraft pulp and effect on residual lignin

    Science.gov (United States)

    Biljana Bujanovic; Richard S. Reiner; Sally A. Ralph; Rajai H. Atalla

    2011-01-01

    To advance the understanding of delignification with polyoxometalates (POMs) that have been explored for use in bleaching of chemical pulps, the transformation of lignin during anaerobic treatment of birch kraft pulp with an equilibrated POM mixture composed of Na5(+2)[SiV1(-0.1)MoW10(+0.1)O

  3. Ultra violet resonance Raman spectroscopy in lignin analysis: determination of characteristic vibrations of p-hydroxyphenyl, guaiacyl, and syringyl lignin structures.

    Science.gov (United States)

    Saariaho, Anna-Maija; Jääskeläinen, Anna-Stiina; Nuopponen, Mari; Vuorinen, Tapani

    2003-01-01

    Raman spectroscopy of wood and lignin samples is preferably carried out in the near-infrared region because lignin produces an intense laser-induced fluorescence background at visible excitation wavelengths. However, excitation of aromatic and conjugated lignin structures with deep ultra violet (UV) light gives resonance-enhanced Raman signals while the overlapping fluorescence is eliminated. In this study, ultra violet resonance Raman (UVRR) spectroscopy was used to define characteristic vibration bands of model compounds of p-hydroxyphenyl, guaiacyl, and syringyl lignin structures at three excitation wavelengths (229, 244, and 257 nm). The intensities of each band, relative to the intensity of the aromatic vibration band at 1600 cm-1, were defined and the most suitable excitation wavelength was suggested for each structure. p-Hydroxyphenyl structures showed intensive characteristic bands at 1217-1214 and 1179-1167 cm-1 with excitation at 244 nm, whereas the bands of guaiacyl structures were more intensive with 257 nm excitation. Most intensive characteristic bands of guaiacyl structures were found at 1289-1279, 1187-1185, 1158-1155, and 791-704 cm-1. Syringyl structures had almost identical spectra with 244 and 257 nm excitations with characteristic bands at 1514-1506, 1333-1330, and 981-962 cm-1. The characteristic bands of the three structural units were also found from the compression wood, softwood, and hardwood samples, indicating that UVRR spectroscopy can be applied for the determination of chemical structures of lignin.

  4. Understanding the Nature and Reactivity of Residual Lignin for Improved Pulping and Bleaching Efficiency; FINAL

    International Nuclear Information System (INIS)

    Yuan-Zong Lai

    2001-01-01

    One of the most formidable challenges in kraft pulping to produce bleached chemical pulps is how to effectively remove the last 5-10% of lignin while maintaining the fiber quality. To avoid a severe fiber degradation, kraft pulping is usually terminated in the 25-30 kappa number range and then followed by an elementally chlorine free (ECF) or a totally chlorine free (TCF) bleaching sequence to reduce the environmental impacts

  5. Understanding the Nature and Reactivity of Residual Lignin for Improved Pulping and Bleaching Efficiency

    Energy Technology Data Exchange (ETDEWEB)

    Yuan-Zong Lai

    2001-11-30

    One of the most formidable challenges in kraft pulping to produce bleached chemical pulps is how to effectively remove the last 5-10% of lignin while maintaining the fiber quality. To avoid a severe fiber degradation, kraft pulping is usually terminated in the 25-30 kappa number range and then followed by an elementally chlorine free (ECF) or a totally chlorine free (TCF) bleaching sequence to reduce the environmental impacts.

  6. Biochemical stability of organic matter in soils amended with organic slow N-release fertilizer derived from charred plant residues and ammonoxidized lignin

    Science.gov (United States)

    Knicker, Heike; de la Rosa, José Maria; López Martín, María; Clemente Barragan, Reyes; Liebner, Falk

    2013-04-01

    As an important plant nutrient, N that has been removed from the soil by plant growth is replaced mainly by the use of synthetic fertilizers. Although this practice has dramatically increased food production, the unintended costs to the environment and human health due to surplus and inefficient application have also been substantial. Major losses of N to the environment can be minimized if "sustainable" agricultural practices are combined with reasonable fertilization. The latter can be achieved by applying slow N-release fertilizers. Here, the N is incorporated into an organic matrix, which after its amendment to soils, slowly decompose, allowing the liberation of the nutrient. Deriving from organic waste, such an amendment helps to efficiently recycle resources and increases the C sequestration potential of soils. However, in order to turn this approach into a successful strategy, the material has to be bioavailable but still sufficiently recalcitrant to ensure slow and controlled N-release. In the present study, we tested potential slow N-release fertilizers recycled from organic waste for their biochemical stability in soils. They comprised N-rich charred grass residues and N-lignin derived from waste of the pulp and paper industry and enriched in N by ammonoxidation. The substrates were mixed with soil of an Histic Humaquept and subsequently subjected to microbial degradation at 28°C in a Respicond IV Apparatus for 10 weeks. Additionally, soil material without organic amendment and soils mixed with lignin or charcoal both with and without KNO3 were included into the experiment. During the degradation experiment the CO2 production was determined on an hourly base. The degradation rate constants and the mean residence times were calculated using a double exponential decay model (pools with fast and slow turnover). Alterations of the chemical composition of the organic matter during degradation were studied by solid-state 13C NMR spectroscopy. First results

  7. Characterization and elimination of undesirable protein residues in plant cell walls for enhancing lignin analysis by solution-state 2D gel-NMR methods

    Science.gov (United States)

    Proteins exist in every plant cell wall. Certain protein residues interfere with lignin characterization and quantification. The current solution-state 2D-NMR technique (gel-NMR) for whole plant cell wall structural profiling provides detailed information regarding cell walls and proteins. However, ...

  8. Natural deep eutectic solvent mediated pretreatment of rice straw: bioanalytical characterization of lignin extract and enzymatic hydrolysis of pretreated biomass residue.

    Science.gov (United States)

    Kumar, Adepu K; Parikh, Bhumika S; Pravakar, Mohanty

    2016-05-01

    The present investigation demonstrated pretreatment of lignocellulosic biomass rice straw using natural deep eutectic solvents (NADESs), and separation of high-quality lignin and holocellulose in a single step. Qualitative analysis of the NADES extract showed that the extracted lignin was of high purity (>90 %), and quantitative analysis showed that nearly 60 ± 5 % (w/w) of total lignin was separated from the lignocellulosic biomass. Addition of 5.0 % (v/v) water during pretreatment significantly enhanced the total lignin extraction, and nearly 22 ± 3 % more lignin was released from the residual biomass into the NADES extract. X-ray diffraction studies of the untreated and pretreated rice straw biomass showed that the crystallinity index ratio was marginally decreased from 46.4 to 44.3 %, indicating subtle structural alterations in the crystalline and amorphous regions of the cellulosic fractions. Thermogravimetric analysis of the pretreated biomass residue revealed a slightly higher T dcp (295 °C) compared to the T dcp (285 °C) of untreated biomass. Among the tested NADES reagents, lactic acid/choline chloride at molar ratio of 5:1 extracted maximum lignin of 68 ± 4 mg g(-1) from the rice straw biomass, and subsequent enzymatic hydrolysis of the residual holocellulose enriched biomass showed maximum reducing sugars of 333 ± 11 mg g(-1) with a saccharification efficiency of 36.0 ± 3.2 % in 24 h at 10 % solids loading.

  9. Efeito do conteúdo e da natureza da lignina residual na eficiência e na seletividade do branqueamento com ozônio Effect of residual lignin content and nature on the efficiency and selectivity of ozone bleaching

    Directory of Open Access Journals (Sweden)

    Elenice Pereira Maia

    2003-04-01

    Full Text Available Neste estudo foram avaliados os efeitos do conteúdo e da natureza da lignina residual na eficiência e na seletividade do branqueamento com ozônio de polpa kraft convencional (kraft e pré-deslignificada com oxigênio (kraft-O. Constatou-se que a eficiência do branqueamento com ozônio se eleva com o aumento do conteúdo de lignina residual da polpa. O tratamento com ozônio é mais seletivo para polpas kraft-O, mas para um mesmo tipo de polpa a seletividade de branqueamento com ozônio se eleva com o aumento de lignina residual. A eficiência do branqueamento com ozônio aumenta com o teor de lignina fenólica na polpa, entretanto a seletividade é negativamente afetada pela presença destas estruturas.This study aimed to evaluate the effect of residual lignin content and nature on the efficiency and selectivity of ozone bleaching of conventional (kraft and oxygen delignified (kraft-O pulps. Ozone bleaching efficiency was found to be enhanced by increasing pulp residual lignin content. Ozone treatment is more selective for kraft-O pulps, but for a given type of pulp (kraft or kraft-O, ozone bleaching selectivity increases with increasing pulp lignin content. Ozone bleaching efficiency increases with increasing pulp lignin phenolic hydroxyl content whereas selectivity is negatively affected by these structures.

  10. Changes in lignin content of leaf litters during mulching.

    Science.gov (United States)

    Jin, Zhenfu; Akiyama, Takuya; Chung, Byung Yeoup; Matsumoto, Yuji; Iiyama, Kenji; Watanabe, Satomi

    2003-11-01

    Alkaline nitrobenzene oxidation, ozonation and methoxyl content determinations were applied to decomposing leaf litter of Ginkgo biloba L., Cinnamomum camphora sieb., Zelkova serrata Makino and Firmiana simplex W. F. Wight, respectively, during mulching to investigate the properties and estimate changes in lignin composition and content. Since the Klason lignin residue originated from components highly resistant to degradation by acid, the methoxyl content of Klason residue was used to estimate the lignin content of leaf litter. Quantitative analysis of presumed lignin-derived fragments, by use of alkaline nitrobenzene oxidation and ozonation methods, suggested that the estimated lignin content approximates that of the real lignin content of leaves, which is greatly overestimated by the Klason procedure. The estimated lignin contents ranged from 3.9 to 10.0% while the Klason lignan residue varied from 37.1 to 46.7% in un-mulched leaf litter. The absolute amounts of the measured lignin somewhat decreased during mulching, while the structure of lignin remaining in leaf litters after mulching was considered not to be very different from its original structure.

  11. Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode

    OpenAIRE

    Amare, Meareg; Aklog, Senait

    2017-01-01

    Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6 ? 10?6 to 100 ? 10?6?mol?L?1 with determination coefficient and method detection limit (LoD = 3?s/slope) of 0....

  12. Facilitating the enzymatic saccharification of pulped bamboo residues by degrading the remained xylan and lignin-carbohydrates complexes.

    Science.gov (United States)

    Huang, Caoxing; He, Juan; Li, Xin; Min, Douyong; Yong, Qiang

    2015-09-01

    Kraft pulping was performed on bamboo residues and its impact on the chemical compositions and the enzymatic digestibility of the samples were investigated. To improve the digestibility of sample by degrading the xylan and lignin-carbohydrates complexes (LCCs), xylanase and α-L-arabinofuranosidase (AF) were supplemented with cellulase. The results showed more carbohydrates were remained in the samples pulped with low effective alkali (EA) charge, compared to conventional kraft pulping. When 120 IU/g xylanase and 15 IU/g AF were supplemented with 20 FPU/g cellulase, the xylan degradation yield of the sample pulped with 12% EA charge increased from 68.20% to 88.35%, resulting in an increased enzymatic saccharification efficiency from 58.98% to 83.23%. The amount of LCCs in this sample decreased from 8.63/100C9 to 2.99/100C9 after saccharification with these enzymes. The results indicated that degrading the remained xylan and LCCs in the pulp could improve its enzymatic digestibility. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Potential of lignin from Canna edulis ker residue in the inhibition of α-d-glucosidase: Kinetics and interaction mechanism merging with docking simulation.

    Science.gov (United States)

    Xie, Fan; Gong, Shengxiang; Zhang, Wei; Wu, Jinhong; Wang, Zhengwu

    2017-02-01

    In this study, we extracted lignin from Canna edulis ker residue. Its chemical structure, inhibitory activity on α-d-glucosidase, and kinetics as well as interaction mechanism were investigated by using spectrum analysis and docking simulation. The isolated lignin was composed by guaiacyl and syringal units, and exhibited stronger inhibition on α-d-glucosidase than acarbose with the half maximal inhibitory concentration at 5.3±0.3μM. It was a non-competitive inhibitior with K m and K i values of 0.53±0.02mM and 0.92±0.12μM, respectively. It could quench the intrinsic fluorescence of α-d-glucosidase through a static quenching mode. The calculated values of enthalpy and entropy change were 20.8±2.5kJmol -1 and 172.7±0.8Jmol -1 K -1 , respectively. There was a single binding site on α-d-glucosidase for lignin, and the binding distance was 3.2nm. The molecular docking analysis exhibited that the hydrogen bonds, hydropholic interaction, and van der Waals forces were the main forces for lignin bind to α-d-glucosidase. This work provides a new insight into the interaction between the lignin and α-d-glucosidase, which might be beneficial to type 2 diabetes with the application of lignin in functional food and pharmacy fields. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Solvent-free method for the determination of lignin-derived phenols in sediments.

    Science.gov (United States)

    Pinto, Mayara; Frena, Morgana; Dos Santos Madureira, Luiz Augusto

    2017-05-01

    A solvent-free method that uses headspace solid-phase microextraction and gas chromatography with flame ionization detection is proposed for the determination of lignin-derived phenols in sediments. The extraction and derivatization conditions for the simultaneous analysis of acetosyringone, acetovanillone, syringaldehyde, vanillin, ferulic acid, syringic acid, vanillic acid, p-hydroxybenzoic acid, and p-coumaric acid were optimized using a central composite design. After optimization, the best results were obtained with the following conditions: exposure of the polyacrylate fiber to the headspace with 60 μL of N,O-bis(trimethylsilyl)trifluoroacetamide as a derivatizing agent for 15 min and then extraction in the headspace of 100 mg of sediment (previously spiked with lignin-derived phenols) for 35 min. The accuracy of the method was estimated based on recovery tests at two concentration levels and by comparison with a high-performance liquid chromatography method reported in the literature. Based on the t-test with a confidence level of 95%, no statistical differences were observed. The detection and quantification limits for the target compounds varied according to their characteristics: values at the microgram per gram level for nonacid compounds and milligram per gram level for phenolic acids, due to the lower volatility of the derivatives. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Residual-strength determination in polymetric materials

    International Nuclear Information System (INIS)

    Christensen, R.M.

    1981-01-01

    Kinetic theory of crack growth is used to predict the residual strength of polymetric materials acted upon by a previous history. Specifically, the kinetic theory is used to characterize the state of growing damage that occurs under a constant-stress (load) state. The load is removed before failure under creep-rupture conditions, and the residual instantaneous strength is determined from the theory by taking account of the damage accumulation under the preceding constant-load history. The rate of change of residual strength is found to be strongest when the duration of the preceding load history is near the ultimate lifetime under that condition. Physical explanations for this effect are given, as are numerical examples. Also, the theoretical prediction is compared with experimental data

  16. Lignin Sulfonation - A different Approach

    DEFF Research Database (Denmark)

    Bjørkmann, Anders

    2001-01-01

    . It was found that lignin is very reactive, that is why the sulfonation chemistry alone does not necessarily determine its dissolution rate. It became evident that the ultrastructure dispersion of lignin in wood is beneficial for its dissolution. For W, the rate was much higher at pH 1.5 than at 6. MW lignin...... and MWL dissolved (after extraction of the "immediate" lignin) at higher rates than W lignin. For MWL, the rate difference between pH 1.5 and 6 was moderate, compared to W lignin. Borohydride reduction did not affect the lignin dissolution from W, but gave a large decrease of sulfonation rate for MWL...

  17. Analysis of the relation between the cellulose, hemicellulose and lignin content and the thermal behavior of residual biomass from olive trees.

    Science.gov (United States)

    Garcia-Maraver, A; Salvachúa, D; Martínez, M J; Diaz, L F; Zamorano, M

    2013-11-01

    The heterogeneity of biomass makes it difficult if not impossible to make sweeping generalizations concerning thermochemical treatment systems and the optimal equipment to be used in them. Chemical differences in the structural components of the biomass (cellulose, hemicellulose, and lignin) have a direct impact on its chemical reactivity. The aim of this research was to study the influence of the organic components of the raw material from olive trees (leaves, pruning residues, and wood) in the combustion behavior of this biomass, as well as to find the component responsible for the higher ash content of olive leaves. Accordingly, the study used a thermogravimetric analyzer to monitor the different states and complex transitions that occurred in the biomass as the temperature varied. The decomposition rates of the different samples were analyzed in order to establish a link between each combustion phase and the composition of the raw materials. Two methods were used to determine the hemicellulose and cellulose contents of biomass from olive trees. Significant differences among the results obtained by the different methods were observed, as well as important variations regarding the chemical composition and consequently the thermal behavior of the raw materials tested. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Determination of maleic hydrazide residues in onion

    Directory of Open Access Journals (Sweden)

    Bursić Vojislava

    2010-01-01

    Full Text Available A simple HPLC determination method of maleic hydrazide residues in onions was introduced. The homogenized onion samples were extracted with methanol. The crude ex- tract was purified on SPE SampliQ SCX column. The maleic hydrazide was analyzed by HPLC with UV detection of 313 nm. The HPLC separation was performed on SynChropak Q column with 0.25 M phosphate buffer as the mobile phase. The recoveries of maleic hydrazide from the spiked onions with 1.5, 2.0, 3.0, 5.0, 7.0 and 10.0 mg ml-1, ranged from 89-103%. The detection limit of maleic hydrazide was 0.4 mg ml-1, and the quantification limit was 1.25 mg ml-1. The linearity coefficient was 0.9998. Such an optimized method was applied to the determination of residue content of maleic hydrazide in onions, treated with Royal MH-30 in the amount of 8.0 and 12.0 l ha-1. The samples were analysed after 8, 16 and 25 days from the moment of spraying. The obtained values of maleic hydrazide residues were below the maximum tolerable amount in the Republic of Serbia (10 mg kg-1, as well as the amount regulated by the EU (15 mg kg-1. .

  19. Isolation and Characterization of Gramineae and Fabaceae Soda Lignins

    Directory of Open Access Journals (Sweden)

    Juan Domínguez-Robles

    2017-02-01

    Full Text Available Some agricultural residues such as wheat or barley straw, as well as certain fast-growing plants like Leucaena leucocephala and Chamaecytisus proliferus, could be used as raw materials for the paper industry as an alternative to traditional plants (eucalyptus, pine, etc.. In the present study, four types of lignin obtained from the spent liquors produced by the pulping processes using the abovementioned feedstocks were isolated and characterized. Lignin samples were acquired through an acid precipitation from these spent liquors. The characterization of the precipitated lignin samples were performed using a Fourier transform infrared spectroscopy (FT-IR and both liquid- and solid-state nuclear magnetic resonance spectroscopy (NMR to analyse the chemical structure, and thermogravimetric analysis (TGA for determining the thermal properties. Additionally, chemical composition of lignin fractions was also measured. Even though they were of different botanical origin, all the studied samples except for wheat straw lignin had a similar chemical composition and thermal behaviour, and identical chemical structure. Wheat straw lignin showed a greater amount of Klason lignin and lower carbohydrate content. Furthermore, this lignin sample showed a higher thermal stability and significantly different cross-peak patterns in the 2D-NMR experiments. The molecular structures corresponding to p-coumarate (PCA, ferulate (FA and cinnamyl aldehyde end-groups (J were only detected in wheat isolated lignin.

  20. Isolation and Characterization of Gramineae and Fabaceae Soda Lignins

    Science.gov (United States)

    Domínguez-Robles, Juan; Sánchez, Rafael; Espinosa, Eduardo; Savy, Davide; Mazzei, Pierluigi; Piccolo, Alessandro; Rodríguez, Alejandro

    2017-01-01

    Some agricultural residues such as wheat or barley straw, as well as certain fast-growing plants like Leucaena leucocephala and Chamaecytisus proliferus, could be used as raw materials for the paper industry as an alternative to traditional plants (eucalyptus, pine, etc.). In the present study, four types of lignin obtained from the spent liquors produced by the pulping processes using the abovementioned feedstocks were isolated and characterized. Lignin samples were acquired through an acid precipitation from these spent liquors. The characterization of the precipitated lignin samples were performed using a Fourier transform infrared spectroscopy (FT-IR) and both liquid- and solid-state nuclear magnetic resonance spectroscopy (NMR) to analyse the chemical structure, and thermogravimetric analysis (TGA) for determining the thermal properties. Additionally, chemical composition of lignin fractions was also measured. Even though they were of different botanical origin, all the studied samples except for wheat straw lignin had a similar chemical composition and thermal behaviour, and identical chemical structure. Wheat straw lignin showed a greater amount of Klason lignin and lower carbohydrate content. Furthermore, this lignin sample showed a higher thermal stability and significantly different cross-peak patterns in the 2D-NMR experiments. The molecular structures corresponding to p-coumarate (PCA), ferulate (FA) and cinnamyl aldehyde end-groups (J) were only detected in wheat isolated lignin. PMID:28165411

  1. Electrochemical Determination of Caffeine Content in Ethiopian Coffee Samples Using Lignin Modified Glassy Carbon Electrode

    Directory of Open Access Journals (Sweden)

    Meareg Amare

    2017-01-01

    Full Text Available Lignin film was deposited at the surface of glassy carbon electrode potentiostatically. In contrast to the unmodified glassy carbon electrode, an oxidative peak with an improved current and overpotential for caffeine at modified electrode showed catalytic activity of the modifier towards oxidation of caffeine. Linear dependence of peak current on caffeine concentration in the range 6×10-6 to 100×10-6 mol L−1 with determination coefficient and method detection limit (LoD = 3 s/slope of 0.99925 and 8.37×10-7 mol L−1, respectively, supplemented by recovery results of 93.79–102.17% validated the developed method. An attempt was made to determine the caffeine content of aqueous coffee extracts of Ethiopian coffees grown in four coffee cultivating localities (Wonbera, Wolega, Finoteselam, and Zegie and hence to evaluate the correlation between users preference and caffeine content. In agreement with reported works, caffeine contents (w/w% of 0.164 in Wonbera coffee; 0.134 in Wolega coffee; 0.097 in Finoteselam coffee; and 0.089 in Zegie coffee were detected confirming the applicability of the developed method for determination of caffeine in a complex matrix environment. The result indicated that users’ highest preference for Wonbera and least preference for Zegie cultivated coffees are in agreement with the caffeine content.

  2. Calculated ionisation potentials to determine the oxidation of vanillin precursors by lignin peroxidase.

    NARCIS (Netherlands)

    Have, ten R.; Rietjens, I.M.C.M.; Hartmans, S.; Swarts, H.J.; Field, J.A.

    1998-01-01

    In view of the biocatalytic production of vanillin, this research focused on the lignin peroxidase (LiP) catalysed oxidation of naturally occurring phenolic derivatives: O-methyl ethers, O-acetyl esters, and O-glucosyl ethers. The ionisation potential (IP) of a series of model compounds was

  3. Relationship between lignin structure and delignification degree in Pinus pinaster kraft pulps.

    Science.gov (United States)

    Baptista, C; Robert, D; Duarte, A P

    2008-05-01

    This study examines the structure of residual and dissolved lignins from Pinus pinaster pulps obtained at different degrees of delignification by laboratory conventional kraft pulping. The cooking H factor was varied from 85 to 8049. The residual and dissolved lignin samples were characterised by elemental analysis, residual carbohydrate content, permanganate oxidation and 13C NMR spectroscopy. The reflectance factor of the pulps was also determined in order to tentatively correlate the delignification degree and residual lignin structure with the pulp colour. The obtained results confirmed that the delignification degree increases the condensation of the lignin structure, which might have an influence upon the observed increased pulp colour. The lack of selectivity of kraft pulping process in the case of more delignified pulps was also shown.

  4. Determination of Pesticide Residues in Cannabis Smoke

    Directory of Open Access Journals (Sweden)

    Nicholas Sullivan

    2013-01-01

    Full Text Available The present study was conducted in order to quantify to what extent cannabis consumers may be exposed to pesticide and other chemical residues through inhaled mainstream cannabis smoke. Three different smoking devices were evaluated in order to provide a generalized data set representative of pesticide exposures possible for medical cannabis users. Three different pesticides, bifenthrin, diazinon, and permethrin, along with the plant growth regulator paclobutrazol, which are readily available to cultivators in commercial products, were investigated in the experiment. Smoke generated from the smoking devices was condensed in tandem chilled gas traps and analyzed with gas chromatography-mass spectrometry (GC-MS. Recoveries of residues were as high as 69.5% depending on the device used and the component investigated, suggesting that the potential of pesticide and chemical residue exposures to cannabis users is substantial and may pose a significant toxicological threat in the absence of adequate regulatory frameworks.

  5. Lignin Macromolecule

    Indian Academy of Sciences (India)

    organisrn,s. The lignin ... constituent of wood which must be removed for making good quality paper! lignin. Softwood species have a .... by lowering the pH of the liquor to 2.5 - 3.0 by a suitable mineral acid. This precipitated compound is then ...

  6. Method for the determination of lignin content of a sample by flash pyrolysis in an atmosphere of hydrogen or helium and method therefor

    Science.gov (United States)

    Shakkottai, Parthasarathy (Inventor); Kwack, Eug Y. (Inventor); Lawson, Daniel D. (Inventor)

    1991-01-01

    The lignin content of wood, paper pulp or other material containing lignin (such as filter paper soaked in black liquor) is more readily determined by flash pyrolysis of the sample at approximately 550.degree. C. in a reducing atmosphere of hydrogen or in an inert atmosphere of helium followed by a rapid analysis of the product gas by a mass spectrometer. The heated pyrolysis unit as fabricated comprises a small platinum cup welded to an electrically-heated stainless steel ribbon with control means for programmed short duration (1.5 sec, approximately) heating and means for continuous flow of hydrogen or helium. The pyrolysis products enter an electron-ionization mode mass spectrometer for spectral evaluation. Lignin content is obtained from certain ratios of integrated ion currents of many mass spectral lines, the ratios being linearly related to the Kappa number of Klason lignin.

  7. Characterization of the lignin polymer in Brassicaceae family

    Directory of Open Access Journals (Sweden)

    S. Hemmati

    2017-04-01

    Full Text Available Background and objectives: Residues of medicinal plants after extraction and weeds are suitable candidates for bioethanol production. Significant barriers exist to make the conversion of lignocellulosic feedstock to biofuel cost effective and environmentally friendly; one of which is the lignin polymer. Brassicaceae family is one of the potential targets for biofuel production. The structural characteristics of lignin from Hirschfeldia incana, Sisymbrium altissimum and Cardaria draba were studied in comparison to that of Brassica napus. Methods: Lignin deposition was observed by phloroglucinol and Mäule staining. The total lignin content was determined by Klason method. Maximum UV absorbance and FT-IR spectra were compared. Ratio of syringyl to guaiacyl lignin (S/G ratio as a metric of lignin digestibility was determined by DFRC followed by GC-MS analysis. 1H-NMR spectra of the total lignin was compared with other spectroscopic methods. Results: Staining of thestem cross sections of C. draba showed higher G units in contrast to the higher S units in S. altissimum which was in agreement with 1H-NMR analysis. Total lignin content for H. incana, C. draba and S. altissimum was 27.10%, 23.8% and 24.5%, respectively. The specific maximum UV absorbance appeared between 230-260 nm. FT-IR analysis confirmed the presence of more aromatic structures in the seed maturation stage than the flowering stage. S/G ratio was 0.26, 0.10 and 0.22 for H. incana, C. draba and S. altissimum, respectively.  Conclusion: Except Cardaria draba with the predominance of G subunits in lignin polymer, Hirschfeldia incana and Sisymbrium altissimum are suitable candidates for bioethanol production.

  8. Calculated ionisation potentials to determine the oxidation of vanillin precursors by lignin peroxidase.

    OpenAIRE

    Have, ten, R.; Rietjens, I.M.C.M.; Hartmans, S.; Swarts, H.J.; Field, J.A.

    1998-01-01

    In view of the biocatalytic production of vanillin, this research focused on the lignin peroxidase (LiP) catalysed oxidation of naturally occurring phenolic derivatives: O-methyl ethers, O-acetyl esters, and O-glucosyl ethers. The ionisation potential (IP) of a series of model compounds was calculated and compared to their experimental conversion by LiP, defining a relative IP threshold of approximately 9.0 eV. Based on this threshold value only the O-acetyl esters and glucosides of isoeugeno...

  9. Calculated ionisation potentials determine the oxidation of vanillin precursors by lignin peroxidase.

    Science.gov (United States)

    ten Have, R; Rietjens, I M; Hartmans, S; Swarts, H J; Field, J A

    1998-07-03

    In view of the biocatalytic production of vanillin, this research focused on the lignin peroxidase (LiP) catalysed oxidation of naturally occurring phenolic derivatives: O-methyl ethers, O-acetyl esters, and O-glucosyl ethers. The ionisation potential (IP) of a series of model compounds was calculated and compared to their experimental conversion by LiP, defining a relative IP threshold of approximately 9.0 eV. Based on this threshold value only the O-acetyl esters and glucosides of isoeugenol and coniferyl alcohol would be potential LiP substrates. Both O-acetyl esters were tested and were shown to be converted to O-acetyl vanillin in molar yields of 51.8 and 2.3%, respectively.

  10. Assessment of antioxidant and antimicrobial properties of lignin from corn stover residue pretreated with low-moisture anhydrous ammonia and enzymatic hydrolysis process

    Science.gov (United States)

    To improve the economic viability of biofuel production from biomass resources, it is increasingly important to develop value-added lignin co-products from this process. The main objective of this study was to investigate the antimicrobial and antioxidant activities of the lignin extracts obtained b...

  11. Effect of Rice Straw Extract and Alkali Lignin on the Corrosion Inhibition of Carbon Steel

    International Nuclear Information System (INIS)

    Rabiahtul Zulkafli; Norinsan Kamil Othman; Irman Abdul Rahman; Azman Jalar

    2014-01-01

    A paddy residue based corrosion inhibitor was prepared by treating finely powdered rice straw with aqueous ethanol under acid catalyst (0.01 M H 2 SO 4 ). Commercial alkali lignin was obtained from Sigma-Aldrich. Prior to the corrosion test, the extraction yield and alkali lignin was characterized via FTIR to determine the functional group. The effect of paddy residue extract and commercial alkali lignin on the corrosion inhibition of carbon steel in 1 M HCl was investigated through the weight loss method, potentiodynamic polarization technique and scanning electron microscopy (SEM). The corrosion inhibition efficiency of the extract and alkali lignin at different immersion times (3 h, 24 h and 42 h) was evaluated. The results show that the paddy waste extract exhibited lesser weight loss of carbon steel in the acidic medium in comparison to the commercial alkali lignin, suggesting that the paddy residue extract is more effective than the commercial alkali lignin in terms of its corrosion inhibition properties. The results obtained proves that the extract from paddy residue could serve as an effective inhibitor for carbon steel in acidic mediums. (author)

  12. Cytocompatible cellulose hydrogels containing trace lignin

    Energy Technology Data Exchange (ETDEWEB)

    Nakasone, Kazuki; Kobayashi, Takaomi, E-mail: takaomi@nagaoakut.ac.jp

    2016-07-01

    Sugarcane bagasse was used as a cellulose resource to prepare transparent and flexible cellulose hydrogel films. On the purification process from bagasse to cellulose, the effect of lignin residues in the cellulose was examined for the properties and cytocompatibility of the resultant hydrogel films. The cellulose was dissolved in lithium chloride/N,N-dimethylacetamide solution and converted to hydrogel films by phase inversion. In the purification process, sodium hydroxide (NaOH) treatment time was changed from 1 to 12 h. This resulted in cellulose hydrogel films having small amounts of lignin from 1.62 to 0.68%. The remaining lignin greatly affected hydrogel properties. Water content of the hydrogel films was increased from 1153 to 1525% with a decrease of lignin content. Moreover, lower lignin content caused weakening of tensile strength from 0.80 to 0.43 N/mm{sup 2} and elongation from 45.2 to 26.5%. Also, similar tendency was observed in viscoelastic behavior of the cellulose hydrogel films. Evidence was shown that the lignin residue was effective for the high strength of the hydrogel films. In addition, scanning probe microscopy in the morphological observation was suggested that the trace lignin in the cellulose hydrogel affected the cellulose fiber aggregation in the hydrogel network. The trace of lignin in the hydrogels also influenced fibroblast cell culture on the hydrogel films. The hydrogel film containing 1.68% lignin showed better fibroblast compatibility as compared to cell culture polystyrene dish used as reference. - Highlights: • Cellulose hydrogel films with trace lignin were obtained from sugarcane bagasse. • Lignin content was found to be in the range of 1.62 − 0.68% by UV–Vis spectroscopy. • Higher lignin content strengthened mechanical properties of the hydrogel films. • Trace lignin affected the hydrogel morphology such as roughness and porosity. • High cell proliferation was observed in the hydrogel containing 1.68% lignin.

  13. Characterization of lignin-rich residues remaining after continuous super-critical water hydrolysis of poplar wood (Populus albaglandulosa) for conversion to fermentable sugars.

    Science.gov (United States)

    Moon, Sun-Joo; Eom, In-Yong; Kim, Jae-Young; Kim, Tae-Seung; Lee, Soo Min; Choi, In-Gyu; Choi, Joon Weon

    2011-05-01

    Poplar wood flour (Populous albaglandulosa) was treated with sub- and super-critical water (subcritical: 325, 350°C; super-critical: 380, 400, 425°C) for 60s at 220 ± 10 atm. Hydrochloric acid (0.05%v/v) was added to samples as acidic catalyst. The final products were separated into water soluble fraction and undegraded solids. The yields of undegraded solids were thoroughly dependent on temperature severity and mainly composed of lignin fragments. Average molecular weights of the lignins were between 1500 and 4400 Da, which was only 1/3-1/8-fold of poplar milled wood lignin (13,250 Da). DFRC (Derivatization Followed by Reductive Cleavage) analysis revealed that C6C3 phenols (coniferyl and sinapyl alcohol) were rarely detected in the lignins, indicating occurrence of two probable lignin reactions during SCW hydrolysis: lignin fragmentation via splitting of β-O-4 linkage and loss of propane side chains. These results were also confirmed by (1)H and (13)C NMR spectroscopic analysis. Copyright © 2011 Elsevier Ltd. All rights reserved.

  14. Nondestructive determination of residual stresses by neutron diffraction

    International Nuclear Information System (INIS)

    Tello, H.; Barrera, E.V.

    1993-01-01

    Nondestructive determination of residual stresses and strains in engineering materials has been limited to analytical models and near-surface measurement techniques such as x-ray diffraction and ultrasonic testing. The use of neutron diffraction for residual stress determination is similar in methodology to x-ray diffraction but provides superior analysis capability because of the lower absorption of neutrons in most materials. Neutron diffraction measurements can be made from sampling depths of several millimeters in most materials as compared to micrometer sampling depth of x-rays. This paper will discuss the principles of neutron diffraction as well as the advantages and limitations of the technique. Specific examples of residual stress measurements using conventional and time-of flight techniques will be provided

  15. Determination of dichlorvos residue levels in vegetables sold in ...

    African Journals Online (AJOL)

    To ensure maximum yield they apply various types of pesticides to control pests and diseases that attack these vegetables. Organophosphate pesticides are widely used in agriculture for the control of various insect pests mainly in developing countries. The purpose of the study was to determine the residual levels of the ...

  16. Combining specificity determining and conserved residues improves functional site prediction

    Directory of Open Access Journals (Sweden)

    Gelfand Mikhail S

    2009-06-01

    Full Text Available Abstract Background Predicting the location of functionally important sites from protein sequence and/or structure is a long-standing problem in computational biology. Most current approaches make use of sequence conservation, assuming that amino acid residues conserved within a protein family are most likely to be functionally important. Most often these approaches do not consider many residues that act to define specific sub-functions within a family, or they make no distinction between residues important for function and those more relevant for maintaining structure (e.g. in the hydrophobic core. Many protein families bind and/or act on a variety of ligands, meaning that conserved residues often only bind a common ligand sub-structure or perform general catalytic activities. Results Here we present a novel method for functional site prediction based on identification of conserved positions, as well as those responsible for determining ligand specificity. We define Specificity-Determining Positions (SDPs, as those occupied by conserved residues within sub-groups of proteins in a family having a common specificity, but differ between groups, and are thus likely to account for specific recognition events. We benchmark the approach on enzyme families of known 3D structure with bound substrates, and find that in nearly all families residues predicted by SDPsite are in contact with the bound substrate, and that the addition of SDPs significantly improves functional site prediction accuracy. We apply SDPsite to various families of proteins containing known three-dimensional structures, but lacking clear functional annotations, and discusse several illustrative examples. Conclusion The results suggest a better means to predict functional details for the thousands of protein structures determined prior to a clear understanding of molecular function.

  17. Diesel-soluble lignin oils and methods of their production

    DEFF Research Database (Denmark)

    2016-01-01

    Solvent consumption in supercritical ethanol, propanol or butanol treatment of either refined pre-extracted lignin or comparatively impure lignin-rich solid residual from hydrothermally pretreated lignocellulosic biomass can be minimized by conducting the reaction at very high loading of lignin...... to solvent. Comparatively impure, crude lignin- rich solid residual can be directly converted by supercritical alcohol treatment to significantly diesel-soluble lignin oil without requirement for pre-extraction or pre- solubilisation of lignin or for added reaction promoters such as catalysts, hydrogen donor...... co-solvents, acids, based or H2 gas. O:C ratio of product oil can readily be obtained using crude lignin residual in such a process at levels 0.20 or lower....

  18. Animal bioavailability of defined xenobiotic lignin metabolites

    International Nuclear Information System (INIS)

    Sandermann, H. Jr.; Arjmand, M.; Gennity, I.; Winkler, R.; Struble, C.B.; Aschbacher, P.W.

    1990-01-01

    Lignin has been recognized as a major component of bound pesticide residues in plants and is thought to be undigestible in animals. Two defined ring-U- 14 C-labeled chloroaniline/lignin metabolites have now been fed to rats, where a release of ∼66% of the bound xenobiotic occurred in the form of simple chloroaniline derivatives. The observed high degree of bioavailability indicates that bound pesticidal residues may possess ecotoxicological significance. In parallel studies, the white-rot fungus Phanerochaete chrysosporium was more efficient, and a soil system was much less efficient, in the degradation of the [ring-U- 14 C]chloroaniline/lignin metabolites

  19. The acetyl bromide method is faster, simpler and presents best recovery of lignin in different herbaceous tissues than Klason and thioglycolic acid methods.

    Science.gov (United States)

    Moreira-Vilar, Flavia Carolina; Siqueira-Soares, Rita de Cássia; Finger-Teixeira, Aline; de Oliveira, Dyoni Matias; Ferro, Ana Paula; da Rocha, George Jackson; Ferrarese, Maria de Lourdes L; dos Santos, Wanderley Dantas; Ferrarese-Filho, Osvaldo

    2014-01-01

    We compared the amount of lignin as determined by the three most traditional methods for lignin measurement in three tissues (sugarcane bagasse, soybean roots and soybean seed coat) contrasting for lignin amount and composition. Although all methods presented high reproducibility, major inconsistencies among them were found. The amount of lignin determined by thioglycolic acid method was severely lower than that provided by the other methods (up to 95%) in all tissues analyzed. Klason method was quite similar to acetyl bromide in tissues containing higher amounts of lignin, but presented lower recovery of lignin in the less lignified tissue. To investigate the causes of the inconsistencies observed, we determined the monomer composition of all plant materials, but found no correlation. We found that the low recovery of lignin presented by the thioglycolic acid method were due losses of lignin in the residues disposed throughout the procedures. The production of furfurals by acetyl bromide method does not explain the differences observed. The acetyl bromide method is the simplest and fastest among the methods evaluated presenting similar or best recovery of lignin in all the tissues assessed.

  20. Radiotracer experiments on lignin reactions, 2

    International Nuclear Information System (INIS)

    Terashima, Noritsugu; Araki, Hiroshi; Suganuma, Nobuo.

    1977-01-01

    The behavior of the specific carbon atoms of lignin during the cooking process was studied. Pine wood meal containing the protolignin labelled with 14-C was prepared, and treated under sulfate cooking conditions. The incorporation and distribution of radioactivity were traced in three fractions separated from the black liquor according to their solubilities and molecular weights. The gamma position carbon at the end of side chain of phenylpropane unit in lignin was eliminated easily from the high molecular weight portion in considerable extent during the cooking process, and a part of the eliminated carbon condenses again with the aromatic ring. However, a large portion of the eliminated gamma-carbon was found in the low molecular fraction of water soluble part of the black liquor. The radioactivity of alpha-carbons in the side chains adjacent to aromatic rings was found to be distributed in three fractions similarly to that of beta-carbons, except that the incorporation of radioactivity of alpha-carbons was slightly low in high molecular fraction, and slightly high in low molecular water soluble fraction as compared with that of beta-carbons and aromatic ring carbons. The number of residual carbon atoms per one monomer unit in high molecular kraft lignin was calculated from the specific incorporation ratio of radioactivity. The carbon skelton was estimated and the molecular formula was given by the elementary analysis and molecular weight determination. (Iwakiri, K.)

  1. Fractionation of hemp hurds by organosolv pretreatment and its effect on production of lignin and sugars.

    Science.gov (United States)

    Gandolfi, Stefano; Ottolina, Gianluca; Consonni, Roberto; Riva, Sergio; Patel, Ilabahen

    2014-07-01

    Fractionation of hemp hurds into its three main components, cellulose, hemicellulose, and lignin, was carried out using organosolv pretreatment. The effect of processing parameters, such as temperature, catalyst concentration, reaction time, and methanol (MeOH) concentration, on the dissolution and recovery of hemicellulose and lignin was determined. More than 75% of total hemicellulose and 75% of total lignin was removed in a single step with low amounts of degradation products under the following conditions: 165 °C, 3% H2 SO4 , 20 min reaction time, and 45% MeOH. Enzymatic hydrolysis of the residual pretreated biomass yielded up to 60% of cellulose-to-glucose conversion. The maximum recovery of the main components was obtained at a combined severity factor value of around one. Characterization of pretreated biomass and isolated lignin was carried out with FTIR and 2D (13) C-(1) H correlation HSQC NMR spectroscopy, the latter technique providing detailed structural information about the obtained methanol organosolv lignin (MOSL). Results suggested that xylopyranoside is the major carbohydrate associated with hemp lignin. The chemical properties of MOSL samples in terms of their phenolic group content and antioxidant capacity were also investigated. The results showed that MOSL samples have a high phenolic group content and antioxidant capacity relative to Klason lignin. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Maturation-related changes of carrot lignins.

    Science.gov (United States)

    Schäfer, Judith; Trierweiler, Bernhard; Bunzel, Mirko

    2018-02-01

    Lignified cell walls are important factors for textural and physiological properties of plant-based foods. However, carrot lignins and their modifications during maturation are poorly described. The objective of this study was to describe carrot lignins in detail and to study lignin structural alterations at later stages of maturity. Klason and acetyl bromide soluble lignin contents of insoluble fibers of carrots harvested at different times (26, 29 and 35 weeks after seeding) ranged between 46.38 and 62.68 g kg -1 and between 19.79 and 28.08 g kg -1 , respectively. As determined by both 2D-nuclear magnetic resonance and the derivatization followed by reductive cleavage method, coniferyl alcohol heavily dominated the traditional monolignol composition in carrot lignins, independently of harvest times. By using 2D-nuclear magnetic resonance experiments on isolated lignins, p-hydroxybenzoate was identified as a less common lignin constituent, attached to lignin γ-hydroxyl groups and being increasingly incorporated with maturation. β-Aryl ethers, phenylcoumaran, resinol and dibenzodioxocin structures were identified as lignin interunit linkages, largely independent of harvest times and with β-aryl ethers being expectedly dominant. Carrots contain guaiacyl-rich lignins that incorporate increasing amounts of p-hydroxybenzoate with maturation. All other lignin characteristics appear to be widely independent of harvest times. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

  3. Practical analysis of specificity-determining residues in protein families.

    Science.gov (United States)

    Chagoyen, Mónica; García-Martín, Juan A; Pazos, Florencio

    2016-03-01

    Determining the residues that are important for the molecular activity of a protein is a topic of broad interest in biomedicine and biotechnology. This knowledge can help understanding the protein's molecular mechanism as well as to fine-tune its natural function eventually with biotechnological or therapeutic implications. Some of the protein residues are essential for the function common to all members of a family of proteins, while others explain the particular specificities of certain subfamilies (like binding on different substrates or cofactors and distinct binding affinities). Owing to the difficulty in experimentally determining them, a number of computational methods were developed to detect these functional residues, generally known as 'specificity-determining positions' (or SDPs), from a collection of homologous protein sequences. These methods are mature enough for being routinely used by molecular biologists in directing experiments aimed at getting insight into the functional specificity of a family of proteins and eventually modifying it. In this review, we summarize some of the recent discoveries achieved through SDP computational identification in a number of relevant protein families, as well as the main approaches and software tools available to perform this type of analysis. © The Author 2015. Published by Oxford University Press. For Permissions, please email: journals.permissions@oup.com.

  4. Computational learning on specificity-determining residue-nucleotide interactions

    KAUST Repository

    Wong, Ka-Chun

    2015-11-02

    The protein–DNA interactions between transcription factors and transcription factor binding sites are essential activities in gene regulation. To decipher the binding codes, it is a long-standing challenge to understand the binding mechanism across different transcription factor DNA binding families. Past computational learning studies usually focus on learning and predicting the DNA binding residues on protein side. Taking into account both sides (protein and DNA), we propose and describe a computational study for learning the specificity-determining residue-nucleotide interactions of different known DNA-binding domain families. The proposed learning models are compared to state-of-the-art models comprehensively, demonstrating its competitive learning performance. In addition, we describe and propose two applications which demonstrate how the learnt models can provide meaningful insights into protein–DNA interactions across different DNA binding families.

  5. A review of experimental methods for determining residual creep life

    International Nuclear Information System (INIS)

    Bolton, C.J.

    1977-11-01

    Experimental methods available for determining how much creep life remains at a particular time in the high temperature service of a component are reviewed. After a brief consideration of the limitations of stress rupture extrapolation techniques, the application of post-exposure creep testing is considered. Ways of assessing the effect of microstructural degradation on residual life are then reviewed. It is pointed out that while this type of work will be useful for certain materials, there are other materials in which 'mechanical damage' such as cavitation will be more important. Cavitation measurement techniques are therefore reviewed. The report ends with a brief consideration of the use of crack growth measurements in assessing the residual life of cracked components. (author)

  6. Impact of Different Lignin Fractions on Saccharification Efficiency in Diverse Species of the Bioenergy Crop Miscanthus

    NARCIS (Netherlands)

    Weijde, van der Tim; Torres Salvador, Andres Francisco; Dolstra, Oene; Dechesne, Annemarie; Visser, Richard G.F.; Trindade, Luisa M.

    2016-01-01

    Lignin is a key factor limiting saccharification of lignocellulosic feedstocks. In this comparative study, various lignin methods—including acetyl bromide lignin (ABL), acid detergent lignin (ADL), Klason lignin (KL), and modified ADL and KL determination methods—were evaluated for their

  7. Proficiency test on the determination of pesticide residues in grapes with multi-residue methods.

    Science.gov (United States)

    Dehouck, Pieter; Grimalt, Susana; Dabrio, Marta; Cordeiro, Fernando; Fiamegos, Yiannis; Robouch, Piotr; Fernández-Alba, Amadeo R; de la Calle, Beatriz

    2015-05-22

    This manuscript presents the results of the International Measurement Evaluation Programme 37 (IMEP-37) study, a proficiency test (PT) which was organised to assess the world-wide performance of food control laboratories on the determination of pesticide residues in grapes. This PT supports the implementation of Regulation (EC) No 396/2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin. Eighty-one participants reported results, forty from EU Member States and forty-one from outside the EU. The test item was a grape sample spiked with 20 selected pesticides. The results of the participants were rated with z- and zeta (ζ-) scores in accordance with ISO 13528 and ISO 17043. The standard deviation for the proficiency assessment, σˆ, of this PT was set at 25% for the 20 measured pesticides based on previous experience with similar measurands. The results reported to IMEP-37 showed that the participants performed satisfactorily, ranging from 81% (carbendazim) to 97% (azoxystrobin, penconazole, pyrimethanil) of the participating laboratories. However, only 30% of the participants managed to analyze all pesticides satisfactorily. Overall, the performance of the participants in this PT was good but there is room for improvement in the development of multi-residue methods for the simultaneous analysis of a large number of pesticides with an increased accuracy. Copyright © 2015 The Authors. Published by Elsevier B.V. All rights reserved.

  8. Lignin-Furfural Based Adhesives

    Directory of Open Access Journals (Sweden)

    Prajakta Dongre

    2015-07-01

    Full Text Available Lignin recovered from the hot-water extract of sugar maple (Acer saccharum is used in this study to synthesize adhesive blends to replace phenol-formaldehyde (PF resin. Untreated lignin is characterized by lignin content and nuclear magnetic resonance (NMR analysis. The molecular weight distribution of the lignin and the blends are characterized by size exclusion chromatography (SEC. The effect of pH (0.3, 0.65 and 1, ex situ furfural, and curing conditions on the tensile properties of adhesive reinforced glass fibers is determined and compared to the reinforcement level of commercially available PF resin. The adhesive blend prepared at pH = 0.65 with no added furfural exhibits the highest tensile properties and meets 90% of the PF tensile strength.

  9. Techniques for characterizing lignin

    Science.gov (United States)

    Nicole M. Stark; Daniel J. Yelle; Umesh P. Agarwal

    2016-01-01

    Many techniques are available to characterize lignin. The techniques presented in this chapter are considered nondegradative, which are commonly applied to lignin. A brief discussion of lignin structure is included with this chapter to aid the reader in understanding why the discussed characterization techniques are appropriate for the study of lignin. Because the...

  10. Validation of a residue method to determine pesticide residues in cucumber by using nuclear techniques

    International Nuclear Information System (INIS)

    Baysoyu, D.; Tiryaki, O.; Secer, E.; Aydin, G.

    2009-01-01

    In this study, a multi-residue method using ethyl acetate for extraction and gel permeation chromatography for clean-up was validated to determine chlorpyrifos, malathion and dichlorvos in cucumber by gas chromatography. For this purpose, homogenized cucumber samples were fortified with pesticides at 0.02 0.2, 0.8 and 1 mg/kg levels. The efficiency and repeatability of the method in extraction and cleanup steps were performed using 1 4C-carbaryl by radioisotope tracer technique. 1 4C-carbaryl recoveries after the extraction and cleanup steps were between 92.63-111.73 % with a repeatability of 4.85% (CV) and 74.83-102.22 % with a repeatability of 7.19% (CV), respectively. The homogeneity of analytical samples and the stability of pesticides during homogenization were determined using radio tracer technique and chromatographic methods, respectively.

  11. Environmental economics of lignin derived transport fuels

    OpenAIRE

    Obydenkova, SV; Kouris, P Panagiotis; Hensen, EJM Emiel; Heeres, Hero J; Boot, MD Michael

    2017-01-01

    This paper explores the environmental and economic aspects of fast pyrolytic conversion of lignin, obtained from 2G ethanol plants, to transport fuels for both the marine and automotive markets. Various scenarios are explored, pertaining to aggregation of lignin from several sites, alternative energy carries to replace lignin, transport modalities, and allocation methodology. The results highlight two critical factors that ultimately determine the economic and/or environmental fuel viability....

  12. Characterization of the effects of lignin and lignin complex particles as filler on a polystyrene film

    International Nuclear Information System (INIS)

    El-Zawawy, Waleed K.; Ibrahim, Maha M.; Belgacem, Mohamed Naceur; Dufresne, Alain

    2011-01-01

    Highlights: ► We have studied the use of Co(II) to form a complex with the lignin. We use first vanillin as the lignin model and we observed a change in color for the produced complex depending on the light wavelength. The use of other transition metals does not give the same observation. ► The use of the transition metal with the lignin precipitated from the black liquor after pulping of agricultural residues, gave a fluorescent color under fluorescent microscope. ► We applied the resulted lignin complex to prepare polymer film that can be used as special polymer packaging which can be color changed under different wavelengths. - Abstract: The work in this research outlines the use of lignin precipitated from lignocellulosic substrate as fillers after modified with transition metal cations, Fe(III), Ni(II) and Co(II), in the production of a polystyrene based composite for polymer packaging applications. Virgin polystyrene was compared with lignin and lignin complex filled composites with loading of 5% by weight prepared using twin screw extrusion. The lignin complexes were first characterized by the UV spectra to identify the new absorption bands occurred due to the complex formation. Moreover, lignin model, namely vanillin, was used to notify the geometric structure of the resulting complexes applying the GC mass spectra. Scanning electron microscopy was used to indicate the change in the morphological structure of the filler particles. On the other hand, the mechanical and thermal analysis for the resulting polymer composites was studied and it was noticed that the type of lignin or lignin complex plays a roll in the results. The inclusion of the Co(II)–lignin complex was observed to increase the tensile strength of the resulting polymer composite and a decrease of the glass transition temperature. Furthermore, light wave lengths and UV fluorescent microscope were used to identify the change of color for the resulting polymer film.

  13. Characterization of the effects of lignin and lignin complex particles as filler on a polystyrene film

    Energy Technology Data Exchange (ETDEWEB)

    El-Zawawy, Waleed K., E-mail: wkzawawy@yahoo.com [Cellulose and Paper Department, National Research Center, El-Tahrir St., Giza (Egypt); Ibrahim, Maha M. [Cellulose and Paper Department, National Research Center, El-Tahrir St., Giza (Egypt); Belgacem, Mohamed Naceur; Dufresne, Alain [Grenoble Institute of Technology (INP) - The International School of Paper, Print Media and Biomaterials (PAGORA), BP 65, 38402 Saint Martin d' Heres cedex, Grenoble (France)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer We have studied the use of Co(II) to form a complex with the lignin. We use first vanillin as the lignin model and we observed a change in color for the produced complex depending on the light wavelength. The use of other transition metals does not give the same observation. Black-Right-Pointing-Pointer The use of the transition metal with the lignin precipitated from the black liquor after pulping of agricultural residues, gave a fluorescent color under fluorescent microscope. Black-Right-Pointing-Pointer We applied the resulted lignin complex to prepare polymer film that can be used as special polymer packaging which can be color changed under different wavelengths. - Abstract: The work in this research outlines the use of lignin precipitated from lignocellulosic substrate as fillers after modified with transition metal cations, Fe(III), Ni(II) and Co(II), in the production of a polystyrene based composite for polymer packaging applications. Virgin polystyrene was compared with lignin and lignin complex filled composites with loading of 5% by weight prepared using twin screw extrusion. The lignin complexes were first characterized by the UV spectra to identify the new absorption bands occurred due to the complex formation. Moreover, lignin model, namely vanillin, was used to notify the geometric structure of the resulting complexes applying the GC mass spectra. Scanning electron microscopy was used to indicate the change in the morphological structure of the filler particles. On the other hand, the mechanical and thermal analysis for the resulting polymer composites was studied and it was noticed that the type of lignin or lignin complex plays a roll in the results. The inclusion of the Co(II)-lignin complex was observed to increase the tensile strength of the resulting polymer composite and a decrease of the glass transition temperature. Furthermore, light wave lengths and UV fluorescent microscope were used to identify

  14. Understanding pulp delignification by laccase-mediator systems through isolation and characterization of lignin-carbohydrate complexes.

    Science.gov (United States)

    Du, Xueyu; Li, Jiebing; Gellerstedt, Göran; Rencoret, Jorge; Del Río, José C; Martínez, Angel T; Gutiérrez, Ana

    2013-09-09

    The effects and mechanism of pulp delignification by laccases in the presence of redox mediators have been investigated on unbleached eucalyptus kraft pulp treated with laccases from Pycnoporus cinnabarinus (PcL) and Myceliophthora thermophila (MtL) and 1-hydroxybenzotriazole (HBT) and methyl syringate (MeS) as mediators, respectively. Determination of the corrected κ number in eucalyptus pulps after the enzymatic treatments revealed that the PcL-HBT system exhibited a more remarkable delignification effect than the MtL-MeS system. To obtain further insight, lignin-carbohydrate complexes were fractionated and subsequently characterized by nuclear magnetic resonance, thioacidolysis (followed by gas chromatography and size exclusion chromatography), and pyrolysis-gas chromatography-mass spectrometry (pyrolysis-GC-MS) analyses before and after the enzymatic treatments and their controls. We can conclude that the laccase-mediator treatments altered the lignin structures in such a way that more lignin was recovered in the xylan-lignin fractions, as shown by Klason lignin estimation, with smaller amounts of both syringyl (S) and guaiacyl (G) uncondensed units, as shown by thioacidolysis and gas chromatography, especially after the PcL-HBT treatment. The laccase-mediator treatment produced oxidation at Cα and cleavage of Cα and Cβ bonds in pulp lignin, as shown by pyrolysis-GC-MS. The general mechanism of residual lignin degradation in the pulp by laccase-mediator treatments is discussed in light of the results obtained.

  15. Determination of Pesticides Residues in Cucumbers Grown in Greenhouse and the Effect of Some Procedures on Their Residues.

    Science.gov (United States)

    Leili, Mostafa; Pirmoghani, Amin; Samadi, Mohammad Taghi; Shokoohi, Reza; Roshanaei, Ghodratollah; Poormohammadi, Ali

    2016-11-01

    The objective of this study was to determine the residual concentrations of ethion and imidacloprid in cucumbers grown in greenhouse. The effect of some simple processing procedures on both ethion and imidacloprid residues were also studied. Ten active greenhouses that produce cucumber were randomly selected. Ethion and imidacloprid as the most widely used pesticides were measured in cucumber samples of studied greenhouses. Moreover, the effect of storing, washing, and peeling as simple processing procedures on both ethion and imidacloprid residues were investigated. One hour after pesticide application; the maximum residue levels (MRLs) of ethion and imidacloprid were higher than that of Codex standard level. One day after pesticide application, the levels of pesticides were decreased about 35 and 31% for ethion and imidacloprid, respectively, which still were higher than the MRL. Washing procedure led to about 51 and 42.5% loss in ethion and imidacloprid residues, respectively. Peeling procedure also led to highest loss of 93.4 and 63.7% in ethion and imidacloprid residues, respectively. The recovery for both target analytes was in the range between 88 and 102%. The residue values in collected samples one hour after pesticides application were higher than standard value. The storing, washing, and peeling procedures lead to the decrease of pesticide residues in greenhouse cucumbers. Among them, the peeling procedure has the greatest impact on residual reduction. Therefore, these procedures can be used as simple and effective processing techniques for reducing and removing pesticides from greenhouse products before their consumption.

  16. Modulating lignin in plants

    Science.gov (United States)

    Apuya, Nestor; Bobzin, Steven Craig; Okamuro, Jack; Zhang, Ke

    2013-01-29

    Materials and methods for modulating (e.g., increasing or decreasing) lignin content in plants are disclosed. For example, nucleic acids encoding lignin-modulating polypeptides are disclosed as well as methods for using such nucleic acids to generate transgenic plants having a modulated lignin content.

  17. Effect of lignin on morphology, biodegradability, mechanical and thermal properties of low linear density polyethylene/lignin biocomposites

    Science.gov (United States)

    Ghozali, M.; Triwulandari, E.; Haryono, A.; Yuanita, E.

    2017-07-01

    This research is purposed to study effects of lignin compositions on morphology, biodegradability, mechanical and thermal properties of low linear density polyethylene (LLDPE)/Lignin biocomposites. LLDPE/Lignin biocomposites has been manufactured by adding LLDPE, lignin and compatibilizer into rheomix at 200°C with a stirring speed of 70 rpm for 30 min. The composition of lignin added was 5, 10, 15, and 20 phr with compatibilizer 5 phr. LLDPE/lignin films has been made by using hydraulic hot press at 200-210°C with pressure of 6 bar for 20 min. Fourier Transform Infrared (FTIR) spectrum analysis was conducted to determine the functional groups of LLDPE/Lignin biocomposites. The surface morphology was observed by using Scanning Electron Microscope (SEM). The mechanical properties was measured as a tensile strength and thermal stability was measured by Thermogravimetric Analysis (TGA). In addition, biodegradation test was also conducted to determine the level of biodegradability. TGA results indicated that at 456°C LLDPE and lignin had similar thermal stability and the addition of lignin into LLDPE/lignin bicomposites can reduce the thermal stability up to temperature of 450-460°C. However, the thermal stability is increased at temperature over 460°C. The tensile strength and elongation at break of all LLDPE/Lignin biocomposites at various compositions is lower compared to those of LLDPE. The more lignin were added into LLDPE/Lignin biocomposites, the more the materials were biodegraded.

  18. Analytical methods for lignin characterization - Differential scanning calorimetry

    NARCIS (Netherlands)

    Koullas, D.P.; Koukios, E.G.; Avgerinos, E.; Abaecherli, A.; Gosselink, R.; Vasile, C.; Lehnen, R.; Saake, B.; Suren, J.

    2006-01-01

    Results of a round robin on lignin thermal analyses are reported. Six laboratories have conducted thermal analyses of four lignin types to determine their cp values and softening points, and to study the thermal behaviour, materials endo- and exotherms included. The lignin types examined were wood

  19. Determination of ractopamine in animal hair: application to residue depletion in sheep and residue monitoring.

    Science.gov (United States)

    Suo, Decheng; Zhao, Genlong; Wang, Ruiguo; Su, Xiaoou

    2014-12-01

    An ultra-performance liquid chromatography tandem mass spectrometry method to determine ractopamine (RAC) in hair samples from swine, sheep, and cattle was developed. The procedure to extract from incurred hair was optimized. The samples were extracted with 0.1mol/L HCl solution. The mixture was heated to 60°C in water bath for 4h. The extracts were purified by solid-phase extraction, dried under a stream of nitrogen, and then reconstituted in mobile phase for analysis, which was performed with a Waters BEH-C18 column. The limit of detection was 0.3ng/g, the limit of quantification was 1ng/g, the recoveries were between 87% and 105%, and the coefficient of variation was less than 15%. The depletion of RAC in hair was studied in healthy sheep after administration of RAC at 1000ng/g body weight for five consecutive days. The RAC residues were still detected with 82.5±7.2ng/g hair 27 days after drug administration. Five samples tested positive, in which the amount of RAC detected was 13-253ng/g from 569 hair samples collected from farms and slaughterhouses. These results show that animal hair is a suitable medium to monitor the illegal use of RAC in livestock production. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Advances in the chemical utilization of alkali lignin

    International Nuclear Information System (INIS)

    Van der Klashorst, G.H.

    1985-06-01

    Large quantities of alkali lignin are produced as by-products by the South African pulping industry. The potential utilization of industrial soda/anthraquinone (soda/AQ) eucalyptus, kraft pine and soda bagasse lignin was subsequently investigated. The molecular mass distributions of the three lignins were similar when determined by high pressure gel permeation chromatography (HP-GPC). The quantitative and quanlitative occurrence of various low molecular mass lignin fragments in the different spent liquors, on the other hand, indicated that the three lignins have substantial chemical differences. Analysis of the purified degraded lignins by NMR, methoxyl content determinations, elemental analysis, carbohydrate content determinations etc., quantified various of the chemical properties of the lignin. The properties of the three lignins were ultimately used to make recommendations regarding the potential use of each lignin. One such application was investigated and it was shown that soda bagasse lignin can be used successfully in phenol formaldehyde resin applications. The reaction of formaldehyde with lignin model compounds in acidic medium was also investigated. This reaction was shown to give fast crosslinking of alkyl substituted phenolic and etherified phenolic lignin model compounds at positions meta to the aromatic hydroxy groups

  1. Structure variations of carbonizing lignin

    International Nuclear Information System (INIS)

    Otani, C.; Polidoro, H.A.; Otani, S.; Craievich, A.F.

    1984-01-01

    The studied lignin is a by-product of the process of ethanol production from eucaliptus. It was heat-treated under inert atmosphere conditions at increasing temperatures from 300C up to 2400C. The structural variations were studied by wide-angle X-ray diffraction, small-angle X-ray scattering and infrared absorption spectroscopy. The bulk and 'real' density of the compacted materials have also been determined as functions of the final temperature. These experimental results enabled us to establish a mechanism of structure variation based on the formation of a turbostratic graphite-like and porous structure within the initially amorphous lignin matrix. (Author) [pt

  2. Lignin Valorization: Emerging Approaches

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T [National Renewable Energy Laboratory (NREL), Golden, CO (United States)

    2018-04-03

    Lignin, an aromatic biopolymer found in plant cell walls, is a key component of lignocellulosic biomass and generally utilized for heat and power. However, lignin's chemical composition makes it an attractive source for biological and catalytic conversion to fuels and chemicals. Bringing together experts from biology, catalysis, engineering, analytical chemistry, and techno-economic/life-cycle analysis, Lignin Valorization presents a comprehensive, interdisciplinary picture of how lignocellulosic biorefineries could potentially employ lignin valorization technologies. Chapters will specifically focus on the production of fuels and chemicals from lignin and topics covered include (i) methods for isolating lignin in the context of the lignocellulosic biorefinery, (ii) thermal, chemo-catalytic, and biological methods for lignin depolymerization, (iii) chemo-catalytic and biological methods for upgrading lignin, (iv) characterization of lignin, and (v) techno-economic and life-cycle analysis of integrated processes to utilize lignin in an integrated biorefinery. The book provides the latest breakthroughs and challenges in upgrading lignin to fuels and chemicals for graduate students and researchers in academia, governmental laboratories, and industry interested in biomass conversion.

  3. Determination of residual stresses at ILL present and future

    CERN Document Server

    Pirling, T

    2002-01-01

    The ILL is constructing, in collaboration with the Manchester Materials Science Centre, a neutron strain imager for the non-destructive determination of residual stresses. The project is funded by ILL and the EPSRC (Engineering and Physical Science Research Council) on a fifty-fifty basis. A special feature of the instrument is the sample table, which will be a Stewart platform or hexapod. It allows most flexible sample movement, having a load capacity of more than 500 kg and allowing sample sizes of up to 2-m length. A new supermirror neutron guide and a specially developed two-dimensional focusing monochromator will provide more than 2.6 times the neutron flux of the present instrument. A limitation of the neutron strain scanning technique is the surface effect, which introduces huge errors when scanning through interfaces or surfaces. Experiments have shown that the use of radial collimators for beam-defining optics reduces the surface error drastically. Such a configuration is one option of the present st...

  4. Determination of gas residues in uranium dioxide pellets

    International Nuclear Information System (INIS)

    Riella, H.G.

    1978-01-01

    The measurement of low amounts of residual gases, excluding water, in ceramic grade uranium dioxide pellets, using high temperature vacuum extraction technique, is dealt with. The high temperature extraction gas analysis apparatus was designed and assembled for sequential analysis of up to eight uranium dioxide pellets by run. The system consists of three major units, namely outgassing unit, transfer unit and analytical unit. The whole system is evacuated to a final pressure of less then 10 -5 torr. A weighed pellet is transfered into the outgassing unit for subsequent dropping into a Platinum-Rhodium crucible which is heated inductively up to 1600 0 C during 30 minutes. The released gases are imediately transfered from the outgassing to analytical unit passing through a cold trap at -95 0 C to remove water vapor. The gases are transfered to previously calibrated volumetric bulb where the total pressure and temperature are determined. An estimate of the gas content in the pellets at STP condition is obtained from the measured volume, pressure and temperature of the gas mixture by applying ideal gases equation. Analysis to two lots (fourteen samples) of uranium dioxide pellets by the method described here indicated a mean gas content of 0,060cm 3 /g UO 2 . The lower limit of this technique is 0,03cm 3 /g UO 2 (STP). The time required for the analysis of eight pellets is about 9 hours [pt

  5. Hydrothermal Liquefaction of Enzymatic Hydrolysis Lignin: Biomass Pretreatment Severity Affects Lignin Valorization

    DEFF Research Database (Denmark)

    Jensen, Mads M.; Djajadi, Demi T.; Torri, Cristian

    2018-01-01

    Alkalinehydrothermal liquefaction (HTL) of lignin-rich enzymatichydrolysis residues (EnzHR) from wheat straw and Miscanthusx giganteus was performed at 255, 300, and 345 °C to investigate valorization of this side-stream from second-generation bioethanol production. The EnzHR were from biomass...... contributed with additional chemical information as well as confirming trends seen from quantified monomers. This work is relevant for future lignin valorization in biorefineries based on current second-generation bioethanol production....

  6. Production of hydrogen by lignins fast pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Baumlin, Sebastien; Broust, Francois; Bazer-Bachi, Frederic; Bourdeaux, Thomas; Herbinet, Olivier; Toutie Ndiaye, Fatou; Ferrer, Monique; Lede, Jacques [Laboratoire des Sciences du Genie Chimique, CNRS-ENSIC, 1, rue Grandville, BP 20451, 54001 Nancy Cedex (France)

    2006-12-15

    This paper reports the results of experiments performed on the flash pyrolysis of lignin samples submitted to controlled heat flux densities (short flashes of a concentrated radiation). Two types of lignins are used: Kraft and Organocell lignins. Microscopic observations of the reacted samples reveal the formation of an intermediate liquid compound that precedes the further formation of char, vapours and gases. The rates of mass loss and the production rates of the products are determined for both lignins. The results are compared to each other and to those obtained in former similar studies made with cellulose. The analyses of the produced gases reveal high syngas and H{sub 2} contents (respectively 87 and 50mol%). This composition is compared to results obtained in other different thermal conditions with lignins and other types of biomasses. The possible mechanism of hydrogen formation is further discussed. (author)

  7. The degradation of wheat straw lignin

    Science.gov (United States)

    Liang, Jiaqi

    2017-03-01

    Lignin is a kind of formed by polymerization of aromatic alcohol, prices are lower and sources of renewable resources. Using lignin as raw material, through the push to resolve together preparation phenolic high value-added fine chemicals alkanes and aromatic hydrocarbons, such as the high grade biofuels, can partly replace fossil fuels as raw material to the production process, biomass resources is an important part of the comprehensive utilization of effective components. In lignin push solve clustering method, catalytic hydrogenolysis can directly to the lignin into liquid fuels, low oxygen content in the use of biofuels shows great potential. In this paper, through the optimization of the reaction time, reaction temperature, catalyst type and solvent type, dosage of catalyst, etc factors, determines the alcoholysis - hydrogen solution two-step degradation of lignin, the optimal process conditions: lignin alcoholysis under 50% methanol and NaOH catalyst in the solution, the lignin in methanol solution and 50% hydrogen solution under the Pd/C catalyst. In this process, the degradation of lignin yield can reach 42%.

  8. Formation of a tyrosine adduct involved in lignin degradation by Trametopsis cervina lignin peroxidase: a novel peroxidase activation mechanism

    Science.gov (United States)

    Yuta Miki; Rebecca Pogni; Sandra Acebes; Fatima Lucas; Elena Fernandez-Fueyo; Maria Camilla Baratto; Maria I. Fernandez; Vivian De Los Rios; Francisco J. Ruiz-duenas; Adalgisa Sinicropi; Riccardo Basosi; Kenneth E. Hammel; Victor Guallar; Angel T. Martinez

    2013-01-01

    LiP (lignin peroxidase) from Trametopsis cervina has an exposed catalytic tyrosine residue (Tyr181) instead of the tryptophan conserved in other lignin-degrading peroxidases. Pristine LiP showed a lag period in VA (veratryl alcohol) oxidation. However, VA-LiP (LiP after treatment with H2O2...

  9. Determination of specificity influencing residues for key transcription factor families

    DEFF Research Database (Denmark)

    Patel, Ronak Y.; Garde, Christian; Stormo, Gary D.

    2015-01-01

    Transcription factors (TFs) are major modulators of transcription and subsequent cellular processes. The binding of TFs to specific regulatory elements is governed by their specificity. Considering the gap between known TFs sequence and specificity, specificity prediction frameworks are highly...... desired. Key inputs to such frameworks are protein residues that modulate the specificity of TF under consideration. Simple measures like mutual information (MI) to delineate specificity influencing residues (SIRs) from alignment fail due to structural constraints imposed by the three...

  10. Lignin depolymerization by fungal secretomes and a microbial sink

    Energy Technology Data Exchange (ETDEWEB)

    Salvachúa, Davinia; Katahira, Rui; Cleveland, Nicholas S.; Khanna, Payal; Resch, Michael G.; Black, Brenna A.; Purvine, Samuel O.; Zink, Erika M.; Prieto, Alicia; Martínez, María J.; Martínez, Angel T.; Simmons, Blake A.; Gladden, John M.; Beckham, Gregg T.

    2016-08-25

    In Nature, powerful oxidative enzymes secreted by white rot fungi and some bacteria catalyze lignin depolymerization and some microbes are able to catabolize the resulting aromatic compounds as carbon and energy sources. Taken together, these two processes offer a potential route for microbial valorization of lignin. However, many challenges remain in realizing this concept, including that oxidative enzymes responsible for lignin depolymerization also catalyze polymerization of low molecular weight (LMW) lignin. Here, multiple basidiomycete secretomes were screened for ligninolytic enzyme activities in the presence of a residual lignin solid stream from a corn stover biorefinery, dubbed DMR-EH (Deacetylation, Mechanical Refining, and Enzymatic Hydrolysis) lignin. Two selected fungal secretomes, with high levels of laccases and peroxidases, were utilized for DMR-EH lignin depolymerization assays. The secretome from Pleurotus eryngii, which exhibited the highest laccase activity, reduced the lignin average molecular weight by 63% and 75% at pH 7 compared to the Mw of the control treated at the same conditions and the initial DMR-EH lignin, respectively, and was applied in further depolymerization assays as a function of time. As repolymerization was observed after 3 days of incubation, an aromatic-catabolic microbe (Pseudomonas putida KT2440) was incubated with the fungal secretome and DMR-EH lignin. These experiments demonstrated that the presence of the bacterium enhances lignin depolymerization, likely due to bacterial catabolism of LMW lignin, which may partially prevent repolymerization. In addition, proteomics was also applied to the P. eryngii secretome to identify the enzymes present in the fungal cocktail utilized for the depolymerization assays, which highlighted a significant number of glucose/ methanol/choline (GMC) oxidoreductases and laccases. Overall, this study demonstrates that ligninolytic enzymes can be used to partially depolymerize a solid, high

  11. Depolymerization of lignin via co-pyrolysis with 1,4-butanediol in a microwave reactor

    Science.gov (United States)

    The production of valuable compounds from low cost but abundant residual lignin has proven to be challenging. The lack of effective biochemical lignin depolymerization processes has led many to focus on thermochemical conversion methods. Bench scale microwave pyrolysis of lignin has been performed...

  12. Analytical methodology for sulfonated lignins

    NARCIS (Netherlands)

    Brudin, S.; Schoenmakers, P.

    2010-01-01

    There is a significant need to characterize and classify lignins and sulfonated lignins. Lignins have so far received a good deal of attention, whereas this is not true for sulfonated lignins. There is a clear demand for a better understanding of sulfonated lignins on a chemical as well as physical

  13. Noncatalytic Direct Liquefaction of Biorefinery Lignin by Ethanol

    DEFF Research Database (Denmark)

    Nielsen, Joachim Bachmann; Jensen, Anders; Madsen, Line Riis

    2017-01-01

    There is a growing interest in lignin valorization to biofuels and chemicals. Here, we propose a novel and simple noncatalytic process to directly liquefy lignin rich solid residual from second generation bioethanol production by solvolysis with ethanol. Through an extensive parameter study...... in batch autoclaves assessing the effects of varying reaction temperature, reaction time, and solvent:lignin ratio, it is shown that hydrothermally pretreated enzymatic hydrolysis lignin solvolysis in supercritical ethanol can produce a heptane soluble bio-oil without the need for exhaustive deoxygenation....... The process does not require addition of catalyst or a reducing agent such as hydrogen. The process is advantageously carried out with a low reaction period ((ethanol:lignin (w/w) ratio of 2:1) which is a previously unexplored domain for lignin...

  14. A new spectrophotometric method for determination of residual ...

    African Journals Online (AJOL)

    Polydiallyldimethylammonium chloride (polyDADMAC) is a water-soluble cationic polyelectrolyte used for water treatment. Its residues in treated water are contaminants as they react with chlorine to produce a carcinogenic compound. Commonly-used techniques for quantification of the polycation, such as colloidal and ...

  15. Rapid multi-residue method for the determination of pesticide ...

    African Journals Online (AJOL)

    Exposure to pesticides can represent a potential risk to humans. Agricultural workers are at risk of chronic toxicity. Hence, the evaluation of pesticide residues in their blood gives an indication about the extent of exposure and help in assessing adverse health effects. The aim of our study was to develop analytical method for ...

  16. Determination of residual stress within complex-shaped coarse-grained cobalt-chrome biomedical castings

    OpenAIRE

    Conroy, Brian P; Tanner, David A

    2016-01-01

    peer-reviewed ASTM F75 femoral knee implant casting components distort during manufacture due to residual stress re-distribution or inducement. These castings pose a number of challenges for residual stress determination methods; they have a complex geometry, their micro-structure is inhomogeneous, they work-harden rapidly and they have a coarse, elastically-anisotropic grain structure. The contour method is anticipated to be the most promising residual stress determination technique. X-ra...

  17. Determination of organophosphorus pesticide residues in tomatoes by gas chromatography

    International Nuclear Information System (INIS)

    Souissi, Sihem

    2010-01-01

    Chloropyriphos and malathion are two organophosphorus pesticides from many others pesticides widely used by famers in agriculture .Because of their bad effect on human health, officials standards are set by the international organisations and communities to ensure safer food for consumer .In the same way, scientists over the world are working hard to develop new detection techniques responding to the international requirements. In this study, an ' IAEA-ethylacetate method ', an adaptation of the popular QuEChERS multi residue method, was optimized to analyse chloropyriphos and Malathion residues in tomatoes .Ethyl-Acetate was used as an extraction solvent the PSA was kept for the clean up procedure. GC-NPD is used for samples analysis .The method optimized is specifique, selective with a recovery averaged more than 70 pour cent. A complete validation of the method is necessary to be used for routine analysis.

  18. Determination and Extraction of Acetamiprid Residues in Fruits and Vegetables

    Directory of Open Access Journals (Sweden)

    Allah Nawaz

    2015-12-01

    Full Text Available   Vegetables (chilies, tomato, cauliflower and cucumber and fruits (mango and apple samples were spiked with known quantity (0.50 mg kg-1 of acetamiprid reference standard for testing the retrieval percentage of acetamiprid residue in those vegetables and fruits. The efficiency of different extracting (ethyl acetate and dichloromethane + acetone 8:2 and eluting (ethyl acetate and dichloromethane + acetone 8:2 solvents and adsorbents (activated charcoal and florisil for clean up purpose was calculated using HPLC. Amongst the extracting solvents ethyl-acetate was observed an effective extracting solvent alone which produced maximum 90-96%  recovery for acetamiprid residues while among the eluting solvents a combination of dichloromethane and acetone ( ratio 8:2 produced superior recoveries i.e. 87-95%. Similarly, between the adsorbents used for clean up purpose activated charcoal and florisil in tandem (first from charcoal and then through florisil yielded recoveries 82-90 % whereas adsorbents used alone in form of activated florisil and charcoal recovered only 70 to 78 % and 71 to 73% acetamiprid residues, respectively in all vegetables and fruits.

  19. A method for the determination of residual beta activity in drinking water samples

    Energy Technology Data Exchange (ETDEWEB)

    Idoeta, R. [Dpto. Ingenieria Nuclear y Mecanica de Fluidos, E. T. S. Ingenieria de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n. 48013 Bilbao (Spain)], E-mail: raquel.idoeta@ehu.es; Herranz, M.; Abelairas, A.; Legarda, F. [Dpto. Ingenieria Nuclear y Mecanica de Fluidos, E. T. S. Ingenieria de Bilbao - Universidad del Pais Vasco (UPV/EHU), Alda. Urquijo s/n. 48013 Bilbao (Spain)

    2007-09-15

    The determination of residual beta activity in drinking water is usually needed in most monitoring programs. In this work a procedure for its determination is described and expressions for the calculations of detection limits and uncertainties are proposed.

  20. A method for the determination of residual beta activity in drinking water samples

    International Nuclear Information System (INIS)

    Idoeta, R.; Herranz, M.; Abelairas, A.; Legarda, F.

    2007-01-01

    The determination of residual beta activity in drinking water is usually needed in most monitoring programs. In this work a procedure for its determination is described and expressions for the calculations of detection limits and uncertainties are proposed

  1. Multivariate concentration determination using principal component regression with residual analysis.

    Science.gov (United States)

    Keithley, Richard B; Heien, Michael L; Wightman, R Mark

    2009-10-01

    Data analysis is an essential tenet of analytical chemistry, extending the possible information obtained from the measurement of chemical phenomena. Chemometric methods have grown considerably in recent years, but their wide use is hindered because some still consider them too complicated. The purpose of this review is to describe a multivariate chemometric method, principal component regression, in a simple manner from the point of view of an analytical chemist, to demonstrate the need for proper quality-control (QC) measures in multivariate analysis and to advocate the use of residuals as a proper QC method.

  2. Novel approaches to determining residual stresses by ultramicroindentation techniques: Application to sandblasted austenitic stainless steel

    International Nuclear Information System (INIS)

    Frutos, E.; Multigner, M.; Gonzalez-Carrasco, J.L.

    2010-01-01

    This research addresses the determination of residual stresses in sandblasted austenitic steel by ultramicroindentation techniques using a sharp indenter, of which the sensitivity to residual stress effects is said to be inferior to that of spherical ones. The introduction of an angular correction in the model of Wang et al. which relates variations in the maximum load to the presence of residual stresses is proposed. Similarly, the contribution to the hardness of grain size refinement and work hardening, developed as a consequence of the severe plastic deformation during blasting, is determined in order to avoid overestimation of the residual stresses. Measurements were performed on polished cross sections along a length of several microns, thus obtaining a profile of the residual stresses. Results show good agreement with those obtained by synchrotron radiation on the same specimens, which validates the method and demonstrates that microindentation using sharp indenters may be sensitive to the residual stress effect.

  3. Novel approaches to determining residual stresses by ultramicroindentation techniques: Application to sandblasted austenitic stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Frutos, E. [Centro de Bioingenieria, Biomateriales y Nanomedicina, CIBER-BBN, Instituto de Salud Carlos III (Spain)] [Centro Nacional de Investigaciones Metalurgicas, CENIM-CSIC, 28040 Madrid (Spain); Multigner, M. [Centro Nacional de Investigaciones Metalurgicas, CENIM-CSIC, 28040 Madrid (Spain)] [Centro de Bioingenieria, Biomateriales y Nanomedicina, CIBER-BBN, Instituto de Salud Carlos III (Spain); Gonzalez-Carrasco, J.L., E-mail: jlg@cenim.csic.es [Centro Nacional de Investigaciones Metalurgicas, CENIM-CSIC, 28040 Madrid (Spain)] [Centro de Bioingenieria, Biomateriales y Nanomedicina, CIBER-BBN, Instituto de Salud Carlos III (Spain)

    2010-07-15

    This research addresses the determination of residual stresses in sandblasted austenitic steel by ultramicroindentation techniques using a sharp indenter, of which the sensitivity to residual stress effects is said to be inferior to that of spherical ones. The introduction of an angular correction in the model of Wang et al. which relates variations in the maximum load to the presence of residual stresses is proposed. Similarly, the contribution to the hardness of grain size refinement and work hardening, developed as a consequence of the severe plastic deformation during blasting, is determined in order to avoid overestimation of the residual stresses. Measurements were performed on polished cross sections along a length of several microns, thus obtaining a profile of the residual stresses. Results show good agreement with those obtained by synchrotron radiation on the same specimens, which validates the method and demonstrates that microindentation using sharp indenters may be sensitive to the residual stress effect.

  4. Lignin charcoal: byproduct of acid hydrolysis of eucalypt wood. [E. urophylla

    Energy Technology Data Exchange (ETDEWEB)

    Foelkel, C.E.B.; Zvinakevicius, C.; Carolino, J.M.; Pimenta, D.L.

    1981-01-01

    Studies are described in which wood of Eucalyptus urophylla was subjected to hydrolysis with sulphuric acid and the acidic or neutralized lignin residue was converted to charcoal in a laboratory oven with a nitrogen atmosphere. The lignin charcoal compared favourably with charcoal from eucalypt wood with regard to fixed carbon content and calorific capacity. Yield of charcoal from the lignin was about 53% based on the residue, or 15-16% based on the original amount of wood.

  5. Study On The Procedures For Determining Of Pesticide Residues In Green Vegetables

    International Nuclear Information System (INIS)

    Le Tat Mua; Nguyen Tien Dat; Nguyen Van Minh; Nguyen Ngoc Tuan; Le Thi Ngoc Trinh; Ta Thi Tuyet Nhung; Truong Van Tai; Tran Thanh Nha; Nguyen Thi Hong Tham

    2007-01-01

    Researches presented in this work are divided into two main parts. One part embraces the residue analytical methods. The other part comprises applying of these residue analytical methods for analysis of plant material. Part I: Residue analytical methods (Analytical procedures): Determination of Endosulphan in plant material by GC/ECD; Determination of Methamidofos in plant material by GC/FTD; Determination of Deltamethrin, Cyhalothrin, Cyfluthrin in plant material by GC/ECD; Determination of Maneb in plant material by HPLC/UV; Determination of Zineb in plant material by F-AAS; Determination of Organo-Asenic and Mercury in plant material by RNAA; The limits of detection and determination (LOD, LOQ), Recovery, Efficiency, the Calibration curve are validated. Part II: Applying of Residue Analytical Methods for analysis of endosulphan, methamidofos, maneb, zineb, cyhalothrin, deltamethrin, cyfluthrin, metallo-organic compounds in Spinach, Cabbage, Pimento, Japanese Bean, Japanese Pumpkin, Tomato, Potato, Sweet Potato. The results and conclusion are present in this work. (author)

  6. Catalytic Oxidation and Depolymerization of Lignin in Aqueous Ionic Liquid

    International Nuclear Information System (INIS)

    Das, Lalitendu; Xu, Siquan; Shi, Jian

    2017-01-01

    Lignin is an integral part of the plant cell wall, which provides rigidity to plants, also contributes to the recalcitrance of the lignocellulosic biomass to biochemical and biological deconstruction. Lignin is a promising renewable feedstock for aromatic chemicals; however, an efficient and economic lignin depolymerization method needs to be developed to enable the conversion. In this study, we investigated the depolymerization of alkaline lignin in aqueous 1-ethyl-3-methylimidazolium acetate [C 2 C 1 Im][OAc] under oxidizing conditions. Seven different transition metal catalysts were screened in presence of H 2 O 2 as oxidizing agent in a batch reactor. CoCl 2 and Nb 2 O 5 proved to be the most effective catalysts in degrading lignin to aromatic compounds. A central composite design was used to optimize the catalyst loading, H 2 O 2 concentration, and temperature for product formation. Results show that lignin was depolymerized, and the major degradation products found in the extracted oil were guaiacol, syringol, vanillin, acetovanillone, and homovanillic acid. Lignin streams were characterized by Fourier transform infrared spectroscopy and gel permeation chromatography to determine effects of the experimental parameters on lignin depolymerization. The weight-average molecular weight (M w ) of liquid stream lignin after oxidation, for CoCl 2 and Nb 2 O 5 catalysts were 1,202 and 1,520 g mol −1 , respectively, lower than that of Kraft lignin. Polydispersity index of the liquid stream lignin increased as compared with Kraft lignin, indicating wide span of the molecular weight distribution as a result of lignin depolymerization. Results from this study provide insights into the role of oxidant and transition metal catalysts and the oxidative degradation reaction sequence of lignin toward product formation in presence of aqueous ionic liquid.

  7. Catalytic Oxidation and Depolymerization of Lignin in Aqueous Ionic Liquid

    Energy Technology Data Exchange (ETDEWEB)

    Das, Lalitendu [Biosystems and Agricultural Engineering, University of Kentucky, Lexington, KY (United States); Xu, Siquan [Biosystems and Agricultural Engineering, University of Kentucky, Lexington, KY (United States); College of Chemical Engineering, Nanjing Forestry University, Nanjing (China); Shi, Jian, E-mail: j.shi@uky.edu [Biosystems and Agricultural Engineering, University of Kentucky, Lexington, KY (United States)

    2017-08-10

    Lignin is an integral part of the plant cell wall, which provides rigidity to plants, also contributes to the recalcitrance of the lignocellulosic biomass to biochemical and biological deconstruction. Lignin is a promising renewable feedstock for aromatic chemicals; however, an efficient and economic lignin depolymerization method needs to be developed to enable the conversion. In this study, we investigated the depolymerization of alkaline lignin in aqueous 1-ethyl-3-methylimidazolium acetate [C{sub 2}C{sub 1}Im][OAc] under oxidizing conditions. Seven different transition metal catalysts were screened in presence of H{sub 2}O{sub 2} as oxidizing agent in a batch reactor. CoCl{sub 2} and Nb{sub 2}O{sub 5} proved to be the most effective catalysts in degrading lignin to aromatic compounds. A central composite design was used to optimize the catalyst loading, H{sub 2}O{sub 2} concentration, and temperature for product formation. Results show that lignin was depolymerized, and the major degradation products found in the extracted oil were guaiacol, syringol, vanillin, acetovanillone, and homovanillic acid. Lignin streams were characterized by Fourier transform infrared spectroscopy and gel permeation chromatography to determine effects of the experimental parameters on lignin depolymerization. The weight-average molecular weight (M{sub w}) of liquid stream lignin after oxidation, for CoCl{sub 2} and Nb{sub 2}O{sub 5} catalysts were 1,202 and 1,520 g mol{sup −1}, respectively, lower than that of Kraft lignin. Polydispersity index of the liquid stream lignin increased as compared with Kraft lignin, indicating wide span of the molecular weight distribution as a result of lignin depolymerization. Results from this study provide insights into the role of oxidant and transition metal catalysts and the oxidative degradation reaction sequence of lignin toward product formation in presence of aqueous ionic liquid.

  8. Catalytic Oxidation and Depolymerization of Lignin in Aqueous Ionic Liquid

    Directory of Open Access Journals (Sweden)

    Lalitendu Das

    2017-08-01

    Full Text Available Lignin is an integral part of the plant cell wall, which provides rigidity to plants, also contributes to the recalcitrance of the lignocellulosic biomass to biochemical and biological deconstruction. Lignin is a promising renewable feedstock for aromatic chemicals; however, an efficient and economic lignin depolymerization method needs to be developed to enable the conversion. In this study, we investigated the depolymerization of alkaline lignin in aqueous 1-ethyl-3-methylimidazolium acetate [C2C1Im][OAc] under oxidizing conditions. Seven different transition metal catalysts were screened in presence of H2O2 as oxidizing agent in a batch reactor. CoCl2 and Nb2O5 proved to be the most effective catalysts in degrading lignin to aromatic compounds. A central composite design was used to optimize the catalyst loading, H2O2 concentration, and temperature for product formation. Results show that lignin was depolymerized, and the major degradation products found in the extracted oil were guaiacol, syringol, vanillin, acetovanillone, and homovanillic acid. Lignin streams were characterized by Fourier transform infrared spectroscopy and gel permeation chromatography to determine effects of the experimental parameters on lignin depolymerization. The weight-average molecular weight (Mw of liquid stream lignin after oxidation, for CoCl2 and Nb2O5 catalysts were 1,202 and 1,520 g mol−1, respectively, lower than that of Kraft lignin. Polydispersity index of the liquid stream lignin increased as compared with Kraft lignin, indicating wide span of the molecular weight distribution as a result of lignin depolymerization. Results from this study provide insights into the role of oxidant and transition metal catalysts and the oxidative degradation reaction sequence of lignin toward product formation in presence of aqueous ionic liquid.

  9. Reductive Catalytic Fractionation of Corn Stover Lignin

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, Eric M.; Katahira, Rui; Reed, Michelle; Resch, Michael G.; Karp, Eric M.; Beckham, Gregg T.; Román-Leshkov, Yuriy

    2016-12-05

    Reductive catalytic fractionation (RCF) has emerged as an effective biomass pretreatment strategy to depolymerize lignin into tractable fragments in high yields. We investigate the RCF of corn stover, a highly abundant herbaceous feedstock, using carbon-supported Ru and Ni catalysts at 200 and 250 degrees C in methanol and, in the presence or absence of an acid cocatalyst (H3PO4 or an acidified carbon support). Three key performance variables were studied: (1) the effectiveness of lignin extraction as measured by the yield of lignin oil, (2) the yield of monomers in the lignin oil, and (3) the carbohydrate retention in the residual solids after RCF. The monomers included methyl coumarate/ferulate, propyl guaiacol/syringol, and ethyl guaiacol/syringol. The Ru and Ni catalysts performed similarly in terms of product distribution and monomer yields. The monomer yields increased monotonically as a function of time for both temperatures. At 6 h, monomer yields of 27.2 and 28.3% were obtained at 250 and 200 degrees C, respectively, with Ni/C. The addition of an acid cocatalysts to the Ni/C system increased monomer yields to 32% for acidified carbon and 38% for phosphoric acid at 200 degrees C. The monomer product distribution was dominated by methyl coumarate regardless of the use of the acid cocatalysts. The use of phosphoric acid at 200 degrees C or the high temperature condition without acid resulted in complete lignin extraction and partial sugar solubilization (up to 50%) thereby generating lignin oil yields that exceeded the theoretical limit. In contrast, using either Ni/C or Ni on acidified carbon at 200 degrees C resulted in moderate lignin oil yields of ca. 55%, with sugar retention values >90%. Notably, these sugars were amenable to enzymatic digestion, reaching conversions >90% at 96 h. Characterization studies on the lignin oils using two-dimensional heteronuclear single quantum coherence nuclear magnetic resonance and gel permeation chromatrography revealed

  10. Types of pesticides and determination of their residues

    International Nuclear Information System (INIS)

    Kassem, A.R.

    2010-01-01

    The pesticide is any material or component used to protect from pests. Its toxic effect is related to the chemical structure, which can be divided into 3 types : 1- Metal pesticides : Sulphur, cupper, zinc, mercury; 2- Vegetal pesticides : advanced and less toxic to the general health; 3- Synthetic organo pesticides : organo chlorine, organophosphorous, carbamate and pyrethroids. Pesticides in the soil undergo biological dissociation according to their concentration and chemical structure. High concentration of the pesticides in the soil may lead to fertility decrease due to destruction of micro-organisms by the pesticides. Many methods are used to analyze the residues of pesticides in plant or soil : 1- Chromatographic methods : Gas chromatography, gas liquid chromatography and high performance liquid chromatography; 2- Spectroscopy methods : spectrophotometer and mass spectrometer; 3- Isotopic methods : based on tracers technique which is the most sensitive and accurate method and can estimate minor amounts of the pesticides. (author)

  11. The chemistry of subcritical water reactions of a hardwood derived lignin and lignin model compounds with nitrogen, hydrogen, carbon monoxide and carbon dioxide

    Science.gov (United States)

    Hill Bembenic, Meredith A.

    Biofuels, like cellulosic ethanol, may only be cost effective if the lignin byproduct is upgraded to value-added products. However, lignin's inherent aromatic structure and interunit crosslinkages hinder effective conversion. High temperature H2O is considered for lignin conversion, because H2O exhibits unusual properties at higher temperatures (particularly at its supercritical point of 374°C and 3205 psi) including a decreased ion product and a decreased static dielectric constant (similar to those of polar organic solvents at room temperature) such that there is a high solubility for organic compounds, like lignin. Much of the research concerning lignin and supercritical H2O has focused on further decomposition to gases (e.g., H2, CH4, and CO2) where nearly no char formation is expected in the presence of a catalyst. However, the conditions required for supercritical H2O are difficult to maintain, catalysts can be expensive, and gases are not favorable to the current liquid fuel infrastructure. Reactions using Organosolv lignin, subcritical H2O (365°C) and various industrial gases (N2, H2, CO, and CO2 at an initial pressure of 500 psi) for 30 min. were examined to determine both lignin's potential to generate value-added products (e.g., monomer compounds and methanol) and the role (if any) of the H2O and the gases during the reactions. The behavior of H2O at reaction temperature and pressure is expected to be similar to the behavior of supercritical H 2O without the need to maintain supercritical conditions. Different characterization techniques were used for the products collected including primarily GC/FID-TCD of the evolved gases, GC/MS analysis of the organic liquids, solid phase microextraction analysis of the water, and solid state 13C-NMR analysis of the residues. The reactor pressure at temperature was shown to influence the reactivity of the H2O and lignin, and the highest conversions (≈54--62%) were obtained when adding a gas. However, the

  12. Open-pit mining of lignin waste storage

    Directory of Open Access Journals (Sweden)

    А. В. Михайлов

    2017-03-01

    Full Text Available The purpose of this paper is to develop performance criteria for fleet selection in surface mining of lignin as a raw material for factory-made fuel. The East Siberian Biotechnical Plant (ESBP proposes to close the Lignin Waste Storage (LWS at Tulun, Irkutsk Region of Russia. The LWS is a 9.6 ha facility used for the long-term storage of hydrolysis lignin and some fly ash. The project provided whole-year open-pit mining of lignin storage with one mining ledge within 3 years. Productivity – 1500 t/day or 447 000 t/year. Excavated lignin will be stockpile on the Pellet Plant territory for later processing. Part of this closure effort would involve constructing an artificial reservoir on the place of LWS. The objectives of this project were as follows: determine equipment needs and develop optimal procedures for the lignin excavation and transportation. Lignin moving may include site preparation, excavation, transportation and road surfacing. Lignin excavation is conduct by using techniques similar to those used for open-pit mining of peat. For this project, the excavator is the most important piece of equipment required for lignin removal and handling. The mining process consist of excavating the lignin (using Kraneks ЕК-270LC and hauling it to pellet plant via six off-road tractors&semitrailers (John Deere 7730& ISON-8520.

  13. [Residues of organochlorine compounds in plant drugs. 1. Gas chromatographic determination of residues of organochlorine insecticides].

    Science.gov (United States)

    Benecke, R; Thieme, H; Brotka, J

    1986-02-01

    A method for the identification and determination of HCH-and DDT-isomers and their respective metabolites in vegetable drugs is presented. The plant material is extracted with hexane in a Soxhlet apparatus in the presence of silicagel and sodium sulfate. For removing interfering endogenous plant constituents a Celite oleum column cleanup and usually and acetonitrile partitioning to follow are necessary. A mixed stationary phase OV-17/QF-1 has proved effective for the gc separation on packed columns. 3H-ECD is used for detection. For the quantitative determination by using an external standard the peak height measurement is recommended. Recoveries of all insecticides were in the order of 70-105% with coefficients of variation between 6 and 20%. To ensure the results the alkaline treatment and oxidation of extracts are proposed.

  14. Specific determination of ferbam residues in fog-water.

    Science.gov (United States)

    Agarwal, Smita; Aggarwal, Shankar G; Singh, Pahup

    2003-12-23

    A specific method for the determination of a fungicide, i.e. iron(III) dimethyldithiocarbamate (ferbam) in fog-water samples is described. The method is based on the releasing of equivalent amount of iron from the fungicide and subsequently determination by spectrophotometrically or by flame-atomic absorption spectrometrically (flame-AAS). The fungicide was extracted with chloroform/toluene from the samples and digested with nitric acid. For spectrophotometric determination, the solution was then treated with ammonium thiocyanate solution in presence of the surfactants and absorbance was measured at 475 nm. Whereas, the digested solution was directly applied for flame-AAS determination of ferbam. The molar absorptivity in terms of ferbam was determined to be (3.49)x10(4) l mol(-1) cm(-1). The detection limits for spectrophotometric and flame-AAS methods were calculated to be 62 and 111 ppb ferbam (R.S.D. fog-water. The methods have been successfully applied to fog samples collected from agriculture sites of Raipur (central India).

  15. Residual stress in sprayed Ni+5%Al coatings determined by neutron diffraction

    CERN Document Server

    Matejicek, J; Gnaeupel-Herold, T; Prask, H J

    2002-01-01

    Coatings of nickel-based alloys are used in numerous high-performance applications. Their properties and lifetimes are influenced by factors such as residual stress. Neutron diffraction is a powerful tool for nondestructive residual stress determination. In this study, through-thickness residual stress profiles in Ni+5%Al coatings on steel substrates were determined. Two examples of significantly different spraying techniques - plasma spraying and cold spraying - are highlighted. Different stress-generation mechanisms are discussed with respect to process parameters and material properties. (orig.)

  16. The recent development of neutronic techniques for determination of residual stresses

    International Nuclear Information System (INIS)

    Lodini, A.

    2001-01-01

    Neutron diffraction is a well-established non-destructive method for the measurement of residual stress deep inside materials. This paper gives a short overview of the use of neutrons for materials research and measurement techniques. Neutron diffraction has been applied in determining residual stresses in metal matrix composites. Measurement and prediction of residual stress for plastic deformation are presented. More recently, the neutron diffraction technique has also been applied for the determination of plastic strain which results from microstructural defects and leads to peak broadening. Influence of the shot penning treatment on austenitic steel is presented. (author)

  17. determination of cypermethrin residues in gingkgo biloba leaves by ...

    African Journals Online (AJOL)

    A simple and rapid method was described for the determination of cypermethrin in Ginkgo biloba leaves by high performance liquid chromatography (HPLC) with UV detection. A mixture of hexane and acetone (99:1) was used to extract the samples. After the sample cleanup was carried out with a mixture of petroleum ether ...

  18. Structural characterization of lignin from grape stalks (Vitis vinifera L.).

    Science.gov (United States)

    Prozil, Sónia O; Evtuguin, Dmitry V; Silva, Artur M S; Lopes, Luísa P C

    2014-06-18

    The chemical structure of lignin from grape stalks, an abundant waste of winemaking, has been studied. The dioxane lignin was isolated from extractive- and protein-free grape stalks (Vitis vinifera L.) by modified acidolytic procedure and submitted to a structural analysis by wet chemistry (nitrobenzene and permanganate oxidation (PO)) and spectroscopic techniques. The results obtained suggest that grape stalk lignin is an HGS type with molar proportions of p-hydroxyphenyl (H), guaiacyl (G) and syringyl (S) units of 3:71:26. Structural analysis by (1)H and (13)C NMR spectroscopy and PO indicates the predominance of β-O-4' structures (39% mol) in grape stalk lignin together with moderate amounts of β-5', β-β, β-1', 5-5', and 4-O-5' structures. NMR studies also revealed that grape lignin should be structurally associated with tannins. The condensation degree of grape stalks lignin is higher than that of conventional wood lignins and lignins from other agricultural residues.

  19. Validation of a methodology multi-residue for the determination of pesticides residuals in strawberry (fragraria spp.) by gas chromatography

    International Nuclear Information System (INIS)

    Montano Garces, Mauricio; Guerrero Dallos, Jairo Arturo

    2001-01-01

    This study describes the validation of multi-residue analytical methodology for the simultaneous determination of 19 organ chlorine, organophosphorus and organ nitrogen pesticides in strawberry. Pesticides residues were extracted from strawberry samples with ethyl acetate, the extracts were cleaned-up by GPC, the quantitative analysis was carried out by high resolution gas chromatography (GC) with a pulsed splitless injection mode and simultaneous detection by m-ECD and NPD coupled in parallel. The methodology is specific, selective, and accurate and robust the calibration curves in matrix matched analytical standards show linearity over the concentration range of 0.04-5.00 mg/kg with limits of detection and quantitation between 0.007-0.5 mg/kg and 0.01-1.00 mg/kg respectively. The recovery experiments yielding averages between 80-110% for most of the pesticides. The distribution of analyze in the laboratory sample was evaluated and it was found its homogeneity. The methodology was applied in field samples and was mainly found Captan residues below MRL

  20. Fungal demethylation of Kraft lignin.

    Science.gov (United States)

    Zou, Linyou; Ross, Brian M; Hutchison, Leonard J; Christopher, Lew P; Dekker, Robert F H; Malek, Lada

    2015-06-01

    Demethylation of industrial lignin has been for long coveted as a pathway to the production of an abundant natural substitute for fossil-oil derived phenol. In an attempt to possibly identify a novel Kraft lignin-demethylating enzyme, we surveyed a collection of fungi by using selected ion flow tube-mass spectrometry (SIFT-MS). This method readily identifies methanol resulting from lignin demethylation activity. Absidia cylindrospora, and unidentified Cylindrocladium sp. and Aspergillus sp. were shown to metabolize lignin via different pathways, based on the HPLC analysis of lignin fragments. Of these three, Cylindrocladium and Aspergillus were shown to retain most of the lignin intact after 3 weeks in culture, while removing about 40% of the available methoxy groups. Our results demonstrate that after optimization of culture and lignin recovery methods, biological modification of Kraft lignin may be a feasible pathway to obtaining demethylated lignin for further industrial use. Crown Copyright © 2015. Published by Elsevier Inc. All rights reserved.

  1. Comparison of soxhlet and microwave-assisted extractions for the determination of fenitrothion residues in beans.

    Science.gov (United States)

    Diagne, Rokhaya G; Foster, Gregory D; Khan, Shahamat U

    2002-05-22

    White and black "niebe" beans [Vigna unguiculata (L.) Walp] from Senegal were treated with fenitrothion (O,O-dimethyl O-4-nitro-m-tolyl phosphorothioate), and the residues were determined by high-performance liquid chromatography (HPLC) and electron capture gas chromatography (EC-GC). Fenitrothion residues from the beans were extracted by Soxhlet extraction (SE) and microwave-assisted extraction (MAE). A column cleanup procedure was used to remove the coextractives in the extract before HPLC and EC-GC analyses. The overall mean recoveries of fenitrothion residues in the 0.19-1.90 microg/kg fortification range determined from extracts obtained by SE and MAE were 88.4 and 89.8%, respectively, with respective relative standard deviations of <4%. The results show that MAE is a viable alternative to the commonly used SE for the determination of fenitrothion residues in beans.

  2. Effects of N-ammonoxidized lignins amendment on N availability and soil fertility: An incubation study

    Science.gov (United States)

    María De la Rosa, José; López-Martín, María; Liebner, Falk; Knicker, Heike

    2013-04-01

    The shift towards a biobased economy will probably generate the application of bioenergy by-products and charred residues to the soil as either amendments or fertilizers. The process of ammonoxidation (application of gaseous oxygen and aqueous ammonia under ambient pressure breaks down aromatic lignin moieties and introduces N in the form of urea, amides and amines), converts lignin, a major by-product of the pulp and paper industry, or other ligneous materials into artificial humic matter (N-lignin). The use of N-ammonoxidized lignin as soil improvers is in theory an economically viable solution, especially interesting for agricultural areas of Mediterranean countries, in which additional factors such as water shortage and fires contribute to declining N availability by lowering nutrient diffusion, litter input or sequestration of N in charred structures. However, limited research has been done to determine how this will influence C and N dynamics and soil fertility. Therefore we performed pot experiments in which a perennial ryegrass (Lolium perenne L.) was grown on a typical Andalusian soil (chromic Luvisol) after amendment of N-lignins highly enriched in 15N (Sarkanda and Indulin ammonoxidized lignins) for 75 days. For comparison, the incubation was also carried out on soils fertilized with 15NO3 and unfertilized (control). The application of ammonoxidized lignins altered the pH and electrical conductivity of the soil. At higher concentrations a retardation of seed germination was evidenced, an observation that needs further considerations before N-enriched technical lignins can be applied in agriculture. After 75 days, the plant shoots from the pots amended with15N-Indulin and 15N-Sarkanda accumulated 8% and 20%, respectively of the initial 15N (15N0). The N was efficiently sequestered from fast release or leaching and most of 15N0 remained in the soil (64%) in the 15N-Indulin pots. In contrast, the 15N-Sarkanda pots showed a lower efficiency in the N

  3. Liquid chromatographic determination of tetracycline residues in animal feeds.

    Science.gov (United States)

    Martinez, E E; Shimoda, W

    1988-01-01

    A liquid chromatographic method for the multiresidue determination of tetracyclines (TCs) in feeds is described. The levels of quantitation were 10 ppm each for tetracycline-HCl (TC), oxytetracycline (OTC), and chlortetracycline-HCl (CTC); the detection limit was 40 ppb for each. The calibration curves were linear between 2.5 and 100 ppm. The procedure involved double extraction with pH 2.0 and pH 4.5 McIlvain buffers, cleanup on a Sephadex LH-20 column, separation on a Nova-Pak C18 column, and detection at 370 nm. Recoveries of 10 micrograms/g of each TC in multiresidue feed samples ranged from 55.8 to 75.5% for OTC, 71.6 to 100% for TC, and 22.4 to 60.6% for CTC. The identities of the TCs were confirmed by thin layer chromatography.

  4. Liquid chromatographic determination of tetracycline residues in meat and fish.

    Science.gov (United States)

    Onji, Y; Uno, M; Tanigawa, K

    1984-01-01

    A simple and rapid method was developed for quantitative determination of common tetracyclines, such as oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC), in meat and fish. Tetracyclines were extracted with aqueous HCl, and then centrifuged. The supernate was applied to an Amberlite XAD-2 column, which was washed with water and eluted with methanol. The eluate was concentrated to about 0.5 mL under vacuum at 35 degrees C, and then measured by liquid chromatography and UV detection. Two analytical columns were used for confirmation. The average recoveries of OTC, TC, and CTC from meat and fish fortified at 1, 1, and 3 ppm were 82.6, 81.5, and 67.0% respectively.

  5. Role of paramagnetic polyconjugated clusters in lignin antioxidant activity (in vitro)

    International Nuclear Information System (INIS)

    Dizhbite, T; Ponomarenko, J; Andersone, A; Dobele, G; Lauberts, M; Krasilnikova, J; Telysheva, G; Mironova-Ulmane, N

    2012-01-01

    Using physico-chemical methods (EPR, SEC, Py-GC/MS and UV/VIS spectroscopy) and wet chemical analysis, the characteristics of 6 hardwood lignins in terms of functionality, molecular weight and composition of lignin substructures were determined and considered together with the results of DPPH., ABTS. + and O 2 . − antioxidant assays with the aim to understand the relationships governing antioxidant properties of lignin. The strong positive linear correlation between lignin antioxidant capacity in the three assays used and the extent of conjugation of paramagnetic polyconjugated clusters in lignin macromolecules was found. The biological activity of the most active alkaline lignins was assessed by in vitro experiment with human blood.

  6. Comparison of thin layer chromatographic and gas chromatographic determination of propoxur residues in a cocoa ecosystem

    International Nuclear Information System (INIS)

    Yeboah, P.O.; Lowor, S.; Akpabli, C.K.

    2005-01-01

    The fate of propoxur in a cocoa ecosystem has been studied using thin layer chromatographic (TLC) and gas chromatographic (GC) methods. Residues of propoxur as determined by both TLC and GC were not significantly different. TLC analysis of propoxur residues in soil, cocoa leaves and pods did not require any rigorous cleanup since residues measured from cleaned extracts and without cleanup were not significantly different. The residue levels of propoxur in the soil were found to decrease rapidly and, by the 21st day, none was detected in the topsoil (0-15 cm). Evidence of leaching of propoxur residues in the soil has also been demonstrated. The amount left in the top soil after the first seven days were 27%, 23% and 24% of the initial one as determined by the TLC without cleanup, TLC with cleanup and GLC, respectively. No propoxur residue was detected in topsoil 21 days after spraying. About 38% of pesticides detected on the cocoa pod on the day of treatment remained on the pod seven days after treatment. The residue detected on the leaves on the day of treatment was higher than that in or on the soil. This decreased rapidly to 1.7% in 21 days compared to 16% for the soil and 23% for the pod. (author)

  7. Residual stress determination of rail tread using a laser ultrasonic technique

    International Nuclear Information System (INIS)

    Wang, Jing; Feng, Qibo

    2015-01-01

    A non-destructive method for measuring the residual stress on rail tread that uses a laser-generated ultrasonic technique is proposed. The residual stress distribution of different parts on both the new rail and used rail were examined. The surface acoustic waves (SAWs) are excited by a scanning line laser and detected by a laser ultrasonic detection system. A digital correlation method was used for calculating the changes in velocity of SAWs, which reflects the stress distribution. A wavelet de-noising technique and a least square fit were used for signal processing to improve the measurement accuracy. The effects of ultrasonic propagation distance and surface roughness on the determination of residual stress were analyzed and simulated. Results from the study demonstrate that the stress distribution results are accordant with the practical situation, and the laser-generated SAWs technique is a promising tool for the determination of residual stress in the railway inspection and other industrial testing fields. (paper)

  8. Type I and type II residual stress in iron meteorites determined by neutron diffraction measurements

    Science.gov (United States)

    Caporali, Stefano; Pratesi, Giovanni; Kabra, Saurabh; Grazzi, Francesco

    2018-04-01

    In this work we present a preliminary investigation by means of neutron diffraction experiment to determine the residual stress state in three different iron meteorites (Chinga, Sikhote Alin and Nantan). Because of the very peculiar microstructural characteristic of this class of samples, all the systematic effects related to the measuring procedure - such as crystallite size and composition - were taken into account and a clear differentiation in the statistical distribution of residual stress in coarse and fine grained meteorites were highlighted. Moreover, the residual stress state was statistically analysed in three orthogonal directions finding evidence of the existence of both type I and type II residual stress components. Finally, the application of von Mises approach allowed to determine the distribution of type II stress.

  9. Specific features of the determination of residual stresses in materials by diffraction techniques

    Science.gov (United States)

    Gorkunov, E. S.; Zadvorkin, S. M.; Goruleva, L. S.

    2017-12-01

    Residual stresses arising in separate machine parts and structural components during production and use to a large extent govern their lifetime. In this connection, the development and improvement of nondestructive methods for the determination of residual stresses is an important task for nondestructive testing. Standards regulate only the determination of macroscopic stresses, and in practice these stresses are most often determined with the application of the sin2ψ method. This paper, using quenched structural steels as an example, compares the results of residual stress determination by the sin2ψ method with those obtained by the method based on the analysis of the diffraction line profile as dependent on the value of the irradiated volume. It is demonstrated that, as the irradiated volume decreases, the value of residual stresses determined by the sin2ψ method may vary considerably, up to the change of the sign. For a more complete characteristic of residual stresses it is proposed to use, besides the determination of macrostresses by the shift of the diffraction lines, the value of microscopic stresses calculated from the line profile analysis.

  10. Evidence for lignin oxidation by the giant panda fecal microbiome.

    Directory of Open Access Journals (Sweden)

    Wei Fang

    Full Text Available The digestion of lignin and lignin-related phenolic compounds from bamboo by giant pandas has puzzled scientists because of the lack of lignin-degrading genes in the genome of the bamboo-feeding animals. We constructed a 16S rRNA gene library from the microorganisms derived from the giant panda feces to identify the possibility for the presence of potential lignin-degrading bacteria. Phylogenetic analysis showed that the phylotypes of the intestinal bacteria were affiliated with the phyla Proteobacteria (53% and Firmicutes (47%. Two phylotypes were affiliated with the known lignin-degrading bacterium Pseudomonas putida and the mangrove forest bacteria. To test the hypothesis that microbes in the giant panda gut help degrade lignin, a metagenomic library of the intestinal bacteria was constructed and screened for clones that contained genes encoding laccase, a lignin-degrading related enzyme. A multicopper oxidase gene, designated as lac51, was identified from a metagenomic clone. Sequence analysis and copper content determination indicated that Lac51 is a laccase rather than a metallo-oxidase and may work outside its original host cell because it has a TAT-type signal peptide and a transmembrane segment at its N-terminus. Lac51 oxidizes a variety of lignin-related phenolic compounds, including syringaldazine, 2,6-dimethoxyphenol, ferulic acid, veratryl alcohol, guaiacol, and sinapinic acid at conditions that simulate the physiologic environment in giant panda intestines. Furthermore, in the presence of 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid (ABTS, syringic acid, or ferulic acid as mediators, the oxidative ability of Lac51 on lignin was promoted. The absorbance of lignin at 445 nm decreased to 36% for ABTS, 51% for syringic acid, and 51% for ferulic acid after incubation for 10 h. Our findings demonstrate that the intestinal bacteria of giant pandas may facilitate the oxidation of lignin moieties, thereby clarifying the digestion

  11. Direct rate assessment of laccase catalysed radical formation in lignin by electron paramagnetic resonance spectroscopy

    DEFF Research Database (Denmark)

    Munk, Line; Andersen, Mogens Larsen; Meyer, Anne S.

    2017-01-01

    Laccases (EC 1.10.3.2) catalyse removal of an electron and a proton from phenolic hydroxyl groups, including phenolic hydroxyls in lignins, to form phenoxy radicals during reduction of O2. We employed electron paramagnetic resonance spectroscopy (EPR) for real time measurement of such catalytic...... to suspensions of the individual lignin samples produced immediate time and enzyme dose dependent increases in intensity in the EPR signal with g-values in the range 2.0047–2.0050 allowing a direct quantitative monitoring of the radical formation and thus allowed laccase enzyme kinetics assessment on lignin...... formation than the Tv laccase on all three types of lignin substrates. When comparing the equal laccase dose rates on the three lignin substrates the enzymatic radical formation rate on the wheat straw lignin residue was consistently higher than those of the organosolv lignins. The pH-temperature optimum...

  12. Properties and Possible Applications for Lignin Streams Obtained from Rice Straw Processing

    DEFF Research Database (Denmark)

    Mussatto, Solange I.

    This study aimed to evaluate the chemical and physical properties of lignin streams recovered from rice straw processing and to study the extraction of antioxidant phenolic compounds from these materials. The evaluated samples included two different cellulignin fermentation residues (FR’s) and an......This study aimed to evaluate the chemical and physical properties of lignin streams recovered from rice straw processing and to study the extraction of antioxidant phenolic compounds from these materials. The evaluated samples included two different cellulignin fermentation residues (FR......’s) and an acid-precipitated lignin from alkaline-deacetylated black liquor (DBLL). For comparison, a standard lignin sample (Kraft lignin, from Sigma-Aldrich) was also assayed. Besides providing a better understanding about such materials, the obtained results made also possible to propose some potential...... applications for such lignin samples....

  13. Hydroxide catalysts for lignin depolymerization

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T; Biddy, Mary J.; Kruger, Jacob S.; Chmely, Stephen C.; Sturgeon, Matthew

    2017-10-17

    Solid base catalysts and their use for the base-catalyzed depolymerization (BCD) of lignin to compounds such as aromatics are presented herein. Exemplary catalysts include layered double hydroxides (LDHs) as recyclable, heterogeneous catalysts for BCD of lignin.

  14. Hydroxide catalysts for lignin depolymerization

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T.; Biddy, Mary J.; Chmely, Stephen C.; Sturgeon, Matthew

    2017-04-25

    Solid base catalysts and their use for the base-catalyzed depolymerization (BCD) of lignin to compounds such as aromatics are presented herein. Exemplary catalysts include layered double hydroxides (LDHs) as recyclable, heterogeneous catalysts for BCD of lignin.

  15. Determination of properties of clean coal technology post-process residue

    Directory of Open Access Journals (Sweden)

    Agnieszka Klupa

    2016-01-01

    Full Text Available This article presents the possibilities of using modern measuring devices to determine the properties of process residues (Polish acronym: UPP. UPP was taken from the combustion process from a power plant in Silesia. Determining the properties of UPP is the basis for making decisions about its practical application, for example, as a raw material to obtain useful products such as: pozzolan, cenosphere or zeolite, for which there is demand. The development of advanced technology and science has given rise to modern and precise research tools that contribute to the development of appropriate methods to assess the properties of post-process residue. For this study the following were used: scanning electron microscope with EDS microanalysis and an analyzer for particle size-, shape- and number- analysis. The study conducted confirms the effectiveness of SEM analysis to determine the properties of post-process residue from Clean Coal Technologies (CCT. The results obtained are an introduction to further research on the determination of properties of CCT post-process residue. Research to determine the properties of CCT post-process residue only began relatively recently.

  16. Lignin-based polyurethane materials

    OpenAIRE

    Cateto, C.A.; Barreiro, M.F.; Rodrigues, A.E.; Belgacem, M.N.

    2008-01-01

    Four technical lignins (Alcell, Indulin AT, Sarkanda and Curan 27-11P) were used as macromonomers in the synthesis of polyurethane materials following two global approaches. In the first one Alcell and Indulin AT lignins were used directly as co-monomers in combination with a linear polycaprolactone (PCL) in order to produce polyurethane elastomers where lignin content varied between 10 and 25% (w/w) with respect to polyol mixture (PCL+lignin). The thermomechanical properties o...

  17. Determination of Profenofos Pesticidal Residue in Lettuce (Lactuca sativa L. by Gas Chromatographic Method

    Directory of Open Access Journals (Sweden)

    Yohannes Alen

    2015-05-01

    Full Text Available The determination of profenofos pesticidal residue in the lettuce (Lactuca sativa L. by using gas chromatography using flame photometric detector (FPD had been investigated. The lettuce was collected from Padang Luar area, Agam distric, West Sumatera. Sample for determination of profenofos residue divided into three groups: unwashed (A, washed with water (B, and washed with detergent (C. Maceration with sonication was used for the extraction using ethylacetateas a solvent. The results showed that profenofos pesticide residue in sample A, B and C were 0.204, 0.080 and 0.061 ppm, respectively. These profenofos pesticidal residue are over than the Maximum Residue Limits (MRL that established by The Japan Food Chemical Research Foundation (0.05 ppm even though World Health Organization (WHO has not established Maximum Residue Limits (MRL profenofos on lettuce. Based on the statistical analysis one-way method (Anova using SPSS 20.0 showed that there was a significant concentrations difference between lettuce A from lettuce B and lettuce C with p < 0.05.

  18. Prediction of detailed enzyme functions and identification of specificity determining residues by random forests.

    Directory of Open Access Journals (Sweden)

    Chioko Nagao

    Full Text Available Determining enzyme functions is essential for a thorough understanding of cellular processes. Although many prediction methods have been developed, it remains a significant challenge to predict enzyme functions at the fourth-digit level of the Enzyme Commission numbers. Functional specificity of enzymes often changes drastically by mutations of a small number of residues and therefore, information about these critical residues can potentially help discriminate detailed functions. However, because these residues must be identified by mutagenesis experiments, the available information is limited, and the lack of experimentally verified specificity determining residues (SDRs has hindered the development of detailed function prediction methods and computational identification of SDRs. Here we present a novel method for predicting enzyme functions by random forests, EFPrf, along with a set of putative SDRs, the random forests derived SDRs (rf-SDRs. EFPrf consists of a set of binary predictors for enzymes in each CATH superfamily and the rf-SDRs are the residue positions corresponding to the most highly contributing attributes obtained from each predictor. EFPrf showed a precision of 0.98 and a recall of 0.89 in a cross-validated benchmark assessment. The rf-SDRs included many residues, whose importance for specificity had been validated experimentally. The analysis of the rf-SDRs revealed both a general tendency that functionally diverged superfamilies tend to include more active site residues in their rf-SDRs than in less diverged superfamilies, and superfamily-specific conservation patterns of each functional residue. EFPrf and the rf-SDRs will be an effective tool for annotating enzyme functions and for understanding how enzyme functions have diverged within each superfamily.

  19. Prediction of Detailed Enzyme Functions and Identification of Specificity Determining Residues by Random Forests

    Science.gov (United States)

    Nagao, Chioko; Nagano, Nozomi; Mizuguchi, Kenji

    2014-01-01

    Determining enzyme functions is essential for a thorough understanding of cellular processes. Although many prediction methods have been developed, it remains a significant challenge to predict enzyme functions at the fourth-digit level of the Enzyme Commission numbers. Functional specificity of enzymes often changes drastically by mutations of a small number of residues and therefore, information about these critical residues can potentially help discriminate detailed functions. However, because these residues must be identified by mutagenesis experiments, the available information is limited, and the lack of experimentally verified specificity determining residues (SDRs) has hindered the development of detailed function prediction methods and computational identification of SDRs. Here we present a novel method for predicting enzyme functions by random forests, EFPrf, along with a set of putative SDRs, the random forests derived SDRs (rf-SDRs). EFPrf consists of a set of binary predictors for enzymes in each CATH superfamily and the rf-SDRs are the residue positions corresponding to the most highly contributing attributes obtained from each predictor. EFPrf showed a precision of 0.98 and a recall of 0.89 in a cross-validated benchmark assessment. The rf-SDRs included many residues, whose importance for specificity had been validated experimentally. The analysis of the rf-SDRs revealed both a general tendency that functionally diverged superfamilies tend to include more active site residues in their rf-SDRs than in less diverged superfamilies, and superfamily-specific conservation patterns of each functional residue. EFPrf and the rf-SDRs will be an effective tool for annotating enzyme functions and for understanding how enzyme functions have diverged within each superfamily. PMID:24416252

  20. Enzymatic Biodegradation of Lignin-Cellulose Complex in Plant Origin Material

    OpenAIRE

    Regina VARNAITĖ; Vita RAUDONIENĖ; Danguolė BRIDŽIUVIENĖ

    2011-01-01

    Lignin and cellulose are chemically hardly destructible complex polymeric materials of organic origin. The main enzymes of fungi taking part in lignin degradation are phenoloxidases: lignin peroxidase, Mn-peroxidase and lacase, while in cellulose - endoglucanase. The aim of the investigation was to define the degradation of lignin and cellulose in the later stages of fungi cultivation, to determine the activity of phenoloxidases and endoglucanase and their abilities to degrade this complex. I...

  1. Comparison studies on soda lignin and soda-anthraquinone lignin

    International Nuclear Information System (INIS)

    Ibrahim, M.N.M; Yusof, N.N.M.; Hashim, A.

    2007-01-01

    Soda lignin and soda anthraquinone lignin were compared in this study. The physico-chemical properties and structural features of the isolated lignin were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Ultraviolet (UV), ash test, Carbon-Hydrogen-Nitrogen (CHN) analyzer, Nuclear Magnetic Resonance ( 13 C-NMR) and High Performance Liquid Chromatography (HPLC). Nitrobenzene oxidation was performed on these two types of lignin especially for the HPLC analysis. Based on the CHN, 13 C-NMR and UV results there were no significant differences between soda lignin and soda anthraquinone lignin. The FTIR results also showed that there were no significant differences in terms of functional groups that exist in both lignins. (author)

  2. Chapter 16: Lignin Visualization: Advanced Microscopy Techniques for Lignin Characterization

    Energy Technology Data Exchange (ETDEWEB)

    Zeng, Yining [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Donohoe, Bryon S [National Renewable Energy Laboratory (NREL), Golden, CO (United States)

    2018-04-03

    Visualization of lignin in plant cell walls, with both spatial and chemical resolution, is emerging as an important tool to understand lignin's role in the plant cell wall's nanoscale architecture and to understand and design processes intended to modify the lignin. As such, this chapter reviews recent advances in advanced imaging methods with respect to lignin in plant cell walls. This review focuses on the importance of lignin detection and localization for studies in both plant biology and biotechnology. Challenges going forward to identify and delineate lignin from other plant cell wall components and to quantitatively analyze lignin in whole cell walls from native plant tissue and treated biomass are also discussed.

  3. NMR characterization of lignins isolated from fruit and vegetable insoluble dietary fiber.

    Science.gov (United States)

    Bunzel, Mirko; Ralph, John

    2006-10-18

    Compositional information for lignins in food is rare and concentrated on cereal grains and brans. As lignins are suspected to have important health roles in the dietary fiber complex, the confusing current information derived from nonspecific lignin determination methods needs to be augmented by diagnostic structural studies. For this study, lignin fractions were isolated from kiwi, pear, rhubarb, and, for comparison, wheat bran insoluble dietary fiber. Clean pear and kiwi lignin isolates allowed for substantive structural profiling, but it is suggested that the significance of lignin in wheat has been overestimated by reliance on nonspecific analytical methods. Volume integration of NMR contours in two-dimensional (13)C-(1)H correlation spectra shows that pear and wheat lignins have comparable guaiacyl and syringyl contributions and that kiwi lignins are particularly guaiacyl-rich (approximately 94% guaiacyl) and suggest that rhubarb lignins, which could not be isolated from contaminating materials, are as syringyl-rich (approximately 96% syringyl) as lignins from any known natural or transgenic fiber source. Typical lignin structures, including those newly NMR-validated (glycerols, spirodienones, and dibenzodioxocins), and resinols implicated as possible mammalian lignan precursors in the gut are demonstrated via their NMR correlation spectra in the fruit and vegetable samples. A novel putative benzodioxane structure appears to be associated with the kiwi lignin. It is concluded that the fruits and vegetables examined contain authentic lignins and that the detailed structural analysis exposes limitations of currently accepted analytical methods.

  4. NMR of lignins

    Science.gov (United States)

    John Ralph; Larry L. Landucci

    2010-01-01

    This chapter will consider the basic aspects and findings of several forms of NMR spectroscopy, including separate discussions of proton, carbon, heteronuclear, and multidimensional NMR. Enhanced focus will be on 13C NMR, because of its qualitative and quantitative importance, followed by NMR’s contributions to our understanding of lignin...

  5. DETERMINATION OF RESIDUAL STRESS DISTRIBUTION IN HIGH STRENGTH ALUMINUM ALLOY AFTER EDM

    Directory of Open Access Journals (Sweden)

    Zubair Butt

    2017-03-01

    Full Text Available Thermal energy produced by discrete and random electric sparks in electric discharge machining (EDM melts surface material. A portion of this molten material is removed and the remaining material resolidified by rapid cooling in a hydrocarbon oil. The effect of repeated heating and cooling of the surface and sub surface material with complex temperature gradient results residual stresses in machined part. The aim of this investigation is to determine the distribution of residual stresses in the depth of machined material with respect to discharge current, most important electric parameter during EDM. It is well known that surface finish is dependent on discharge current. Therefore, investigations were carried out for smaller discharge current levels i.e. 3, 6, 9, 12 ampere. Hole-drill strain gauge method is used for the determination of residual stresses in the depth of material. For comparison purpose, residual stresses are also determined for conventionally turned specimens. This study provided quantitative analysis of the residual stresses for various discharge current in EDM which is a key parameter in deciding the service life of material.

  6. The gravimetric method for the determination of residual moisture in freeze-dried biological products.

    Science.gov (United States)

    May, J C; Wheeler, R M; Grim, E

    1989-06-01

    The gravimetric test for the determination of residual moisture in freeze-dried biological products performed in a humidity- and temperature-controlled room with the use of scrupulous gravimetric analytical technique can be used to accurately determine residual moisture in freeze-dried biological products such as antihemophilic factor (human) or honey bee venom allergenic extract. This method determines the first water of hydration of sodium tartrate dihydrate (7.93%) to within 1.3% of the calculated value with a relative standard deviation of 0.3% for 10 replicates. For this gravimetric procedure, freeze-dried samples containing from 1.12 to 4.4% residual moisture had relative standard deviations ranging from 3.6 to 9.1%. Samples containing less than 1.0% residual moisture by the gravimetric method such as intravenous immune globulin and antihemophilic factor (human) had relative standard deviations ranging from 16.7 to 47.0%. Relative standard deviations for residual moisture tests performed on comparable samples by the Karl Fischer and thermogravimetric methods showed similar variability.

  7. The degradation of kraft lignin during hydrothermal treatment for phenolics

    Directory of Open Access Journals (Sweden)

    Tang Kai

    2015-09-01

    Full Text Available Kraft lignin was hydrothermally depolymerized at low temperature/short time in water for producing value-added phenolics. The effects of residence time (15, 60 min and reaction temperature (130, 180, 230ºC on yields of oils and phenolic compounds were studied in detail. Total oil yield was found to range between 7% and 10%. The compositions of oils were analyzed by GC-MS to confirm the main compound to be guaiacol (2-methoxy phenol in the range of 12–55% of oil depending on different reaction conditions. The most interesting was the finding that maximum value of total oil yield (10% of kraft lignin and guaiacol amount (55% of oil was obtained at 130ºC/15, 60 min which is a low reaction temperature/short time, while the residual kraft lignins were analyzed by FTIR with respect to the conversion mechanism of kraft lignin by this process.

  8. Residual monomer content determination in some acrylic denture base materials and possibilities of its reduction

    Directory of Open Access Journals (Sweden)

    Kostić Milena

    2009-01-01

    Full Text Available Background/Aim. Polymethyl methacrylate is used for producing a denture basis. It is a material made by the polymerization process of methyl methacrylate. Despite of the polymerization type, there is a certain amount of free methyl methacrylate (residual monomer incorporated in the denture, which can cause irritation of the oral mucosa. The aim of this study was to determine the amount of residual monomer in four different denture base acrylic resins by liquid chromatography and the possibility of its reduction. Methods. After the polymerization, a postpolymerization treatment was performed in three different ways: in boiling water for thirty minutes, with 500 W microwaves for three minutes and in steam bath at 22º C for one to thirty days. Results. The obtained results showed that the amount of residual monomer is significantly higher in cold polymerizing acrylates (9.1-11%. The amount of residual monomer after hot polymerization was in the tolerance range (0.59- 0.86%. Conclusion. The obtained results denote a low content of residual monomer in the samples which have undergone postpolymerization treatment. A lower percent of residual monomer is established in samples undergone a hot polymerization.

  9. An Image Segmentation Based on a Genetic Algorithm for Determining Soil Coverage by Crop Residues

    Science.gov (United States)

    Ribeiro, Angela; Ranz, Juan; Burgos-Artizzu, Xavier P.; Pajares, Gonzalo; Sanchez del Arco, Maria J.; Navarrete, Luis

    2011-01-01

    Determination of the soil coverage by crop residues after ploughing is a fundamental element of Conservation Agriculture. This paper presents the application of genetic algorithms employed during the fine tuning of the segmentation process of a digital image with the aim of automatically quantifying the residue coverage. In other words, the objective is to achieve a segmentation that would permit the discrimination of the texture of the residue so that the output of the segmentation process is a binary image in which residue zones are isolated from the rest. The RGB images used come from a sample of images in which sections of terrain were photographed with a conventional camera positioned in zenith orientation atop a tripod. The images were taken outdoors under uncontrolled lighting conditions. Up to 92% similarity was achieved between the images obtained by the segmentation process proposed in this paper and the templates made by an elaborate manual tracing process. In addition to the proposed segmentation procedure and the fine tuning procedure that was developed, a global quantification of the soil coverage by residues for the sampled area was achieved that differed by only 0.85% from the quantification obtained using template images. Moreover, the proposed method does not depend on the type of residue present in the image. The study was conducted at the experimental farm “El Encín” in Alcalá de Henares (Madrid, Spain). PMID:22163966

  10. LC-MS/MS determination of pesticide residues in fruits and vegetables.

    Science.gov (United States)

    Stachniuk, Anna; Szmagara, Agnieszka; Czeczko, Renata; Fornal, Emilia

    2017-07-03

    The aim of the research is to evaluate pesticide residue contamination of fresh and frozen fruits and vegetables, agricultural raw material, purchased from Polish farmers for production of frozen fruits and vegetables, and the estimation of the multiresidue method effectiveness expressed as the proportion of pesticides detected in food samples to the total number of pesticides analyzed by multiresidue methods. A total of 144 samples (of black currants, red currants, raspberries, cherries, strawberries, blackberries, cauliflowers and broccoli) were analyzed using LC-MS/MS method for the determination of 60 pesticides. QuEChERS extraction, matrix-matched calibration and dynamic multiple reaction monitoring method were used. Residues of 15 compounds, mainly fungicides and insecticides, were detected in 46 samples. The percentage of samples with residues above the maximum residue levels (MRL) was 15%, whereas samples with residues below MRL were 17%. A total of 13 samples contained more than one pesticide residue. Pesticide residues were detected most often in samples of black currants (50%), broccoli (36.4%), raspberries (29%) and red currants (21.8%). The most frequently detected pesticides were carbendazim and acetamiprid. The proportion of pesticides detected during our study to the total number of analyzed pesticides amounted to 25%. It was compared to literature findings. For three fourth of multiresidue methods, the proportion was below 50% for methods developed for the analysis of less than 100 pesticides, and below 30% for methods developed for the analysis of more than 100 pesticides. It appears that a lot of efforts and means is lost on pesticides never or rarely detected in examined samples. The workload and cost effectiveness of the development and application of multiresidue methods along with the range of pesticides covered by the method should be carefully and thoroughly considered anytime when a new method or workflow is developed. Including non

  11. Wheat straw lignin degradation induction to aromatics by por Aspergillus spp. and Penicillium chrysogenum

    Directory of Open Access Journals (Sweden)

    Baltierra-Trejo Eduardo

    2016-02-01

    Full Text Available Wheat straw is a recalcitrant agricultural waste; incineration of this material represents an important environmental impact. Different reports have been made regarding the use of the structural components of wheat straw, i.e. cellulose, hemicellulose and lignin; however, lignin has been less exploited because it is largely considered the recalcitrant part. Residual wheat straw lignin (REWSLI has a potential biotech-nological value if depolymerization is attained to produce aromatics. Ligninolytic mitosporic fungus represent an alternative where very little research has been done, even though they are capable of depol-ymerize REWSLI in simple nutritional conditions in relatively short periods, when compared to basidio-mycetes. The aim of this research was to study the depolymerization activity of Aspergillus spp and Penicillium spp on semipurified REWSLI as the sole carbon source to produce aromatics. The depoly-merization capacity was determined by the activity of the laccase, lignin peroxidase and manganese peroxidase enzymes. The generated aromatics derived from the REWSLI depolymerization were identi-fied by gas chromatography. Obtained results revealed that Penicillium chrysogenum depolymerized the lignin material by 34.8% during the 28-day experimentation period. Laccase activity showed the largest activity with 111 U L-1 in a seven-day period, this enzyme induction was detected in a smaller period than that required by basidiomycetes to induce it. Moreover, the enzymatic activity was produced with-out the addition of an extra carbon source as metabolic inductor. Aspergillus spp and Penicillium spp generated guaiacol, vanillin, and hydroxybenzoic, vanillinic, syringic and ferulic acid with a maximum weekly production of 3.5, 3.3, 3.2, 3.3, 10.1 and 21.9 mg mL-1, respectively.

  12. Catalytic hydrotreatment of pyrolytic lignins to give alkylphenolics and aromatics using a supported Ru catalyst

    NARCIS (Netherlands)

    Kloekhorst, Arjan; Wildschut, Jelle; Heeres, Hero Jan

    2014-01-01

    The catalytic hydrotreatment of two pyrolytic lignins (pine and forestry residue), obtained from the corresponding fast pyrolysis oils, and organosolv Alcell lignin as a benchmark was explored in a batch set-up using Ru/C as the catalyst (400 degrees C, 4 h, 100 bar initial H-2 pressure). The

  13. Chemical and spectroscopic analysis of lignin in isolated flax fibers.

    Science.gov (United States)

    Morrison, W H; Himmelsbach, D S; Akin, D E; Evans, J D

    2003-04-23

    The chemistry of pure flax fibers, free of contaminating nonfiber components, has not been determined. Fibers from the center sections of the stem of seed and fiber flax (Linum usitatissium L.), which had been retted after soaking in water and removal of the epidermis by hand, underwent chemical and spectroscopic analysis. Wet chemical analysis showed only trace indications of aromatics and no long chain fatty acids or alcohols in fibers. Pyrolysis mass spectroscopy (PyMS) and pyrolysis gas chromatography mass spectrometry (PyGCMS) showed only trace amounts of aromatic constituents that could be attributed to the presence of lignin. Mid-infrared (Mid-IR) and Raman spectroscopy of these fibers showed no aromatic compounds present. This study suggests that earlier work reporting the presence of lignin ranging from 1 to 4% may be the result of residual shive or epidermis/cuticle material remaining after the retting process which may be responsible for the favorable properties desired by the composites industry.

  14. [Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

    Science.gov (United States)

    Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

    2014-05-01

    A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

  15. Residual stress determination of direct metal laser sintered (DMLS) inconel specimens and parts

    Energy Technology Data Exchange (ETDEWEB)

    Watkins, Thomas R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Unocic, Kinga A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Maziasz, Philip J. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bunn, Jeffrey R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Fancher, Christopher M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Peralta, Alonso [Honeywell Aerospace, Phoenix, AZ (United States); Sundarraj, Suresh [Honeywell Aerospace, Phoenix, AZ (United States); Neumann, James [Honeywell Aerospace, Phoenix, AZ (United States)

    2018-01-01

    Residual stress determinations and microstructural studies were performed on a series of Inconel 718Plus prisms built using Direct Metal Laser Sintering (DMLS) at Honeywell Aerospace (hereafter also referred to as Honeywell). The results are being used to validate and improve existing models at Honeywell, and ultimately will expedite the implementation of DMLS throughout various industrial sectors (automotive, biomedical, etc.).

  16. Focus Energy Determination of Mining Microseisms Using Residual Seismic Wave Attenuation in Deep Coal Mining

    Directory of Open Access Journals (Sweden)

    Mingwei Zhang

    2018-01-01

    Full Text Available Based on the energy attenuation characteristics of residual wave in deep rock, a method was developed to determine the microseismic focus energy. Differential energy loss in infinitesimal spreading distance is logically deduced, upon which energy attenuation equation was established. With a logarithmic transformation, a linear relation of the residual seismic energy with distance is formulated. Its intercept was used to determine the microseismic focus energy. The result is compared with that determined by the energy density method. The reliability of the determined focus energy and the impact of the built-in velocity threshold on the residual wave energy computation are discussed. Meanwhile, the energy absorption coefficient used for representing the absorption characteristics of the rock medium in the mining region under study is also clarified. Key findings show that the microseismic focus energy confirmed by the residual wave attenuation is reliable. The result’s accuracy is quite high, especially for the events in deep rock with great homogeneity. The developed focus energy computation method is closely dependent on the integrity of waveform, accuracy of repositioning, and reliability of effective components extraction. The new method has been shown to be effective and practical.

  17. Determination of 86 Pesticide Residues in Leafy Vegetables using gas Chromatography Mass Spectrometry

    OpenAIRE

    , M. T. Selim; , I. Al-Dossary

    2016-01-01

    A multiresidue method is described for detection and determination of 86 compounds of pesticide residues which commonly used in the pest control programs for crop protection. Good sensitivity and selectivity of the method are obtained with limits of quantiŞcation 0.01 mg/kg in almost all cases. The method was applied very satisfactorily to routine analysis as a complement to traditional GC-MS method and Şnally, limit of detection were also 10-20 times lower than maximum residue levels (MRL) e...

  18. SDR: a database of predicted specificity-determining residues in proteins.

    Science.gov (United States)

    Donald, Jason E; Shakhnovich, Eugene I

    2009-01-01

    The specificity-determining residue database (SDR database) presents residue positions where mutations are predicted to have changed protein function in large protein families. Because the database pre-calculates predictions on existing protein sequence alignments, users can quickly find the predictions by selecting the appropriate protein family or searching by protein sequence. Predictions can be used to guide mutagenesis or to gain a better understanding of specificity changes in a protein family. The database is available on the web at http://paradox.harvard.edu/sdr.

  19. Methodology for determining acceptable residual radioactive contamination levels at decommissioned nuclear facilities/sites

    International Nuclear Information System (INIS)

    Watson, E.C.; Kennedy, W.E. Jr.; Hoenes, G.R.; Waite, D.A.

    1979-01-01

    The ultimate disposition of decommissioned nuclear facilities and their surrrounding sites depends upon the degree and type of residual contamination. Examination of existing guidelines and regulations has led to the conclusion that there is a need for a general method to derive residual radioactive contamination levels that are acceptable for public use of any decommissioned nuclear facility or site. This paper describes a methodology for determining acceptable residual radioactive contamination levels based on the concept of limiting the annual dose to members of the public. It is not the purpose of this paper to recommend or even propose dose limits for the exposure of the public to residual radioactive contamination left at decommissioned nuclear facilities or sites. Unrestricted release of facilities and/or land is based on the premise that the potential annual dose to any member of the public using this property from all possible exposure pathways will not exceed appropriate limits as may be defined by Federal regulatory agencies. For decommissioned land areas, consideration should be given to people living directly on previously contaminated areas, growing crops, grazing food animals and using well water. Mixtures of radionuclides in the residual contamination representative of fuel reprocessing plants, light water reactors and their respective sites are presented. These mixtures are then used to demonstrate the methodology. Example acceptable residual radioactive contamination levels, based on an assumed maximum annual dose of one millirem, are calculated for several selected times following shutdown of a facility. It is concluded that the methodology presented in this paper results in defensible acceptable residual contamination levels that are directly relatable to risk assessment with the proviso that an acceptable limit to the maximum annual dose will be established. (author)

  20. Standard test method for determining residual stresses by the hole-drilling strain-gage method

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2008-01-01

    1.1 Residual Stress Determination: 1.1.1 This test method specifies a hole-drilling procedure for determining residual stress profiles near the surface of an isotropic linearly elastic material. The test method is applicable to residual stress profile determinations where in-plane stress gradients are small. The stresses may remain approximately constant with depth (“uniform” stresses) or they may vary significantly with depth (“non-uniform” stresses). The measured workpiece may be “thin” with thickness much less than the diameter of the drilled hole or “thick” with thickness much greater than the diameter of the drilled hole. Only uniform stress measurements are specified for thin workpieces, while both uniform and non-uniform stress measurements are specified for thick workpieces. 1.2 Stress Measurement Range: 1.2.1 The hole-drilling method can identify in-plane residual stresses near the measured surface of the workpiece material. The method gives localized measurements that indicate the...

  1. [Determination of organochlorine pesticide residues in the roots of Zanthoxylum nitidum by GC-MS].

    Science.gov (United States)

    Jiao, Ai-Jun; Feng, Jie; Lai, Mao-Xiang

    2013-04-01

    To determine the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum and provide scientific foundation for the quality control and standard establishment. GC-MS method with selected ion monitoring (SIM) mode was used to analyze the contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum. The samples were extracted with acetone and ultrasonic vibrations, and the analytical samples were purified by anhydrous sodium sulfate-anhydrous magnesium sulfate -PSA -C18-PestiCarb -phase extraction (SPE) cartridge. Eight kinds of organochlorine pesticide were detected simultanously. Small amounts of OP-DDT were detected in samples 1, 4, 5, 6, 11 and 12, no organochlorine pesticide residue was detected in other samples. The RSD of precision ranged from 0.89% to 2.21%, and the average recovery ranged from 85.33% to 103.70%, with the RSD less than 4%. The contents of organochlorine pesticide residues in the roots of Zanthoxylum nitidum are less than 0.2 ppm. This method is sensitive, good purifying, and suitable for analyzing organochlorine pesticide residues in the roots of Zanthoxylum nitidum.

  2. Determination of residual stresses in autofrettaged steel tubes by neutron and X-ray diffraction

    International Nuclear Information System (INIS)

    Pintschovius, L.; Macherauch, E.; Scholtes, B.

    1986-01-01

    The residual stress state of an autofrettaged 30 CrNiMo 8 steel tube has been investigated by neutron and X-ray diffraction. The results of X-ray measurements on the face of a ring cut out of the tube agree well with the neutron results obtained on the central part of an unmachined specimen. The experimentally determined residual stress distributions resemble only to a first approximation that expected from theoretical estimations. As expected, the tangential stress component at the inner diameter was found to be largest and is compressive. However, the distributions of the tangential and radial residual stress components show large deviations from the expected values. The differences between experiment and theory are probably due to neglecting the Bauschinger effect, the decarburization of the surface layers and the residual stresses produced by an alignment procedure before the autofrettage process. Annealing the tube for 1 h at 450 0 C has little effect on the residual stress distribution, except for a reduction in the steep gradient of the tangential stress component close to the inner surface. (orig.)

  3. Procedures for interface residual stress determination using neutron diffraction: Mo-coated steel gear wheel

    International Nuclear Information System (INIS)

    Bruno, Giovanni; Fanara, Carlo; Hughes, Darren J.; Ratel, Nicolas

    2006-01-01

    Residual stresses were determined in steel gear wheels coated with molybdenum using neutron diffraction. A systematic procedure was developed to assess them in both the molybdenum coating and in the steel substrate. A detailed description of the problems associated with measurements of this type is given, together with a procedure aimed at rationalising their solution. Precise sample positioning was developed using a new experimental method and advanced metrology equipment allowing off-line sample alignment and mounting. This reliably replaces the inefficient use of entrance scans, usually adopted in residual stress analysis by neutron diffraction. Corrections were applied to overcome the presence of pseudo-strains and data reduction was performed to coherently interpret the results, including the determination of the centre-of-mass of the diffracting volume. The full three-dimensional stress profile was determined in the coating and the substrate. The data analysis methodology is fully described and recommendations are given for this kind of measurement

  4. Surface lignin change pertaining to the integrated process of dilute acid pre-extraction and mechanical refining of poplar wood chips and its impact on enzymatic hydrolysis.

    Science.gov (United States)

    Liu, Wei; Chen, Wei; Hou, Qingxi; Zhang, Jinping; Wang, Bing

    2017-03-01

    Dilute acid pre-extraction enhanced the mechanically refined poplar pulp substrates' enzymatic hydrolysis efficiency obviously. The results showed that the surface lignin distribution was changed significantly in residual wood chips and pulp substrates, and the surface lignin distribution showed important impact on the following enzymatic hydrolysis. Acid pre-extraction can lead to a redistribution of lignin in fiber cell walls, i.e., the lignin was degraded and migrated to fiber surface in the form of re-deposited lignin and pseudo-lignin. However, higher pre-extraction intensity was not desired due to the formation of redeposited lignin and pseudo-lignin. This study will help to reach a deeper understanding on the lignin distribution in the view of molecular and ultrastructure, and promote the development of a cost-efficient pretreatment strategy for biomass processing. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. Determination and modeling of residual stress in functionally graded WC-Co

    Science.gov (United States)

    Tahvilian, Leila

    Gradual variations in composition and/or structure through the volume of functionally graded materials (FGMs) generally result in corresponding continuous spatial variations in mechanical/physical properties, and often in significant residual stresses that develop during processing. Due to inhomogeneous properties in these materials, residual stress measurement in FGMs can be a very challenging problem. In this study, residual stresses in functionally graded cemented tungsten carbide (FG-WC-Co) were investigated by numerical, analytical and experimental approaches by means of a layer removal technique. The numerical method consisted of finite element analysis (FEA) modeling for the FGM plate, in order to calculate residual stress distribution over the volume and to develop a method for predicting residual stress levels in closely related materials. The analytical procedure embodied a mathematical approach to determine residual stress distributions, and analytically determined values are compared with those obtained from FEA modeling and experimental results. The experimental approach consisted of fabricating and heat treating FG-WC-Co flat samples, then measuring strain changes by strain gauge after each sequential layer removal from the opposite side of the specimen from the graded region. Good agreement was found between analytical, numerical and experimental results. Furthermore, thermal residual stress distribution in FG-WC-Co hollow cylinder was examined with an emphasis on the effects of key variables, the gradient profile and the gradient thickness, on the magnitude and distribution of the stress field. An analytical direct solution based on solving the governing equations of a cylinder composed of a uniform inner core and a functionally graded outer shell was developed. The cylindrical compound was considered as two separate elements: homogeneous cylinder and functionally graded shell. Material properties, such as the elastic modulus and the coefficient of

  6. Exploring the Oxidation of Lignin-Derived Phenols by a Library of Laccase Mutants

    Directory of Open Access Journals (Sweden)

    Isabel Pardo

    2015-09-01

    Full Text Available Saturation mutagenesis was performed over six residues delimiting the substrate binding pocket of a fungal laccase previously engineered in the lab. Mutant libraries were screened using sinapic acid as a model substrate, and those mutants presenting increased activity were selected for exploring the oxidation of lignin-derived phenols. The latter comprised a battery of phenolic compounds of interest due to their use as redox mediators or precursors of added-value products and their biological activity. The new laccase variants were investigated in a multi-screening assay and the structural determinants, at both the substrate and the protein level, for the oxidation of the different phenols are discussed. Laccase activity greatly varied only by changing one or two residues of the enzyme pocket. Our results suggest that once the redox potential threshold is surpassed, the contribution of the residues of the enzymatic pocket for substrate recognition and binding strongly influence the overall rate of the catalytic reaction.

  7. Lignin biodegradation and industrial implications

    Directory of Open Access Journals (Sweden)

    Adam B Fisher

    2014-12-01

    Full Text Available Lignocellulose, which comprises the cell walls of plants, is the Earth’s most abundant renewable source of convertible biomass. However, in order to access the fermentable sugars of the cellulose and hemicellulose fraction, the extremely recalcitrant lignin heteropolymer must be hydrolyzed and removed—usually by harsh, costly thermochemical pretreatments. Biological processes for depolymerizing and metabolizing lignin present an opportunity to improve the overall economics of the lignocellulosic biorefinery by facilitating pretreatment, improving downstream cellulosic fermentations or even producing a valuable effluent stream of aromatic compounds for creating value-added products. In the following review we discuss background on lignin, the enzymology of lignin degradation, and characterized catabolic pathways for metabolizing the by-products of lignin degradation. To conclude we survey advances in approaches to identify novel lignin degrading phenotypes and applications of these phenotypes in the lignocellulosic bioprocess.

  8. Roles of small laccases from Streptomyces in lignin degradation.

    Science.gov (United States)

    Majumdar, Sudipta; Lukk, Tiit; Solbiati, Jose O; Bauer, Stefan; Nair, Satish K; Cronan, John E; Gerlt, John A

    2014-06-24

    Laccases (EC 1.10.3.2) are multicopper oxidases that can oxidize a range of substrates, including phenols, aromatic amines, and nonphenolic substrates. To investigate the involvement of the small Streptomyces laccases in lignin degradation, we generated acid-precipitable polymeric lignin obtained in the presence of wild-type Streptomyces coelicolor A3(2) (SCWT) and its laccase-less mutant (SCΔLAC) in the presence of Miscanthus x giganteus lignocellulose. The results showed that strain SCΔLAC was inefficient in degrading lignin compared to strain SCWT, thereby supporting the importance of laccase for lignin degradation by S. coelicolor A3(2). We also studied the lignin degradation activity of laccases from S. coelicolor A3(2), Streptomyces lividans TK24, Streptomyces viridosporus T7A, and Amycolatopsis sp. 75iv2 using both lignin model compounds and ethanosolv lignin. All four laccases degraded a phenolic model compound (LM-OH) but were able to oxidize a nonphenolic model compound only in the presence of redox mediators. Their activities are highest at pH 8.0 with a low krel/Kapp for LM-OH, suggesting that the enzymes’ natural substrates must be different in shape or chemical nature. Crystal structures of the laccases from S. viridosporus T7A (SVLAC) and Amycolatopsis sp. 75iv2 were determined both with and without bound substrate. This is the first report of a crystal structure for any laccase bound to a nonphenolic β-O-4 lignin model compound. An additional zinc metal binding site in SVLAC was also identified. The ability to oxidize and/or rearrange ethanosolv lignin provides further evidence of the utility of laccase activity for lignin degradation and/or modification.

  9. Analytical protocols for characterisation of sulphur-free lignin

    NARCIS (Netherlands)

    Gosselink, R.J.A.; Abächerli, A.; Semke, H.; Malherbe, R.; Käuper, P.; Nadif, A.; Dam, van J.E.G.

    2004-01-01

    Interlaboratory tests for chemical characterisation of sulphur-free lignins were performed by five laboratories to develop useful analytical protocols, which are lacking, and identify quality-related properties. Protocols have been established for reproducible determination of the chemical

  10. Determination of insecticides malathion and lambda-cyhalothrin residues in zucchini by gas chromatography

    Directory of Open Access Journals (Sweden)

    Hayam M. Lofty

    2013-12-01

    Full Text Available A sensitive gas chromatographic method has been developed for the determination of malathion and lambda-cyhalothrin (λ-cyhalothrin insecticide residues in zucchini. The developed method consists of extraction with acetone, purification and partitioning with methylene chloride, column chromatographic clean-up, and finally capillary gas chromatographic determination of the insecticides. The recoveries of method were greater than 90% and limit of determination was 0.001 ppm for both insecticides. The method was applied to determine residues and the rate of disappearance of malathion and λ-cyhalothrin from fruits of zucchini (open field treatment, 50 cc of Malason/Cormandel 57% EC (emulsifiable concentrate for 100 L of water, 20 cc of LAMBDA SUPER FOG 5% liquid for 100 L of water. The insecticide incorporated into the plants decreased rapidly with a half-life time around 0.77 day (18.5h for malathion and 4 days for λ-cyhalothrin. It is not recommended to use zucchini before 12 h of malathion application. For λ-cyhalothrin, the preharvest interval is 5 days. Four market samples were chosen from different regions from A.R.E. and all of them showed no residues of malathion or λ-cyhalothrin.

  11. Temperature Field Prediction for Determining the Residual Stresses Under Heat Treatment of Aluminum Alloys

    Directory of Open Access Journals (Sweden)

    A. V. Livshits

    2014-01-01

    Full Text Available The article is devoted to non-stationary temperature field blanks from aluminum alloys during heat treatment. It consists of the introduction and two smaller paragraphs. In the introduction the author concerns the influence of residual stresses arising in the manufacturing process of details, on the strength of the whole aircraft construction and, consequently, on their technical and economic parameters, such as weight, reliability, efficiency, and cost. He also notes that the residual stresses appeared during the production of parts change their location, size and direction under the influence of the elastic deformations that occur during the exploitation of aircraft. Redistributed residual stresses may have a chaotic distribution that may cause overlap of these stresses on the stresses caused by the impact of workload of constructions and destruction or damage of aircraft components.The first paragraph is devoted to the existing methods and techniques for determining the residual stresses. The presented methods and techniques are analyzed to show the advantages and disadvantages of each of them. The conclusion is drawn that the method to determine the residual stresses is necessary, its cost is less than those of existing ones, and an error does not exceed 10%.In the second section, the author divides the problem of determining the residual stresses into two parts, and describes the solution methods of the first one. The first problem is to define the temperature field of the work piece. The author uses a Fourier equation with the definition of initial and boundary conditions to describe a mathematical model of the heat cycle of work piece cooling. He draws special attention here to the fact that it is complicated to determine the heat transfer coefficient, which characterizes the process of cooling the work piece during hardening because of its dependence on a number of factors, such as changing temperature-dependent material properties of

  12. Influence of alkaline hydrothermal pretreatment on shrub wood Tamarix ramosissima: Characteristics of degraded lignin

    International Nuclear Information System (INIS)

    Xiao, Ling-Ping; Bai, Yuan-Yuan; Shi, Zheng-Jun; Lu, Qiang; Sun, Run-Cang

    2014-01-01

    The objective of this work was to evaluate the influence of alkaline hydrothermal (AH) pretreatment on the physicochemical properties of the degraded lignins, attempt to upgrade the potential of lignin for value-added chemicals and fuel production. For this purpose, shrub wood Tamarix ramosissima lignin was fractionated using a two-stage process based on an AH pretreatment followed by an alkaline ethanol post-treatment. The recovered lignin fractions were investigated by comparison with milled wood lignin (MWL) in terms of fractionation yield, carbohydrate composition, gel permeation chromatography, Fourier transform infrared spectroscopy, 13 C and 2D heteronuclear single quantum correlation nuclear magnetic resonance, as well as pyrolysis-gas chromatography/mass spectrometry. The result showed that AH pretreatment led to the degradation of β-O-4 linkages and consequently the increased severity caused a release of more S-units lignin fractions with molecular weights between 1300 and 2500 g/mol in the liquid but higher molecular weights (3000–4400 g/mol) in the residues. Moreover, it was found that the lignin syringyl-to-guaiacyl (S/G) ratios from analytical pyrolysis slightly changed after AH pretreatment (S/G, 1.8–2.3) but higher than those of MWL (S/G, 1.7). Overall, the present study demonstrates that these lignins dissolved during AH pretreatment and those recovered from the solid residues isolated with alkaline ethanol post-treatment could be profitably exploited as feedstock in integrated forest biorefineries, rather than traditional use as low-value energy sources.- Highlights: • Alkaline hydrothermal pretreatment and alkaline ethanol post-treatment were proposed. • The influence of AH pretreatment on the lignin structural changes was characterized. • Aryl-O-ether linkages of lignin were extensively cleaved. • Lignin recovered from solid residue is a potential resource for the production of value-added chemicals

  13. Method for improve x-ray diffraction determinations of residual stress in nickel-base alloys

    Science.gov (United States)

    Berman, Robert M.; Cohen, Isadore

    1990-01-01

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys which comprises covering part of a predetermined area of the surface of a nickel-base alloy with a dispersion, exposing the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample.

  14. Method for improving x-ray diffraction determinations of residual stress in nickel-base alloys

    Science.gov (United States)

    Berman, R.M.; Cohen, I.

    1988-04-26

    A process for improving the technique of measuring residual stress by x-ray diffraction in pieces of nickel-base alloys is discussed. Part of a predetermined area of the surface of a nickel-base alloy is covered with a dispersion. This exposes the covered and uncovered portions of the surface of the alloy to x-rays by way of an x-ray diffractometry apparatus, making x-ray diffraction determinations of the exposed surface, and measuring the residual stress in the alloy based on these determinations. The dispersion is opaque to x-rays and serves a dual purpose, since it masks off unsatisfactory signals such that only a small portion of the surface is measured, and it supplies an internal standard by providing diffractogram peaks comparable to the peaks of the nickel alloy so that the alloy peaks can be very accurately located regardless of any sources of error external to the sample. 2 figs.

  15. Determination of macro nickel, vanadium and iron in crude oil and residues by derivative spectrophotometry

    International Nuclear Information System (INIS)

    Liu, W.; Wang, L.; Li, X.

    1992-01-01

    In this paper, a new method with derivative spectrophotometry and 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol as the chromogenic reagent in buffer solution of different pH developed for determining micro amounts of nickel. Vanadium and iron in crude oil and residues is reported. Forth-, Second- and Third-, Fourth-order derivative spectrophotometry were applied to determine nickel, nickel and vanadium, nickel and iron in crude oil and residues, respectively. The derivative maximums chosen for the measurement were at 556 nm for nickel, 540 nm and 643 nm for nickel and vanadium, 524 nm and 604 nm for nickel and iron. Beer's law is valid for the range 1.0 x 10 -6 to 2.5 x 10 -5 M

  16. Determination of thymine glycol residues in irradiated or oxidized DNA by formation of methylglyceric acid

    International Nuclear Information System (INIS)

    Schellenberg, K.A.; Shaeffer, J.

    1986-01-01

    Treatment of DNA solutions with X-irradiation various oxidants including hydrogen peroxide plus ferrous ion, hydrogen peroxide plus copper ion and ascorbate, permanganate, or sonication in the presence of dissolved oxygen all produced varying amounts of thymine glycol residues. After denaturing the DNA with heat, the glycol residues were reduced and labeled at the 6 position with tritium- labeled sodium borohydride. Subsequent reaction with anhydrous methanolic HCl gave a quantitative yield of the methyl ester of methylglyceric acid, which was determined by thin layer chromatography. The method, developed using thymidine as a model, was used to ascertain the requirements for glycol formation in DNA. It was shown that hydroxyl radical generating systems, permanganate, X-irradiation, or sonication in presence of oxygen were required, but hydrogen peroxide in the absence of iron or copper and ascorbate was inactive. Application to determination of DNA damage in vivo is being explored

  17. Characterisation of lignins isolated from sugarcane bagasse pretreated with acidified ethylene glycol and ionic liquids

    International Nuclear Information System (INIS)

    Moghaddam, Lalehvash; Zhang, Zhanying; Wellard, R. Mark; Bartley, John P.; O'Hara, Ian M.; Doherty, William O.S.

    2014-01-01

    Sugarcane bagasse pretreatment processes using acidified aqueous ethylene glycol (EG) and ionic liquids (ILs) have been reported recently. In this study, recovery of lignins from these processes was conducted, as well as determination of their physico-chemical properties. The amount of lignins recovered from 1-butyl-3-methylimidazolium chloride ([bmim]Cl) with HCl as a catalyst and [bmim][CH 3 SO 3 ] was ∼42%, and ∼35%–36% by EG with HCl or H 2 SO 4 as a catalyst, respectively. The isolated lignins were characterised using wet chemistry, spectroscopy and thermogravimetry analysis (TGA), and the results compared to soda lignin from NaOH pretreatment of bagasse. The IL and EG lignins contained no or trace amounts of carbohydrates, slightly lower hydrogen content but slightly higher oxygen contents than soda lignin. The IL and EG lignins contained more C-3 and C-5 reactive sites for Mannich reaction and had more p-hydroxypheny propane unit structures than soda lignin. Two-dimensional heteronuclear single quantum coherence (2D HSQC) nuclear magnetic resonance (NMR) identified the major substructural units in the lignins, and allowed differences among them to be studied. As EG lignins were extracted in very reactive environment, intermediate enol ethers were formed and led to cleavage reactions which were not apparent in the other lignins. 31 P NMR and infra-red spectroscopy results showed that IL and EG lignins had lower total hydroxyl content than soda lignin, probably indicating that a higher degree of self-polymerisation occurred during bagasse pretreatment, despite the use of lower temperature and shorter reaction time. On the basis of the salient features of these lignins, potential applications were proposed. - Highlights: • Lignins were recovered from ethylene glycol (EG) and ionic liquid (IL) processes. • IL and EG lignins contained no or trace amounts of carbohydrates. • IL and EG lignin had more C-3 and C-5 sites for Mannich reaction than soda

  18. REAL STRUCTURE AND RESIDUAL STRESSES IN ADVANCED WELDS DETERMINED BY X-RAY AND NEUTRON DIFFRACTION

    Directory of Open Access Journals (Sweden)

    Karel Trojan

    2017-07-01

    Full Text Available The paper outlines the capability of X-ray diffraction (XRD for evaluation of real structure changes and residual stresses (RS on cross-section of advanced thick welds due to the welding of ferromagnetic plates. The results of neutron diffraction describe a three-dimensional state of RS and also verify previous assumptions of RS redistribution as a result of the surface preparation for determination 2D maps measured by XRD.

  19. Determination of residual ractopamine concentrations by enzyme immunoassay in treated pig's tissues on days after withdrawal.

    Science.gov (United States)

    Pleadin, Jelka; Perši, Nina; Vulić, Ana; Milić, Dinka; Vahčić, Nada

    2012-03-01

    The objective of this study was to measure residual ractopamine concentrations in tissues of pigs as experimental animals after treatment with dietary ractopamine for 28 consecutive days. Ractopamine was administered orally to the experimental group (n=9) in a dose of 0.1mg/kg body mass per day, whereas control animals (n=3) were left untreated. Treated pigs (60kg) were sacrificed on days 1, 3 and 8 of treatment discontinuation and residues were determined in kidney, liver, muscle, brain and heart tissues using previously validated enzyme-linked immunosorbent assay (ELISA) as a quantitative screening method. Validation showed good mean recoveries (approx. 70-90%) with acceptable inter- and intra-day relative standard deviations (RSDractopamine tissue concentrations. The highest ractopamine concentration on day 1 (24h) after the last exposure was recorded in the kidney (12.49±7.96ng/g), followed by the liver (7.21±2.73ng/g), heart (1.26±0.12ng/g) and brain (0.63±0.05ng/g); at this time of withdrawal, residues were not detected in the muscle. Ractopamine was depleted rapidly from all study tissues, with mostly no detectable residues on day 8 of withdrawal. Copyright © 2011 Elsevier Ltd. All rights reserved.

  20. Determination of oxytetracycline residues in cattle meat marketed in the Kilosa district, Tanzania

    Directory of Open Access Journals (Sweden)

    Zuhura I. Kimera

    2015-11-01

    Full Text Available Oxytetracycline is used to treat various diseases in cattle. However, its use may be associated with unacceptable residue levels in food. Oxytetracycline residues in tissues from indigenous cattle were determined in a cross-sectional study conducted in the Kilosa district, Tanzania, between November 2012 and April 2013. A total of 60 tissue samples, including muscle, liver and kidney, were collected from slaughterhouses and butchers and analysed for oxytetracycline using high-performance liquid chromatography. Oxytetracycline residues were found in 71.1% of the samples, of which 68.3% were above acceptable regulatory levels. The mean concentration of oxytetracycline across tissues was 3401.1 μg/kg ± 879.3 μg/kg; concentrations in muscle, liver and kidney were 2604.1 μg/kg ± 703.7 μg/kg, 3434.4 μg/kg ± 606.4 μg/kg and 3533.1 μg/kg ± 803.6 μg/kg, respectively. High levels of oxytetracycline residue in meat from indigenous cattle may pose a health threat to consumers in Kilosa. The findings possibly reflect a general lack of implementation of recommended withdrawal periods, ignorance about drug use and lack of extension services. Strict regulation of the use of antimicrobial drugs in the livestock industry and associated testing of animal-derived food sources prior to marketing are required.

  1. Simultaneous determination of tebuconazole, trifloxystrobin, and its metabolite trifloxystrobin acid residues in gherkin under field conditions.

    Science.gov (United States)

    Paramasivam, Mariappan; Selvi, Chellamuthu; Deepa, Manthirachalam; Jayaprakash, Samiyannan A; Chandrasekaran, Subramanian

    2015-03-01

    A rapid, simple, and selective analytical method for the simultaneous determination of tebuconazole, trifloxystrobin, and its metabolite trifloxystrobin acid residues in gherkin and soil was developed and validated by gas chromatography coupled with mass spectrometry. The samples were extracted with acetonitrile and cleaned up by dispersive solid-phase extraction with primary secondary amine sorbent. The limit of quantification of the method was 0.05 mg/kg for all three compounds. The method was validated using blank samples spiked at three levels and recoveries ranged from 83.5 to 103.8% with a relative standard deviation of 1.2 to 4.8%. The developed method was validated and applied for the analysis of a degradation study sample. The residues of trifloxystrobin and tebuconazole were found to dissipate following first-order kinetics with half-life ranging between 3.31-3.38 and 3.0-3.04 days, respectively, for two different dosages. Pesticide residues were below the European Union maximum residue level after seven days for trifloxystrobin (0.2 mg/kg) and ten days for tebuconazole (0.05 mg/kg), which suggested the use of this fungicide mixture to be safe to humans. These results can be utilized in formulating the spray schedule and safety evaluation on trifloxystrobin and tebuconazole in gherkin crop. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Environmental economics of lignin derived transport fuels.

    Science.gov (United States)

    Obydenkova, Svetlana V; Kouris, Panos D; Hensen, Emiel J M; Heeres, Hero J; Boot, Michael D

    2017-11-01

    This paper explores the environmental and economic aspects of fast pyrolytic conversion of lignin, obtained from 2G ethanol plants, to transport fuels for both the marine and automotive markets. Various scenarios are explored, pertaining to aggregation of lignin from several sites, alternative energy carries to replace lignin, transport modalities, and allocation methodology. The results highlight two critical factors that ultimately determine the economic and/or environmental fuel viability. The first factor, the logistics scheme, exhibited the disadvantage of the centralized approach, owing to prohibitively expensive transportation costs of the low energy-dense lignin. Life cycle analysis (LCA) displayed the second critical factor related to alternative energy carrier selection. Natural gas (NG) chosen over additional biomass boosts well-to-wheel greenhouse gas emissions (WTW GHG) to a level incompatible with the reduction targets set by the U.S. renewable fuel standard (RFS). Adversely, the process' economics revealed higher profits vs. fossil energy carrier. Copyright © 2017 The Author(s). Published by Elsevier Ltd.. All rights reserved.

  3. Determination of residual zirconia in the reaction product of zircon formation from zirconia and silica

    International Nuclear Information System (INIS)

    Hashiba, Minoru; Miura, Eiji; Nurishi, Yukio; Hibino, Taizo

    1978-01-01

    A new chemical method for the determination of zirconia in the reaction product of zircon formation from zirconia and silica is presented in this paper. The reaction product was fused in the temperature range between 400 0 C, and 450 0 C by ammonium sulfate (zirconia/ammonium sulfate = 1/10, weight). Zirconia was extracted by 4N H 2 SO 4 aqueous solution. After the residue was separated by filter paper containing filter pulp, it was washed by hot water thoroughly. By adding aqueous ammonia water to the combined filtrate, zirconium hydroxide was precipitated gelatinously. The precipitate was ignited in platinum crucible at 1000 0 C and the zirconia obtained was weighed. It was confirmed by the following experiments that the present method is very reliable for quantitative determination of residual zirconia. Firstly, in both zirconia and various mixtures of zircon and silica, the recovery of zirconia is about (99.6 +- 0.2)%. Secondly, the reaction for equimolar mixture of zirconia and silica was conducted at several temperatures between 1350 0 C and 1500 0 C. The quantity of residual zirconia on the way of the reaction was reasonably determined by the present method. In conclusion, the present method can be applicable for the study on the reaction mechanism of zircon formation from zirconia and silica. (auth.)

  4. Determination of residual manganese in Mn porphyrin-based superoxide dismutase (SOD) and peroxynitrite reductase mimics.

    Science.gov (United States)

    Rebouças, Júlio S; Kos, Ivan; Vujasković, Zeljko; Batinić-Haberle, Ines

    2009-12-05

    The awareness of the beneficial effects of Mn porphyrin-based superoxide dismutase (SOD) mimics and peroxynitrite scavengers on decreasing oxidative stress injuries has increased the use of these compounds as mechanistic probes and potential therapeutics. Simple Mn2+ salts, however, have SOD-like activity in their own right both in vitro and in vivo. Thus, quantification/removal of residual Mn2+ species in Mn-based therapeutics is critical to an unambiguous interpretation of biological data. Herein we report a simple, sensitive, and specific method to determine residual Mn2+ in Mn porphyrin preparations that combines a hydrometallurgical approach for separation/speciation of metal compounds with a spectrophotometric strategy for Mn determination. The method requires only common chemicals and a spectrophotometer and is based on the extraction of residual Mn2+ by bis(2-ethylhexyl)hydrogenphosphate (D2EHPA) into kerosene, re-extraction into acid, and neutralization followed by UV-vis determination of the Mn2+ levels via a Cd2+-catalyzed metallation of the H2TCPP4- porphyrin indicator. The overall procedure is simple, sensitive, specific, and amenable to adaptation. This quantification method has been routinely used by us for a large variety of water-soluble porphyrins.

  5. Quantification of Lignin and Its Structural Features in Plant Biomass Using 13C Lignin as Internal Standard for Pyrolysis-GC-SIM-MS.

    Science.gov (United States)

    van Erven, Gijs; de Visser, Ries; Merkx, Donny W H; Strolenberg, Willem; de Gijsel, Peter; Gruppen, Harry; Kabel, Mirjam A

    2017-10-17

    Understanding the mechanisms underlying plant biomass recalcitrance at the molecular level can only be achieved by accurate analyses of both the content and structural features of the molecules involved. Current quantification of lignin is, however, majorly based on unspecific gravimetric analysis after sulfuric acid hydrolysis. Hence, our research aimed at specific lignin quantification with concurrent characterization of its structural features. Hereto, for the first time, a polymeric 13 C lignin was used as internal standard (IS) for lignin quantification via analytical pyrolysis coupled to gas chromatography with mass-spectrometric detection in selected ion monitoring mode (py-GC-SIM-MS). In addition, relative response factors (RRFs) for the various pyrolysis products obtained were determined and applied. First, 12 C and 13 C lignin were isolated from nonlabeled and uniformly 13 C labeled wheat straw, respectively, and characterized by heteronuclear single quantum coherence (HSQC), nuclear magnetic resonance (NMR), and py-GC/MS. The two lignin isolates were found to have identical structures. Second, 13 C-IS based lignin quantification by py-GC-SIM-MS was validated in reconstituted biomass model systems with known contents of the 12 C lignin analogue and was shown to be extremely accurate (>99.9%, R 2 > 0.999) and precise (RSD < 1.5%). Third, 13 C-IS based lignin quantification was applied to four common poaceous biomass sources (wheat straw, barley straw, corn stover, and sugar cane bagasse), and lignin contents were in good agreement with the total gravimetrically determined lignin contents. Our robust method proves to be a promising alternative for the high-throughput quantification of lignin in milled biomass samples directly and simultaneously provides a direct insight into the structural features of lignin.

  6. Development of an analytical method for determination of sulfonamide residues in eggs

    International Nuclear Information System (INIS)

    Ben Azzeddine, Chams

    2009-01-01

    For the determination of sulfonamide residues in eggs, Premitest is selected for screening, providing a qualitative biological approach, it is inexpensive, fast, multi-elements and easy to implement. The H. P.L.C. / UV is the quantitative method of choice for confirmation and determination of these contaminants. During my internship, I had the opportunity to participate in the development of this method. It is recognized slower and more expensive but more specific and more sensitive. In this report, I present this optimized method and some criteria checked during my internship. Other criteria are to be completed to validate the method that will be subsequently used for routine analysis.

  7. Simultaneous determination of chloroamphenicol, thiamphenicol and florfenicol residues in bovine milk by micellar electrokinetic chromatography

    OpenAIRE

    Pezza, Leonardo [UNESP; Ríos, Àngel; Nozal, Leonor; Arce, Lourdes; Valcárce, Miguel

    2006-01-01

    A micellar electrokinetic chromatographic method (MEKC) is described for determining residues of amphenicols(chloramphenicol,thiamphenicol and florfenicol) in bovine milk. MEKC is conducted by using a separation buffer consisting of 20 mM Na2HPO4, 10 mM Na2B4O7, 50 mM SDS at pH 8.0; UV detection at 210 nm and 10 kV of voltage. The limit of detection ranged from 4.3-5.3 µg L-1. The MEKC method was applied for the simultaneous determination of amphenicols in milk samples spiked with amphenicols...

  8. Residual stress determination in a 1000 A tungsten thin film by X-rays diffraction

    International Nuclear Information System (INIS)

    Badawi, K.F.; Declemy, A.; Naudon, A.; Goudeau, P.

    1992-01-01

    In this study, we have determined the complete residual stress tensor by X-rays diffraction, using the sin 2 ψ method, in a 1000 A tungsten thin film deposited on a silicon monocrystal. Stresses are tension wise of big magnitude (1.5 GPa). They are almost isotropic in the film plane. Shear stresses are low but not negligeable. After a bombardment by a 320 keV Xe ++ ion beam, the stresses became compressive (about -1.3 GPa). These results demonstrate the feasability of stress determination by the sin 2 ψ method in films as thin as 1000 A and open interesting areas for future research. (orig.)

  9. Adsorption of cellulase on cellulolytic enzyme lignin from lodgepole pine.

    Science.gov (United States)

    Tu, Maobing; Pan, Xuejun; Saddler, Jack N

    2009-09-09

    Enzymatic hydrolysis of lignocellulosic materials is significantly affected by cellulase adsorption onto the lignocellulosic substrates and lignin. The presence of lignin plays an important role in lignocellulosic hydrolysis and enzyme recycling. Three cellulase preparations (Celluclast, Spezyme CP, and MSUBC) were evaluated to determine their adsorption onto cellulolytic enzyme lignin (CEL) from steam-exploded Lodgepole pine (SELP) and ethanol (organosolv)-pretreated Lodgepole pine (EPLP). The adsorption affinity of cellulase (Celluclast) onto isolated lignin (CEL-EPLP and CEL-SELP) was slightly higher than that from corresponding EPLP and SELP substrates on the basis of the Langmuir constants. Effects of temperature, ionic strength, and surfactant on cellulase adsorption onto isolated lignin were also explored in this study. Thermodynamic analysis of enzyme adsorption onto isolated lignin (Gibbs free energy change DeltaG(0) approximately -30 kJ/mol) indicated this adsorption was a spontaneous process. The addition of surfactant (0.2% w/v) could reduce the adsorption of cellulase onto CEL-SELP by 60%. Two types of adsorption isotherm were compared for cellulase adsorption onto isolated lignin. A Langmuir adsorption isotherm showed better fit for the experimental data than a Freundlich adsorption isotherm.

  10. Residual stress determination in a dissimilar weld overlay pipe by neutron diffraction

    International Nuclear Information System (INIS)

    Woo, Wanchuck; Em, Vyacheslav; Hubbard, Camden R.; Lee, Ho-Jin; Park, Kwang Soo

    2011-01-01

    Highlights: → Determined residual stress distribution in a dissimilar weld overlay pipe. → Consists of a ferritic (SA508), austenitic (F316L) steels, Alloy 182 consumable. → Measured significant compression (-600 MPa) near the inner wall of overlay. → Validate integrity of the inner wall for the pressurized nozzle nuclear structure. - Abstract: Residual stresses were determined through the thickness of a dissimilar weld overlay pipe using neutron diffraction. The specimen has a complex joining structure consisting of a ferritic steel (SA508), austenitic steel (F316L), Ni-based consumable (Alloy 182), and overlay of Ni-base superalloy (Alloy 52M). It simulates pressurized nozzle components, which have been a critical issue under the severe crack condition of nuclear power reactors. Two neutron diffractometers with different spatial resolutions have been utilized on the identical specimen for comparison. The macroscopic 'stress-free' lattice spacing (d o ) was also obtained from both using a 2-mm width comb-like coupon. The results show significant changes in residual stresses from tension (300-400 MPa) to compression (-600 MPa) through the thickness of the dissimilar weld overlay pipe specimen.

  11. Determination of antibiotic residues and their interaction in milk with lactate biosensor.

    Science.gov (United States)

    Rinken, T; Riik, H

    2006-03-31

    Milk and dairy products are among the most important foodstuffs and the quality of raw milk is of significant importance from the point of view of human health. For rapid determination of chloramphenicol and penicillin residues in raw milk, lactate oxidase-based amperometric biosensor was used. The concentration of antibiotic residuals was determined by two characteristic reaction parameters, calculated from the biosensor transient response with the dynamic biosensor model. Both chloramphenicol and penicillin caused the decrease of the value of the kinetic parameter, but they changed the total signal change parameter in different ways. The shift of the combined total signal change parameter at the simultaneous presence of these antibiotics indicated their antagonistic effect. Due to the respiration process of bacteria in raw milk, the dynamics of the biosensor signal was different in warm and cold seasons. The respiration characteristics were added to the biosensor model as a negative linear time-depending factor. The reaction characteristic parameters, obtained with this complemented model, showed excellent alignment in different conditions and allowed to detect antibiotic residues and their interaction in raw milk.

  12. Determination of Benzylpenicillin Potassium Residues in Duck Meat Using Surface Enhanced Raman Spectroscopy with Au Nanoparticles

    Directory of Open Access Journals (Sweden)

    Yijie Peng

    2016-01-01

    Full Text Available A new method using surface enhanced Raman spectroscopy (SERS with Au nanoparticles was established for the rapid detection of benzylpenicillin potassium (PG residues in duck meat. Au nanoparticles were used as SERS enhancement substrate, and the maximum absorption peak of Au nanoparticles using the UV-Vis spectrophotometer was 548 nm. In the research, the SERS spectra of PG solutions and PG duck meat extract as well as their vibrational assignment were analyzed. The effects of Au nanoparticles addition, sample addition, NaCl solution addition, and adsorption time on the SERS intensities of PG duck meat extract were discussed. It is revealed that a good linearity can be obtained between the SERS intensities at 993 cm−1 and the PG residues concentrations (0.5~15.0 mg·L−1 detected in duck meat extract. The linear equation was Y=831.68X+1997.1, and the determination coefficient was 0.9553. The determination coefficient of PG in duck meat extract between the actual values and the predictive values was 0.9757, and the root mean square error (RMSEP was 0.6496 mg/L. The recovery rate of PG in duck meat extract was 90~121%. The results showed that the method using SERS with Au nanoparticles could pave a new way for the rapid detection of PG residues in duck meat.

  13. Residual stress determination in a dissimilar weld overlay pipe by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Woo, Wanchuck, E-mail: chuckwoo@kaeri.re.kr [Neutron Science Division, Korea Atomic Energy Research Institute, Daejeon 305-353 (Korea, Republic of); Em, Vyacheslav [Neutron Science Division, Korea Atomic Energy Research Institute, Daejeon 305-353 (Korea, Republic of); Hubbard, Camden R. [Materials Science and Technology Division, Oak Ridge National Laboratory, Oak Ridge, TN 37831 (United States); Lee, Ho-Jin [Nuclear Materials Research Center, Korea Atomic Energy Research Institute, Daejeon 305-353 (Korea, Republic of); Park, Kwang Soo [Corporate R and D Institute, Doosan Heavy Industries and Construction, Changwon 641-792 (Korea, Republic of)

    2011-10-15

    Highlights: {yields} Determined residual stress distribution in a dissimilar weld overlay pipe. {yields} Consists of a ferritic (SA508), austenitic (F316L) steels, Alloy 182 consumable. {yields} Measured significant compression (-600 MPa) near the inner wall of overlay. {yields} Validate integrity of the inner wall for the pressurized nozzle nuclear structure. - Abstract: Residual stresses were determined through the thickness of a dissimilar weld overlay pipe using neutron diffraction. The specimen has a complex joining structure consisting of a ferritic steel (SA508), austenitic steel (F316L), Ni-based consumable (Alloy 182), and overlay of Ni-base superalloy (Alloy 52M). It simulates pressurized nozzle components, which have been a critical issue under the severe crack condition of nuclear power reactors. Two neutron diffractometers with different spatial resolutions have been utilized on the identical specimen for comparison. The macroscopic 'stress-free' lattice spacing (d{sub o}) was also obtained from both using a 2-mm width comb-like coupon. The results show significant changes in residual stresses from tension (300-400 MPa) to compression (-600 MPa) through the thickness of the dissimilar weld overlay pipe specimen.

  14. ELISA validation and determination of cut-off level for chloramphenicol residues in honey

    Directory of Open Access Journals (Sweden)

    Biernacki Bogumił

    2015-09-01

    Full Text Available An analytical validation of a screening ELISA for detection of chloramphenicol (CAP in honey was conducted according to the Commission Decision 2002/657/EC and Guidelines for the Validation of Screening Methods for Residues of Veterinary Medicines. The analyte was extracted from honey with a water and ethyl acetate mixture, and CAP concentrations were measured photometrically at 450 nm. The recovery rate of the analyte from spiked samples was 79%. The cut-off level of CAP in honey as the minimum recovery (0.17 units was established. Detection capability (CCβ was fixed at 0.25 μg kg−1. No relevant interferences between matrix effects and structurally related substances including florfenicol and thiamphenicol were observed. The ELISA method should be useful for determination of CAP residues in honey monitoring.

  15. Determination of Pentachlorophenol and Hexachlorobenzene in Natural Waters Affected by Industrial Chemical Residues

    Directory of Open Access Journals (Sweden)

    Zuin Vânia Gomes

    1999-01-01

    Full Text Available This paper presents the development of a methodology for the simultaneous analysis of pentachlorophenol and hexachlorobenzene in natural waters affected by industrial residues, as its principal goal. Samples were collected in Quarentenário, São Vicente city, where most of the population utilize wells for their supply. The liquid-liquid extraction employed to remove PCP and HCB from the matrix for further identification and quantification, showed very good recovery and repeatability. The recovery range was between 81.5% and 103.0%, with a relative standard deviation of 2.4% and 4.1% for a fortification level of 10 ng L-1. In addition, organochlorine compounds were determined by GC-ECD and/or GC-MS. The limit of quantification was 5 ng L-1 for PCP and 2 ng L-1 for HCB, which are below the maximum level allowed by the EC directives for pesticide residues in drinking water.

  16. Recent Development in Sample Preparation and Analytical Techniques for Determination of Quinolone Residues in Food Products.

    Science.gov (United States)

    Zhang, Zhichao; Cheng, Hefa

    2017-05-04

    Used heavily in food animal production, quinolones occur widely in food products of animal origin. Development of highly sensitive and selective analytical techniques for the detection of quinolone residues, often at trace levels, in food samples is necessary to ensure food safety and understand their public health risk. With complex matrices, food samples typically require a series of pre-treatment steps, such as powdering, homogenization, deproteinization, and filtration. This review summarizes the recent advances in extraction, concentration, and detection techniques for quinolones in food product samples, and briefly compares the advantages and limitations of major techniques. Recent development of quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method and immunoassay- and biosensor-based detection methods for the determination of quinolones residues in food products is discussed in details. A perspective on the trends and needs of future research is also presented.

  17. Determination of Activated Carbon Residual Life using a Microwave Cavity Resonator

    International Nuclear Information System (INIS)

    Mason, A; Wylie, S; Shaw, A; Al-Shamma'a, A I; Thomas, A; Keele, H

    2011-01-01

    This paper presents the continuation of work conducted jointly between Dstl and LJMU. This unique body of work has been, largely, concerned with detecting the residual life of high performance filter materials using electromagnetic (EM) waves within a resonant cavity. Past work has considered both HEPA [1] and ASZM-TEDA[2] activated carbon filter materials. This paper continues the later work, considering the response of ASZM-TEDA activated carbon through the co-ageing of two distinct batches of the material. The paper briefly introduces activated carbon, discusses theory relevant to the work and the methodology used for investigation. A comprehensive set of results is included which seek to validate this technique for determining the residual lifespan of activated carbon.

  18. Residual stress determination in an overlay dissimilar welded pipe by neutron diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Woo, Wan Chuck [ORNL; Em, Vyacheslav [Korea Atomic Energy Research Institute; Hubbard, Camden R [ORNL; Lee, Ho-Jin [Korea Atomic Energy Research Institute; Park, Kwang Soo [Doosan Heavy Industries & Construction

    2011-01-01

    Residual stresses were determined through the thickness of a dissimilar weld overlay pipe using neutron diffraction. The specimen has a complex joining structure consisting of a ferritic steel (SA508), austenitic steel (F316L), Ni-based consumable (Alloy 182), and overlay of Ni-base superalloy (Alloy 52M). It simulates pressurized nozzle components, which have been a critical issue under the severe crack condition of nuclear power reactors. Two neutron diffractometers with different spatial resolutions have been utilized on the identical specimen for comparison. The macroscopic 'stress-free' lattice spacing (d{sub o}) was also obtained from both using a 2-mm width comb-like coupon. The results show significant changes in residual stresses from tension (300-400 MPa) to compression (-600 MPa) through the thickness of the dissimilar weld overlay pipe specimen.

  19. Disentangling evolutionary signals: conservation, specificity determining positions and coevolution. Implication for catalytic residue prediction

    DEFF Research Database (Denmark)

    Teppa, Elin; Wilkins, Angela D.; Nielsen, Morten

    2012-01-01

    within a multiple sequence alignment to investigate their predictive potential and degree of overlap. Results: Our results demonstrate that the different methods included in the benchmark in general can be divided into three groups with a limited mutual overlap. One group containing real-value...... Evolutionary Trace (rvET) methods and conservation, another containing mutual information (MI) methods, and the last containing methods designed explicitly for the identification of specificity determining positions (SDPs): integer-value Evolutionary Trace (ivET), SDPfox, and XDET. In terms of prediction of CR......, we find using a proximity score integrating structural information (as the sum of the scores of residues located within a given distance of the residue in question) that only the methods from the first two groups displayed a reliable performance. Next, we investigated to what degree proximity scores...

  20. Lignin Sulfonation - A different Approach

    DEFF Research Database (Denmark)

    Bjørkmann, Anders

    2001-01-01

    The research on sulfite pulping has been characterized by the attempts to explain its chemistry. The. different approach presented is incited by perceptions about the (still) unsolved problem of the ultrastructural features of lignin in wood. A simple kinetic model has been chosen to describe...... the reaction order of lignin as "concentration" (weight) in the dissolution kinetics, the cooking liquor being used in substantial excess. Three states of lignin were used: in wood as sawdust (W), in milled. wood (MW) and as milled wood lignin (MWL). Cooks were performed at pH 1.5, and 6. (measured at room...... temperature). The lignin was also modified chemically in two ways: alkaline borohydride reduction and diazomethane methylation. The reaction order (with the kinetics used) was found to be about 2/3, which is the value to be expected for particles of equal size reacting, at the particle surface. The cooks were...

  1. Determination of residual dimethylsulphoxide in drug loaded gelatin using thermal desorber - gas chromatography.

    Science.gov (United States)

    Asfaw, Adissu Alemayehu; Wolfs, Kris; Van Schepdael, Ann; Adams, Erwin

    2018-05-10

    Traditional headspace - gas chromatography (HS-GC) methods for the determination of residual solvents (RS) start from a homogenous sample solution. Subsequently, it is challenging to determine RS using HS-GC techniques from insoluble solid samples like gelatin which is practically impossible to dissolve or distribute uniformly in water and common organic solvents. In this study, a thermal desorber combined with capillary gas chromatography and flame ionization detection/mass spectrometry (TD-GC-FID/MS) was used for quantitative determination of residual dimethylsulfoxide (DMSO) in gelatin without sample pretreatment. A sample of gelatin was sandwiched between two quartz filter double layers in a polytetrafluoroethylene insert which was then placed in its entirety into a thermal desorption tube. Factors affecting the performance of TD-GC including desorption time, desorption temperature, desorption flow and type of adsorbent were studied by applying a standard solution of DMSO in methanol on a blank gelatin bed. Validation results of the proposed method showed good linearity with an R 2 -value higher than 0.999 for a wide concentration range and good sensitivity with a limit of detection and limit of quantification of 0.1 μg and 0.2 μg on tube, respectively. The proposed method shows recovery values close to 100%. In addition, a conventional HS-GC method following enzymatic degradation of gelatin was developed to verify the proposed TD-GC method. Both methods were applied for the determination of residual DMSO in gelatin that was loaded with an experimental drug. Results were comparable, but the enzyme assisted HS-GC method was more time consuming and expensive. Copyright © 2018 Elsevier B.V. All rights reserved.

  2. Transition metal catalyzed oxidation of Alcell lignin, soda lignin, and lignin model compounds in ionic liquids

    NARCIS (Netherlands)

    Zakzeski, J.; Jongerius, A.L.; Weckhuysen, B.M.

    2013-01-01

    Lignin is a component of lignocellulosic biomass from which important aromatic compounds can potentially be obtained. In the present work, Alcell and soda lignin were dissolved in the ionic liquid 1-ethyl-3-methylimidazolium diethylphosphate (EMIM DEP) and subsequently oxidized using several

  3. The effects of machine parameters on residual stress determined using micro-Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Sparks, R.G.; Enloe, W.S.; Paesler, M.A.

    1988-12-01

    The effects of machine parameters on residual stresses in single point diamond turned silicon and germanium have been investigated using micro-Raman spectroscopy. Residual stresses were sampled across ductile feed cuts in < 100 > silicon and germanium which were single point diamond turned using a variety of feed rates, rake angles and clearance angles. High spatial resolution micro-Raman spectra (1{mu}m spot) were obtained in regions of ductile cutting where no visible surface damage was present. The use of both 514-5nm and 488.0nm excitation wavelengths, by virtue of their differing characteristic penetration depths in the materials, allowed determinations of stress profiles as a function of depth into the sample. Previous discussions have demonstrated that such Raman spectra will exhibit asymmetrically broadened peaks which are characteristic of the superposition of a continuum of Raman scatterers from the various depths probed. Depth profiles of residual stress were obtained using computer deconvolution of the resulting asymmetrically broadened raman spectra.

  4. Elucidation of Chemical Structure of Wood Lignin by Dissolving in 1-Butyl-3-methylimidazolium Chloride Ionic Liquid

    Directory of Open Access Journals (Sweden)

    Ali Abdulkhani

    2012-12-01

    Full Text Available Residual lignin of wood after MWL isolation was dissolved with 1-butyl-3-methylimidazolium chloride ionic liquid. Chemical structure of isolated MWL from poplar wood (Popolus deltiodes and dissolved residual lignin were characterized with gas chromatography and 1D, 2D NMR techniques. Analytical results showed that  Popolus deltoides wood has more 4-(3-hydroxy-1-propenyl-2-methoxy phenol units (Guayacil lignin than 4-(3-hydroxy-1-propenyl-2,6-dimethoxy phenol units (Syringyl moieties. In addition to Guayacil and Syringyl, the extracted ligin is composed of a small amount of p-benzyl alcohol. The residual lignin is mainly composed of condensed structures which are often of carbohydrate complexes. The lignin structural ratios of dissolved wood in ionic liquid are the same as those of dioxan extracted lignin. Anomeric HSQC analysis of lignin showed that the lignin carbohydrate complex is composed of cellulose, xylan, mannan and arabinan sugars. Side-chain region of lignin structure is mainly composed of β-O-4, phenylcoumaran, resinol and spirodienone moieties.

  5. Peroxidases bound to the growing lignin polymer produce natural like extracellular lignin in a cell culture of Norway spruce

    Directory of Open Access Journals (Sweden)

    Tino Warinowski

    2016-10-01

    Full Text Available Lignin, an important component of plant cell walls, is a polymer of monolignols derived from the phenylpropanoid pathway. Monolignols are oxidized in the cell wall by oxidative enzymes (peroxidases and/or laccases to radicals, which then couple with the growing lignin polymer. We have investigated the characteristics of the polymerization reaction by producing lignin polymers in vitro using different oxidative enzymes and analyzing the structures formed with NMR. The ability of the enzymes to oxidize a high-molecular-weight compounds was tested using cytochrome c as a substrate. The results support an idea that lignin structure is largely determined by the concentration ratios of the monolignol (coniferyl alcohol and polymer radicals involved in the coupling reaction. High rate of the lignin polymer oxidation compared to monolignol oxidation leads to a natural-like structure. The high relative rate can be achieved by an open active site of the oxidative enzyme, close proximity of the enzyme with the polymeric substrate or simply by high enzymatic activity that consumes monolignols rapidly. Monolignols, which are oxidized efficiently, can be seen as competitive inhibitors of polymer oxidation. Our results indicate that, at least in a Norway spruce (Picea abies L. Karst. cell culture, a group of apoplastic, polymer-oxidizing peroxidases bind to the lignin polymer and are responsible for production of natural-like lignin in cell suspension cultures in vivo, and also in vitro. The peroxidases bound to the extracellular lignin had the highest ability to bind to various cell wall polymers in vitro. Extracellular lignin contains pectin-type sugars, making them possible attachment points for these cationic peroxidases.

  6. Peroxidases Bound to the Growing Lignin Polymer Produce Natural Like Extracellular Lignin in a Cell Culture of Norway Spruce.

    Science.gov (United States)

    Warinowski, Tino; Koutaniemi, Sanna; Kärkönen, Anna; Sundberg, Ilari; Toikka, Merja; Simola, Liisa Kaarina; Kilpeläinen, Ilkka; Teeri, Teemu H

    2016-01-01

    Lignin, an important component of plant cell walls, is a polymer of monolignols derived from the phenylpropanoid pathway. Monolignols are oxidized in the cell wall by oxidative enzymes (peroxidases and/or laccases) to radicals, which then couple with the growing lignin polymer. We have investigated the characteristics of the polymerization reaction by producing lignin polymers in vitro using different oxidative enzymes and analyzing the structures formed with NMR. The ability of the enzymes to oxidize high-molecular-weight compounds was tested using cytochrome c as a substrate. The results support an idea that lignin structure is largely determined by the concentration ratios of the monolignol (coniferyl alcohol) and polymer radicals involved in the coupling reaction. High rate of the lignin polymer oxidation compared to monolignol oxidation leads to a natural-like structure. The high relative rate can be achieved by an open active site of the oxidative enzyme, close proximity of the enzyme with the polymeric substrate or simply by high enzymatic activity that consumes monolignols rapidly. Monolignols, which are oxidized efficiently, can be seen as competitive inhibitors of polymer oxidation. Our results indicate that, at least in a Norway spruce ( Picea abies L. Karst.) cell culture, a group of apoplastic, polymer-oxidizing peroxidases bind to the lignin polymer and are responsible for production of natural-like lignin in cell suspension cultures in vivo , and also in vitro . The peroxidases bound to the extracellular lignin had the highest ability to bind to various cell wall polymers in vitro . Extracellular lignin contains pectin-type sugars, making them possible attachment points for these cationic peroxidases.

  7. Uncertainty of pesticide residue concentration determined from ordinary and weighted linear regression curve.

    Science.gov (United States)

    Yolci Omeroglu, Perihan; Ambrus, Árpad; Boyacioglu, Dilek

    2018-03-28

    Determination of pesticide residues is based on calibration curves constructed for each batch of analysis. Calibration standard solutions are prepared from a known amount of reference material at different concentration levels covering the concentration range of the analyte in the analysed samples. In the scope of this study, the applicability of both ordinary linear and weighted linear regression (OLR and WLR) for pesticide residue analysis was investigated. We used 782 multipoint calibration curves obtained for 72 different analytical batches with high-pressure liquid chromatography equipped with an ultraviolet detector, and gas chromatography with electron capture, nitrogen phosphorus or mass spectrophotometer detectors. Quality criteria of the linear curves including regression coefficient, standard deviation of relative residuals and deviation of back calculated concentrations were calculated both for WLR and OLR methods. Moreover, the relative uncertainty of the predicted analyte concentration was estimated for both methods. It was concluded that calibration curve based on WLR complies with all the quality criteria set by international guidelines compared to those calculated with OLR. It means that all the data fit well with WLR for pesticide residue analysis. It was estimated that, regardless of the actual concentration range of the calibration, relative uncertainty at the lowest calibrated level ranged between 0.3% and 113.7% for OLR and between 0.2% and 22.1% for WLR. At or above 1/3 of the calibrated range, uncertainty of calibration curve ranged between 0.1% and 16.3% for OLR and 0% and 12.2% for WLR, and therefore, the two methods gave comparable results.

  8. Protocol Development and Equivalency Testing of the FACTS Procedure for Chlorine Residual Determination in Drinking Water.

    Science.gov (United States)

    1984-03-15

    l1 no . P .3tion was for electrode Aand sample 5. the B *Oe~~.1~.,.i.1 oidO I 1000611 ll600*0*l0 6i61 salu01II l.,0000 electrode determined a value...probability ant Residuals Pro. AW1A WQTC Dihaloacetanitriles b Chlorination , lev el ! in he uset] For a 95 percent Louisville Ky iDec 1978, Natural Waters Pro...Free As aitable Chlorine and Health Effects Pacifi, (;rn,. Cat!percent signific:an:e 1e el . i = 0 01 is DPD-Coiorimetrc DPD-Sleadifa( and Oct 19811 In

  9. A Simple and Rapid Extraction for Gas Chromatographic Determination of Thiabendazole and Imazalil Residues in Lemons

    Directory of Open Access Journals (Sweden)

    Navickiene Sandro

    2002-01-01

    Full Text Available A rapid and efficient method is described for the determination of thiabendazole and imazalil residues in lemons (peel and pulp. The procedure is based on the extraction with an hexane:ethyl acetate mixture (1:1, v/v and gas chromatographic analysis using thermionic specific detection (TSD. The possibility of matrix effect was also studied. Mean recoveries from 8 replicates of fortified samples ranged from 79% to 109%, with relative standard deviation values between 2.4% to 12.8%. The detection and quantification limits of the method were 0.2 mg kg-1 and 0.5 mg kg-1, respectively.

  10. Quantitative determination of pefloxacin mesylate by residual-base neutralisation method

    Directory of Open Access Journals (Sweden)

    HULIKALCHANDRA SHEKAR PRAMEELA

    2004-05-01

    Full Text Available This work describes two procedures based on residual base determination for the quantification of pefloxacin mesylate (PFM in bulk drug and in pharmaceutical products. In the first method involving titrimetry, the drug solution is treated with a measured excess of sodium hydroxide followed by back titration of the residual base with hydrochloric acid using a phenol red-bromothymol blue mixed indicator. The second spectrophotometrie method involves treatment of a fixed amount of sodium hydroxide – phenol red mixture with varying amounts of the drug, and measuring the decrease in the absorbance of the dye at 560 nm. In the titrimetric method, a reaction stoichiometry of 1:1 was found in the quantification range of 4–20 mg of drug. The spectrophotometric method allows the determination of PFM in the 5–40 mg ml-1 range. The molar absorptivity is 5.91¤103 l mol-1 cm-1 and the Sandell sensitivity is 56.37 ng cm-2. The methods were applied successfully to the determination of PFM in pharmaceutical preparations.

  11. Determination of oxyfluorfen herbicide and oxyfluorfen amine residues in garbanzo beans by liquid chromatography.

    Science.gov (United States)

    Zhou, M; Miles, C J

    1991-01-01

    Oxyfluorfen and oxyfluorfen amine were determined by liquid chromatography (LC) with ultraviolet (UV) and photoconductivity detection (PCD). A simple extraction procedure acceptably recovered both analytes from garbanzo beans over a wide range of fortifications (0.05 to 20 ppm) (83 +/- 4 for oxyfluorfen; 85 +/- 4 for oxyfluorfen amine). Percent recoveries decreased slightly as the fortification level decreased. Both analytes could be determined simultaneously at a concentration greater than 0.2 ppm in garbanzo beans. Detection limits were 3 ng for oxyfluorfen and 100 ng for oxyfluorfen amine using LC/UV, and 12 ng for both oxyfluorfen and oxyfluorfen amine with LC/PCD. Different knitted reaction coils and photoreactors were evaluated. Photoproduct yields and identification were determined by ion chromatography. The LC/PCD method measures oxyfluorfen and oxyfluorfen amine separately and has a shorter analysis time, while the standard method using gas chromatography measures total residues and is more sensitive.

  12. The determination of pesticide residues in local vegetables by means of neutron activation technique

    International Nuclear Information System (INIS)

    Mongkolphantha, S.; Karasuddhi, P.; Yamkate, P.; Serichareonsatit, N.

    1975-01-01

    Analytical methods based on neutron activation have been developed for studying pesticides residues of bromine, arsenic and mercury in local vegetables and fruits. The concentration of bromine, arsenic and mercury in samples are enriched prior to neutron irradiations by a technique of dry-ashing and freeze-drying for the determination of arsenic, bromine and mercury respectively. The element bromine is determined instrumentally while arsenic and mercury are determined destructively using a distillation technique. The limit of detection under the conditions used for bromine, arsenic and mercury as obtained are 0.01, 0.001 and 0.0001 microgram respectively. A total of 45 varieties of vegetables and 20 varieties of fruits are analyzed. The results of the investigation and the concentration range in part per million of bromine, arsenic and mercury are also presented

  13. Comparison between some determination methods of residual styrene in plastic scintillators

    International Nuclear Information System (INIS)

    Bezuglyi, V.D.; Ponomarev, Yu.P.; Gunder, O.A.; Biteman, V.B.; Senchishin, V.G.

    1988-01-01

    Scintillators made of plastic materials based on polystyrene with addition of p-terphenyl and 1,4-di-[(2,5-phenyl)oxazolyl] benzene have found wide application principally in the detection of radioactivity. The stability of the scintillating characteristics of these materials depends to great degree on the concentration of the residual monomer and for this reason it is important to have a sufficiently convenient method for the determination of this latter. We investigated the bromometric and acid-base titration methods with visual and potentiometric titration end point detection. We also examined the polarographic methods, direct and indirect, using the electroreduction of the mercury acetate complex of the monomer. We checked the methods on a scintillator sample and on synthetic mixtures, i.e., mixtures of monomer, polymer, and p-terphenyl. We compared the determination results for styrene and showed that the most accurate procedure is the bromometric determination with potentiometric indication of the end-point

  14. Characteristics of Lignin from Flax Shives as Affected by Extraction Conditions

    Science.gov (United States)

    Ross, Kelly; Mazza, Giuseppe

    2010-01-01

    Lignin, a polyphenolic molecule, is a major constituent of flax shives. This polyphenolic molecular structure renders lignin a potential source of a variety of commercially viable products such as fine chemicals. This work compares the performance of different lignin isolation methods. Lignin from flax shive was isolated using both conventional alkaline extraction method and a novel experimental pressurized low polarity water (PLPW) extraction process. The lignin yields and chemical composition of the lignin fractions were determined. The conventional alkali treatment with 1.25 M NaOH, heated at 80 °C for 5 h, extracted 92 g lignin per kg flax shives, while lignin yields from the PLPW extracts ranged from 27 to 241 g lignin per kg flax shives. The purity and monomeric composition of the lignins obtained from the different extraction conditions was assessed via UV spectroscopy and alkaline nitrobenzene oxidation. Lignin obtained from conventional alkali treatment with 1.25 M NaOH, heated at 80 °C for 5 h was of low purity and exhibited the lowest yields of nitrobenzene oxidation products. With respect to alkali assisted PLPW extractions, temperature created an opposing effect on lignin yield and nitrobenzene oxidation products. More lignin was extracted as temperature increased, yet the yield of nitrobenzene oxidation products decreased. The low yield of nitrobenzene oxidation products may be attributed to either the formation of condensed structures or the selective dissolution of condensed structures of lignin during the pressurized alkaline high temperature treatment. Analytical pyrolysis, using pyroprobe GC-MS, was used to investigate the molecular composition of the lignin samples. The total yield of pyrolysis lignin products was 13.3, 64.7, and 30.5% for the 1.25 M NaOH extracted lignin, alkaline assisted PLPW extracted lignin, and the unprocessed flax shives, respectively. Key lignin derived compounds such as guaiacol, 4-vinyl guaiacol, 4-methyl guaiacol

  15. Characteristics of Lignin from Flax Shives as Affected by Extraction Conditions

    Directory of Open Access Journals (Sweden)

    Kelly Ross

    2010-10-01

    Full Text Available Lignin, a polyphenolic molecule, is a major constituent of flax shives. This polyphenolic molecular structure renders lignin a potential source of a variety of commercially viable products such as fine chemicals. This work compares the performance of different lignin isolation methods. Lignin from flax shive was isolated using both conventional alkaline extraction method and a novel experimental pressurized low polarity water (PLPW extraction process. The lignin yields and chemical composition of the lignin fractions were determined. The conventional alkali treatment with 1.25 M NaOH, heated at 80 °C for 5 h, extracted 92 g lignin per kg flax shives, while lignin yields from the PLPW extracts ranged from 27 to 241 g lignin per kg flax shives. The purity and monomeric composition of the lignins obtained from the different extraction conditions was assessed via UV spectroscopy and alkaline nitrobenzene oxidation. Lignin obtained from conventional alkali treatment with 1.25 M NaOH, heated at 80 °C for 5 h was of low purity and exhibited the lowest yields of nitrobenzene oxidation products. With respect to alkali assisted PLPW extractions, temperature created an opposing effect on lignin yield and nitrobenzene oxidation products. More lignin was extracted as temperature increased, yet the yield of nitrobenzene oxidation products decreased. The low yield of nitrobenzene oxidation products may be attributed to either the formation of condensed structures or the selective dissolution of condensed structures of lignin during the pressurized alkaline high temperature treatment. Analytical pyrolysis, using pyroprobe GC-MS, was used to investigate the molecular composition of the lignin samples. The total yield of pyrolysis lignin products was 13.3, 64.7, and 30.5% for the 1.25 M NaOH extracted lignin, alkaline assisted PLPW extracted lignin, and the unprocessed flax shives, respectively. Key lignin derived compounds such as guaiacol, 4-vinyl guaiacol, 4

  16. Immunologic determination of chloramphenicol residue in commercial birds at Nsukka, Enugu State, Southeast Nigeria

    Directory of Open Access Journals (Sweden)

    Ekene Vivienne Ezenduka

    2018-04-01

    Full Text Available Aim: This study aimed to determine the presence and prevalence of chloramphenicol (CAP, a drug which was banned for use in food-producing animals due to many side effects residue in commercial birds slaughtered at Ikpa abattoir and its awareness and usage in farms at Nsukka, Enugu State, Nigeria. Materials and Methods: A cross-sectional survey was done with the use of a questionnaire on usage and awareness of CAP and screening for its presence in commercial poultry in the study area. The questionnaire was supplied to 35 commercial farms, and liver samples from 300 commercial broilers were analyzed using an enzyme-linked immunosorbent assay technique; the prevalence was then determined. Results: Of the 35 farms evaluated, 33 (94% responded. In the management practice, 57.6% of the farms use intensive deep litter, 18.2% intensive battery cage, and 24.2% extensive farming system. 19 (69.7% farms rear only broilers, 12.1% layers, and 15.1% both. The feeding management showed that 21.1% of farmers produce their own feed with inclusion of antibiotics while 78.8% use commercial feed, of which 11.5% incorporate antibiotics. The findings also showed that 54.4% of the respondents use CAP and only 30.3% are aware of the consequences of antimicrobial residue in food and have knowledge of the legislation on the prudent use of antimicrobials in food animals. Of the 300 samples screened for CAP residue, 18.7% were positive with concentrations ranging from 0.5 to 6.2 parts per billion. Conclusion: CAP is still very much in use in the study area, despite the ban, and it is present in the tissues of commercial birds meant for human consumption.

  17. An overview of the main foodstuff sample preparation technologies for tetracycline residue determination.

    Science.gov (United States)

    Pérez-Rodríguez, Michael; Pellerano, Roberto Gerardo; Pezza, Leonardo; Pezza, Helena Redigolo

    2018-05-15

    Tetracyclines are widely used for both the treatment and prevention of diseases in animals as well as for the promotion of rapid animal growth and weight gain. This practice may result in trace amounts of these drugs in products of animal origin, such as milk and eggs, posing serious risks to human health. The presence of tetracycline residues in foods can lead to the transmission of antibiotic-resistant pathogenic bacteria through the food chain. In order to ensure food safety and avoid exposure to these substances, national and international regulatory agencies have established tolerance levels for authorized veterinary drugs, including tetracycline antimicrobials. In view of that, numerous sensitive and specific methods have been developed for the quantification of these compounds in different food matrices. One will note, however, that the determination of trace residues in foods such as milk and eggs often requires extensive sample extraction and preparation prior to conducting instrumental analysis. Sample pretreatment is usually the most complicated step in the analytical process and covers both cleaning and pre-concentration. Optimal sample preparation can reduce analysis time and sources of error, enhance sensitivity, apart from enabling unequivocal identification, confirmation and quantification of target analytes. The development and implementation of more environmentally friendly analytical procedures, which involve the use of less hazardous solvents and smaller sample sizes compared to traditional methods, is a rapidly increasing trend in analytical chemistry. This review seeks to provide an updated overview of the main trends in sample preparation for the determination of tetracycline residues in foodstuffs. The applicability of several extraction and clean-up techniques employed in the analysis of foodstuffs, especially milk and egg samples, is also thoroughly discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Influence of RANEY Nickel on the Formation of Intermediates in the Degradation of Lignin

    Directory of Open Access Journals (Sweden)

    Daniel Forchheim

    2012-01-01

    Full Text Available Lignin forms an important part of lignocellulosic biomass and is an abundantly available residue. It is a potential renewable source of phenol. Liquefaction of enzymatic hydrolysis lignin as well as catalytical hydrodeoxygenation of the main intermediates in the degradation of lignin, that is, catechol and guaiacol, was studied. The cleavage of the ether bonds, which are abundant in the molecular structure of lignin, can be realised in near-critical water (573 to 673 K, 20 to 30 MPa. Hydrothermal treatment in this context provides high selectivity in respect to hydroxybenzenes, especially catechol. RANEY Nickel was found to be an adequate catalyst for hydrodeoxygenation. Although it does not influence the cleavage of ether bonds, RANEY Nickel favours the production of phenol from both lignin and catechol. The main product from hydrodeoxygenation of guaiacol with RANEY Nickel was cyclohexanol. Reaction mechanism and kinetics of the degradation of guaiacol were explored.

  19. Fundamental understanding of distracted oxygen delignification efficiency by dissolved lignin during biorefinery process of eucalyptus.

    Science.gov (United States)

    Zhao, Huifang; Li, Jing; Zhang, Xuejin

    2018-02-27

    In this work, a fundamental understanding of oxygen delignification distracted by dissolved lignin was investigated. In the new biorefinery model of shortening kraft pulping integrated with extended oxygen delignification process, increasing content of residual lignin in the original pulp could result in enhanced delignification efficiency, higher pulp viscosity and less carbonyl groups. However, the invalid oxygen consumption by dissolved lignin could be increased with the increase of process temperature and alkali dosage. The normalized ultraviolet absorbance (divided by absorbance at 280 nm) also showed that the content of chromophoric group in dissolved lignin decreased with oxygen delignification proceeded, both of which indicated that dissolved lignin could enhance the invalid oxygen consumption. Therefore, a conclusion that replacement of the liquor at the initial phase of oxygen delignification process would balance the enhancement of delignification efficiency and invalid oxygen consumption was achieved. Copyright © 2018 Elsevier Ltd. All rights reserved.

  20. Determination of erythromycin and tylosin residues in honey by LC/MS/MS.

    Science.gov (United States)

    Granja, Rodrigo; Niño, Alfredo Montes; Zucchetti, Roberto; Niño, Rosario Montes; Patel, Raj; Salerno, Alessandro Gonzalez

    2009-01-01

    Antibiotics are used in apiculture to protect bees against a variety of brood diseases. As a result of the development of resistance to oxytetracycline, erythromycin and tylosin are increasingly used for the prevention and treatment of these diseases. Therefore, Brazilian authorities have added these antibiotics to the National Regulatory Monitoring Program for the control of residues in honey. An analytical method has been developed for the determination of residues of erythromycin and tylosin in honey. The procedure involves solid-phase extraction of diluted honey samples with Bond Elut cartridges, followed by LC/MS with electrospray positive ionization in the multiple reaction monitoring mode. Two characteristic transitions were monitored for both drugs. Average analyte recoveries of erythromycin and tylosin ranged from 99 to 109% from sets of replicate honey samples fortified with drug concentrations of 5, 10, 15, and 20 microg/kg. The method decision limits were determined to be 1.27 and 0.59 microg/kg for erythromycin and tylosin, respectively. The detection capabilities were 5 and 5.2 microg/kg for erythromycin and tylosin, respectively.

  1. Gravimetric quantitative determination of packaging residues in feed from former food.

    Science.gov (United States)

    Amato, Giuseppina; Desiato, Rosanna; Giovannini, Tiziana; Pinotti, Luciano; Tretola, Marco; Gili, Marilena; Marchis, Daniela

    2017-08-01

    Valorisation of former foodstuff products (FFP) in feed is part of a long-term strategy for sustainability. An approach to valorise FFP outside the waste value chain is their use as an alternative source of feed materials, with a subsequent optimisation of the environmental impact of products. In the current practice of food production, food packaging is provided to ensure the maintenance of food quality and safety during transport and storage. One of the problems of reusing FFP is how to deal with packaging materials or remains that can become residues in the feed. The aim of this study is to propose a fast and sensitive gravimetric method, fit for routine official controls, for the determination of packaging residues in feed. The developed method can briefly be summarised as: (1) visual selection of the undesired ingredients which can be identified as remnants of packaging materials; (2) weighing of the selected materials; (3) defatting; (4) dehydration; (5) final weighing; and (6) reporting of weight and percentage. Moreover, the method has been validated through the determination of some of the parameters listed in Council Regulation 2004/882/EC (i.e., specificity, limit of quantification (LOQ), recovery, repeatability, within-laboratory reproducibility and measurement uncertainty).

  2. Proposal of methodology for determining of potential residual biomass for agriculture and forestry in Slovak republic

    Directory of Open Access Journals (Sweden)

    Štefan Kuzevič

    2013-11-01

    Full Text Available The issue of efficient use of biomass as a renewable source of energy in the process of sustainable development of every country is a problem that is often tackled nowadays being also imposed by the legislation of the European Union. In the process of the accession to the EU, the Slovak republic incorporated the obligations as defined by the EU Directive 2001/77/EC on the promotion of electricity produced from renewable energy sources. Out of all the renewable sources of energy, biomass has the greatest economic potential to be used on the territory of Slovakia. The use of biomass for the purposes of electricity generation is the most promising alternative to generate not only thermal but also electrical energy. This paper presents the proposal of methodology developed to determine the utilization potential of residual biomass in the sectors of forestry and agriculture within a certain area of eastern Slovakia. The theoretical proposal is developed based on using Corine Land Cover. The application of Corine Land Cover and GIS tools made it possible to effectively determine residual biomass for the selected sectors of the economy.

  3. Determination the Amount of Illegal Furazolidone Residues in Broilers in Ahvaz Abattoir by HPLC Method

    Directory of Open Access Journals (Sweden)

    A Fazlara

    2014-06-01

    Full Text Available Background & aim: due to the risks to human health, particularly in terms of carcinogenicity, the application of Furazolidone in animals which their products are consumed by human population is strongly prohibited. The purpose of this study was to determine the amount of unauthorized furazolidone in broiler chickens slaughtered in Ahvaz by using HPLC. Methods: In the present cross-sectional study which was conducted within six months, 100 broiler carcasses were randomly collected from Ahvaz slaughterhouses. Then by using ice, the carcasses were transported to the laboratory in less than 24 hours inorder to illicit the amount of furazolidone drug by the HPLC method. After extraction and degrading processes, using Ethyl-acetate and related protocols for isolation of Furazolidone from muscles, and also calibrating HPLC system to obtain standard curves, the amount of 20 microliters of each sample was injected to the HPLC device and the amounts of Furazolidone were determined in the mixture of pectoral and femoral muscles. Finally the obtained results were statistically analysed by using one sample t-test in the SPSS software. Results: The mean Furazolidone concentration in the mixture of femoral and thorasic muscles was 28.15±2.37 mg/kg. Thirty-nine percent of the samples were positive for containing illegal Furazolidone residue. Conclusion: According to the results of the current study, more attention is seriously recommended by authorized responsibilities to prevent the antibiotic residues such as furazolidone in poultry meat.

  4. Standard Test Method for Gravimetric Determination of Nonvolatile Residue (NVR) in Environmentally Controlled Areas for Spacecraft

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2008-01-01

    1.1 This test method covers the determination of nonvolatile residue (NVR) fallout in environmentally controlled areas used for the assembly, testing, and processing of spacecraft. 1.2 The NVR of interest is that which is deposited on sampling plate surfaces at room temperature: it is left to the user to infer the relationship between the NVR found on the sampling plate surface and that found on any other surfaces. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

  5. Standard Test Method for Gravimetric Determination of Nonvolatile Residue From Cleanroom Wipers

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 This test method covers the determination of solvent extractable nonvolatile residue (NVR) from wipers used in assembly, cleaning, or testing of spacecraft, but not from those used for analytical surface sampling of hardware. 1.2 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard. 1.3 The NVR of interest is that which can be extracted from cleanroom wipers using a specified solvent that has been selected for its extractive qualities. Alternative solvents may be selected, but since their use may result in different values being generated, they must be identified in the procedure data sheet. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  6. The procedure for determining the residual life of high-temperature aggregates

    Science.gov (United States)

    Nikiforov, A. S.; Prihodko, E. V.; Kinzhibekova, A. K.; Karmanov, A. E.

    2018-01-01

    One of the main reasons for the withdrawal of high-temperature aggregates for repairs is the destruction of enclosing structures due to the occurrence of temperature stresses. A wide range of refractory materials used, a large number of product names, a difference in the operation of even the same aggregates makes it impossible to apply general principles for determining the residual resource of high-temperature aggregates, which is based, as a rule, on the determination of temperature stresses. In the article there is suggested a technique based on the method of simulation modeling, allowing to estimate the remaining resource and reliability of the operating equipment. There are given data on the calculation of these indicators for a 25-ton steel-casting ladle. The values obtained make it possible to evaluate the rationality of the further operation of the high-temperature unit by the condition of reliability of the enclosing structures.

  7. Determination of Diphenylamine in Gunshot Residue by HPLC-MS/MS

    Directory of Open Access Journals (Sweden)

    Hongcheng Mei

    2016-01-01

    Full Text Available A high performance liquid chromatography tandem mass spectrometry/mass spectrometry (HPLC-MS/MS protocol was developed for the determination of diphenylamine (DPA. Four productions of DPA were selected for qualitative assay and the peak area of the main product ion for quantitation. By means of separation using an Agilent Extend-C18 column (CA, USA (150 mm × 4.6 mm, 5 μm with methanol-water (90:10 as the mobile phase, DPA was detected by electrospray ionization (ESI tandem mass spectrometry in positive mode. The linearity of the peak area versus concentration ranged 5-500 ng/mL, r 2 = 0.9978. The limit of detection (S/N =3 of this method was 0.3 ng/mL. This method is applicable for the determination of DPA in gunshot residue.

  8. [Study on determination of anthraquinones in dachengqi tang residues of Magnolia officinalis and Citrus aurantium removed in decoction process].

    Science.gov (United States)

    Wang, Yue-Sheng; Deng, Jie-Hua; Wei, Hui-Zhen; Rao, Yi; Shen, Feng-Yun; Jin, Hao-Xin

    2013-03-01

    The traditional decoction method of Dachengqi Tang is that "First boiling Magnolia officinalis and Citrus aurantium with a pipeful of water, taking out five litres from the decoction, removing residues, adding rheum officinale, boiling again, taking out two litres from it, removing residues, adding mirabilite, boiling it with low fire". According to it, residues of M. officinalis and C. aurantium should be removed after decocting. This essay aims to study the content of anthraquinones, in order to proof whether the removal of residues of M. officinalis and C. aurantium is scientific. The traditional method was adopted to prepare Dachengqi Tang. Decoction A (original method) was obtained by removing residues of M. officinalis and C. aurantium, whereas decoction B was obtained without removing residues of M. officinalis and C. aurantium. The content of anthraquinones of both methods was determined with HPLC. The content of both combined and free anthraquinones in decoction A was higher than that of decoction B. The content of total anthraquinones in residues of decoction A was lower than that of residue B. The traditional decoction method of removing residues of M. officinalis and C. aurantium from Dachengqi Tang is scientific, because it improves the dissolution rate of effective ingredients, which provides a theoretical basis for effective substances of the drug.

  9. Isolation, identification and characterization of lignin-degrading bacteria from Qinling, China.

    Science.gov (United States)

    Yang, C-X; Wang, T; Gao, L-N; Yin, H-J; Lü, X

    2017-12-01

    Lignin is an aromatic heteropolymer forming a physical barrier and it is a big challenge in biomass utilization. This paper first investigated lignin-degradation bacteria from rotten wood in Qinling Mountain. Nineteen potential strains were selected and ligninolytic enzyme activities were determined over 84 h. Strains that had higher enzyme activities were selected. Further, the biodegradation of wheat straw lignin and alkali lignin was evaluated indicating that Burkholderia sp. H1 had the highest capability. It was confirmed by gel permeation chromatography and field emission scanning electron microscope that alkali lignin was depolymerized into small fragments. The degraded products were analysed using gas chromatography-mass spectrometry. The total ion chromatograph of products treated for 7 days showed the formation of aromatic compounds, an important intermediate from lignin degradation. Interestingly, they disappeared in 15 days while the aldehyde and ester compounds increased. The results suggest that the lignin-degrading bacteria are abundant in rotten wood and strain H1 has high potential to break down lignin. The diversity of lignin-degrading bacteria in Qinling Mountain is revealed. The study of Burkholderia sp. H1 expands the range of bacteria for lignin degradation and provides novel bacteria for application to lignocellulosic biomass. © 2017 The Society for Applied Microbiology.

  10. Reinforcing styrene butadiene rubber with lignin-novolac epoxy resin networks

    Directory of Open Access Journals (Sweden)

    P. Yu

    2015-01-01

    Full Text Available In this study, lignin-novolac epoxy resin networks were fabricated in the styrene butadiene rubber (SBR matrix by combination of latex compounding and melt mixing. Firstly, SBR/lignin compounds were co-coagulated by SBR latex and lignin aqueous solution. Then the novolac epoxy resin (F51 was added in the SBR/lignin compounds by melt compounding method. F51 was directly cured by lignin via the ring-opening reaction of epoxy groups of F51 and OH groups (or COOH groups of lignin during the curing process of rubber compounds, as was particularly evident from Fourier transform infrared spectroscopy (FTIR studies and maximum torque of the curing analysis. The existence of lignin-F51 networks were also detected by scanning electron microscope (SEM and dynamic mechanical analysis (DMA. The structure of the SBR/lignin/F51 was also characterized by rubber process analyzer (RPA, thermogravimetric analysis (TGA and determination of crosslinking density. Due to rigid lignin-F51 networks achieved in SBR/lignin/F51 composites, it was found that the hardness, modulus, tear strength, crosslinking density, the temperature of 5 and 10% weight-loss were significantly enhanced with the loading of F51.

  11. Determining the Residual Cypermethrin, Permethrin, Indoxacarb and Mancozeb in Tomato Produced in Bushehr Province Farms

    Directory of Open Access Journals (Sweden)

    Maimanat Tobeh Khak

    2016-05-01

    Full Text Available Food is necessary for a healthy lifestyle, but it’s an important way of spreading many pathogens and toxic chemicals. The food contamination may happen during planting, harvesting, storing, processing or transporting. Hence, the food quality monitoring is necessary. Plants constitute the main source of food for human being. Fighting against pests and plant diseases in some cases, prevents product loss. It is obvious that the pest control is crucial for the future agriculture, industry and hygiene. Despite the current discussions and critics in scientific conventions about the adverse effects of pesticide use on human life, chemical based methods of pest control are still the most common among the farmers. Pesticide residues in agricultural products due to inappropriate and excessive consumption of pesticides is a worldwide problem that has overshadowed the health of human societies (1. Bushehr province, according to its weather conditions, is one of the major tomato growers in the country in autumn and winter. In this study, the residues of 9 toxins (Cypermethrin, Permethrin, Indoxacarb And Mancozeb, Chlorothalonil, Iprodione, Thiophanate methyl, Carbendazim Golsam, and Abamectin has been investigated in 37 Tomato samples from the farms of Jam, Dashtestan, Dashti, Deir and kangan cities, and Except Abamectin other toxins were detected. Cypermethrin rate was higher than standard in 2.8% of the samples. The residues of Permethrin, Indoxacarb, Mancozeb, Chlorothalonil, Iprodione and Thiophanate methyl was lower than the allowed limits in all the samples. The amount of Carbendazim was determined to be higher than the allowed limits in 4.8% of the samples.

  12. A radioimmunoassay for lignin in plant cell walls

    Energy Technology Data Exchange (ETDEWEB)

    Dawley, R.M.

    1989-01-01

    Lignin detection and determination in herbaceous tissue requires selective, specific assays which are not currently available. A radioimmunoassay (RIA) was developed to study lignin metabolism in these tissues. A {beta}-aryl ether lignin model compound was synthesized, linked to keyhole limpet hemocyanin using a water-soluble carbodiimide, and injected into rabbits. The highest titer of the antiserum obtained was 34 {eta}g/mL of model derivatized BSA. An in vitro system was developed to characterize the RIA. The model compound was linked to amino activated polyacrylamide beads to mimic lignin in the cell walls. {sup 125}I Radiolabelled protein A was used to detect IgG antibody binding. The RIA was shown in the in vitro system to exhibit saturable binding. The amount of antibody bound decreased when the serum was diluted. Immunoelectrophoresis and competitive binding experiments confirmed that both aromatic rings of the lignin model compound had been antigenic. Chlorogenic acid, a phenolic known to be present in plant cells, did not compete for antibody binding. The RIA was used to measure lignin in milled plant samples and barley seedlings. Antiserum binding to wheat cell walls and stressed barley segments was higher than preimmune serum binding. Antibody binding to stressed barley tissue decreased following NaClO{sub 2} delignification. The RIA was found to be less sensitive than expected, so several avenues for improving the method are discussed.

  13. Lignin-degrading enzyme activities.

    Science.gov (United States)

    Chen, Yi-ru; Sarkanen, Simo; Wang, Yun-Yan

    2012-01-01

    Over the past three decades, the activities of four kinds of enzyme have been purported to furnish the mechanistic foundations for macromolecular lignin depolymerization in decaying plant cell walls. The pertinent fungal enzymes comprise lignin peroxidase (with a relatively high redox potential), manganese peroxidase, an alkyl aryl etherase, and laccase. The peroxidases and laccase, but not the etherase, are expressed extracellularly by white-rot fungi. A number of these microorganisms exhibit a marked preference toward lignin in their degradation of lignocellulose. Interestingly, some white-rot fungi secrete both kinds of peroxidase but no laccase, while others that are equally effective express extracellular laccase activity but no peroxidases. Actually, none of these enzymes has been reported to possess significant depolymerase activity toward macromolecular lignin substrates that are derived with little chemical modification from the native biopolymer. Here, the assays commonly employed for monitoring the traditional fungal peroxidases, alkyl aryl etherase, and laccase are described in their respective contexts. A soluble native polymeric substrate that can be isolated directly from a conventional milled-wood lignin preparation is characterized in relation to its utility in next-generation lignin-depolymerase assays.

  14. Determination of an acceptable assimilable organic carbon (AOC) level for biological stability in water distribution systems with minimized chlorine residual.

    Science.gov (United States)

    Ohkouchi, Yumiko; Ly, Bich Thuy; Ishikawa, Suguru; Kawano, Yoshihiro; Itoh, Sadahiko

    2013-02-01

    There is considerable interest in minimizing the chlorine residual in Japan because of increasing complaints about a chlorinous odor in drinking water. However, minimizing the chlorine residual causes the microbiological water quality to deteriorate, and stricter control of biodegradable organics in finished water is thus needed to maintain biological stability during water distribution. In this investigation, an acceptable level of assimilable organic carbon (AOC) for biologically stable water with minimized chlorine residual was determined based on the relationship between AOC, the chlorine residual, and bacterial regrowth. In order to prepare water samples containing lower AOC, the fractions of AOC and biodegradable organic matter (BOM) in tap water samples were reduced by converting into biomass after thermal hydrolysis of BOM at alkaline conditions. The batch-mode incubations at different conditions of AOC and chlorine residual were carried out at 20 °C, and the presence or absence of bacterial regrowth was determined. The determined curve for biologically stable water indicated that the acceptable AOC was 10.9 μg C/L at a minimized chlorine residual (0.05 mg Cl(2)/L). This result indicated that AOC removal during current water treatment processes in Japan should be significantly enhanced prior to minimization of the chlorine residual in water distribution.

  15. [Determination of residual toluene diisocyanate in sponge bra by gas chromatography].

    Science.gov (United States)

    Wang, Aixia; Ye, Ping; Huang, Nan; Chen, Yan; Li, Xinggen

    2017-06-08

    A gas chromatography (GC) with internal standard method was developed for the determination of residual toluene diisocyanate (TDI) in sponge bra. The samples were extracted with ethyl acetate dehydrated, and cleaned up with 0.22 μm microfiltration membrane. The residual toluene diisocyanate was separated on a DB-624 capillary column using temperature programming. The flame ionization detector (FID) was used at 250 ℃. The inlet temperature was 180 ℃ with nitrogen as carrier gas. The linear range was 10-200 mg/L ( R 2 =0.9989) for TDI. The average recovery ranged from 80.5% to 91.6% with RSD not more than 7.9%( n =6). The limit of detection (LOD) and limit of quantification (LOQ) were 10 mg/kg and 100 mg/kg, respectively. The developed method was then utilized to analyse the 100 batches of sponge bra samples from the manufacturing enterprises, the entity shops and electric business platforms. The method is simple, time-saving and environment friendly with high sensitivity and good reproducibility, and has practical application value due to its low-cost and short-circle.

  16. Application of Scharer's quantitative method for the determination of residual alkaline phosphatase activity in standard Minas

    Directory of Open Access Journals (Sweden)

    C.F. Soares

    2013-08-01

    Full Text Available Milk pasteurization is a critical issue in the dairy industry, and failures in this process can affect final product safety. Scharer's enzymatic method is still traditionally used to verify pasteurization efficiency compliance, and it is based on screening for residual alkaline phosphatase in milk. Although several methods are used to quantify enzymatic activity to assess milk pasteurization efficiency, there is a small amount of published data regarding the use of these methods to quantify alkaline phosphatase in cheese. In this study, the Scharer's modified method was used to determine the levels of residual alkaline phosphatase in standard minas cheese, before and after 20 days of ripening. The cheeses were made using raw or pasteurized milk with the addition of different concentrations of raw milk (0; 0.05%; 0.10%; 0.20%; and 0.50%. In the fresh cheese samples, the method showed a sensitivity of only 0.50% with the addition of raw milk to the pasteurized milk used to make cheese. In addition, levels of up 0.20% of raw milk in pasteurized milk, the concentrations of phenol was inferior to 1μg phenol/g of dairy product which is the preconized indicator value for adequate pasteurization.

  17. Neutron and ultrasonic determination of residual stress in an aluminum ring-plug

    International Nuclear Information System (INIS)

    Prask, H.J.; Gnaeupel-Herold, T.; Clark, A.V.; Hehman, C.S.; Nguyen, T.N.

    2000-01-01

    Stress is a principal cause of material failure. This has been a well-recognized problem for decades, yet--in general--neutron diffraction remains the only way to measure sub-surface residual stresses without destroying the component. A field-portable ultrasonic strain-meter is being developed at NIST (Boulder) to determine residual stresses in engineering specimens, nondestructively. To test this and other techniques an array of stress-measurement standards are being prepared. These will be characterized by neutron diffraction and then used to evaluate, quantitatively, the potential of new methods. The first standard specimen produced for this purpose is a large shrink-fit ring-plug of 2024 aluminum (305 mm OD, 25.4 mm thick, 101.6 mm diameter plug). Because of large grain size, a sample-rotation averaging technique was developed to make reliable neutron measurements possible. A comparison of the neutron diffraction and ultrasonic results for this specimen will be presented, along with strain gauge results

  18. Integrated disposable electrochemical immunosensors for the simultaneous determination of sulfonamide and tetracycline antibiotics residues in milk.

    Science.gov (United States)

    Conzuelo, Felipe; Campuzano, Susana; Gamella, María; Pinacho, Daniel G; Reviejo, A Julio; Marco, M Pilar; Pingarrón, José M

    2013-12-15

    The design, preparation and analytical performance of a novel integrated amperometric immunosensor based on the immobilization of selective capture antibodies on the surface of Protein G-modified screen-printed dual carbon electrodes (SPdCEs) for the multiplexed determination of sulfonamide and tetracycline antibiotics residues in milk is reported in this work. Protein G was covalently immobilized onto a 4-aminobenzoic acid (4-ABA) film grafted on the disposable electrode, and a direct competitive immunoassay using horseradish peroxidase (HRP)-labeled tracers was performed. The amperometric responses measured at -0.2 V vs. the silver pseudo-reference electrode of the SPdCE upon the addition of H2O2 in the presence of hydroquinone (HQ) as mediator were used to monitor the extent of the immunoreactions. The developed methodology showed very low limits of detection (in the low ppb level) for sulfonamide and tetracycline antibiotics tested in untreated milk samples, and a good selectivity against other antibiotic residues frequently detected in milk and dairy products. The usefulness of the dual immunosensor was demonstrated by analyzing spiked milk samples as well as a reference milk containing a certified oxytetracycline (OTC) content. Good recoveries were attained in an analysis time of 30 min. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. Higher acid-chlorite reactivity of cell corner middle lamella lignin in black spruce

    Science.gov (United States)

    Umesh P. Agarwal

    2007-01-01

    To determine if there was a delignification behavior difference between secondary wall (S2) and middle lamella (cell corner or CC) lignin, black spruce cross-sections were acid-chlorite delignified and the tissue was evaluated in-situ by Raman imaging. Lignin concentration in S2 and CC was determined in numerous latewood cell areas in the two hour delignified cross...

  20. REVIEW ARTICLE: Determination of residual stresses in materials and industrial components by neutron diffraction

    Science.gov (United States)

    Albertini, Gianni; Bruno, Giovanni; Carradò, Adele; Fiori, Fabrizio; Rogante, Massimo; Rustichelli, Franco

    1999-03-01

    We present a review of the determination of residual stresses in materials and components of industrial interest by using the non-destructive technique of neutron diffraction. The fundamental aspects are discussed, together with a brief description of the experimental facilities. Several experimental results are then reported, particularly concerning applications to materials and components for power plants (CrMo steel, AISI304 stainless steel and 2.25Cr1Mo ferritic steel), aerospace and automotive technology (Al alloys, metal matrix composites, nickel superalloy gas-turbine components) and fusion-reactor technology (AISI316L for the first wall). A few thermomechanical treatments are considered, such as welding, cold-expanded holes, thermoelastic coupling and thermal and mechanical fatigue. Moreover, a few applications to general industrial problems are shown, namely brazed ceramic-steel components, coatings and fatigue-cracked samples. In some cases, experimental results are compared with numerical models or results from x-ray diffraction measurements.

  1. Bio-based polyurethane prepared from Kraft lignin and modified castor oil

    OpenAIRE

    L. B. Tavares; C. V. Boas; G. R. Schleder; A. M. Nacas; D. S. Rosa; D. J. Santos

    2016-01-01

    Current challenges highlight the need for polymer research using renewable natural sources as a substitute for petroleum-based polymers. The use of polyols obtained from renewable sources combined with the reuse of industrial residues such as lignin is an important agent in this process. Different compositions of polyurethane-type materials were prepared by combining technical Kraft lignin (TKL) with castor oil (CO) or modified castor oil (MCO1 and MCO2) to increase their reactivity towards d...

  2. Lignin modification in the initial phase of softwood kraft pulp delignification with polyoxometalates (POMs)

    Science.gov (United States)

    Biljana Bujanovic; Sally A. Ralph; Richard S. Reiner; Rajai H. Atalla

    2007-01-01

    Commercial softwood kraft pulp with kappa number 30.5 (KP30.5) was delignified with polyoxometalates (POM, Na5(+2)[SiV1(-0.1)MoW10(+0.1)O40]), and POM-treated kraft pulp of kappa number 23.6 was obtained (KPPOM,23.6). Residual lignin from pulps was isolated by mild acid hydrolysis and characterized by analytical and spectral methods to gain insight into lignin...

  3. Determination and residual characteristic of alkylphenols in household food detergents of Taiwan.

    Science.gov (United States)

    Pan, Yi-Ping; Tsai, Shih-Wei

    2009-07-01

    The non-ionic surfactants are mostly composed of alkylphenols for the ingredients of synthetic food detergents. Due to the ability to mimic hormones, it has been noticed that the exposures of alkylphenols might cause a variety of adverse effects. To assess the associate risks from possible exposures, concentrations of alkylphenols, including 4-nonylphenol (4-NP), technical nonylphenol isomers (t-NP(S)), and 4-tert-octylphenol (4-t-OP), in household food detergents of Taiwan were determined. Gas chromatography with mass spectrometer (GC/MS) was used to analyze alkylphenols in samples. The Taguchi experimental design was utilized to study the possible factors that might affect the residual characteristics of alkylphenols from detergents on dishware and fruits. By the analysis of variance, the orders of importance of different parameters were determined. The results showed that the concentrations of alkylphenols in food detergents ranged from 1.71 x 10(-5) to 2.13 x 10(-3) (APs/detergent, mgg(-1)). For residual characteristics, the cleaning temperature was found to be the only significant factor that will affect the 4-t-OP left on the dishware, while the concentrations of detergents used will affect the left of t-NPs and 4-NP on dishware as well. On the other hand, the varieties of fruits, the concentrations of detergents, and the concentrations of alkylphenols were found to have significant effects for the t-NPs left on fruits. As for the exposure assessments, the maximum dose of APs exposures from the use of household food detergents in Taiwan was also estimated in the study.

  4. Performance of biofuel processes utilising separate lignin and carbohydrate processing.

    Science.gov (United States)

    Melin, Kristian; Kohl, Thomas; Koskinen, Jukka; Hurme, Markku

    2015-09-01

    Novel biofuel pathways with increased product yields are evaluated against conventional lignocellulosic biofuel production processes: methanol or methane production via gasification and ethanol production via steam-explosion pre-treatment. The novel processes studied are ethanol production combined with methanol production by gasification, hydrocarbon fuel production with additional hydrogen produced from lignin residue gasification, methanol or methane synthesis using synthesis gas from lignin residue gasification and additional hydrogen obtained by aqueous phase reforming in synthesis gas production. The material and energy balances of the processes were calculated by Aspen flow sheet models and add on excel calculations applicable at the conceptual design stage to evaluate the pre-feasibility of the alternatives. The processes were compared using the following criteria: energy efficiency from biomass to products, primary energy efficiency, GHG reduction potential and economy (expressed as net present value: NPV). Several novel biorefinery concepts gave higher energy yields, GHG reduction potential and NPV. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. Morphology, Tensile Strength and Oil Resistance of Gum Rubber Sheets Prepared from Lignin Modified Natural Rubber

    Directory of Open Access Journals (Sweden)

    Asrul M.

    2014-07-01

    Full Text Available The paper describes the preparation of lignin filled natural rubber latex composite and its subsequent use to obtain lignin modified rubber. Two types of lignin i.e.: rubber wood and commercial alkali lignin were used as rubber filler. Gum rubber sheets were prepared from the lignin modified rubber and their properties were compared to Standard Malaysian Rubber (SMR 20 and a type of rubber obtained from the coagulation of high ammonia latex. Rubber morphology was investigated using Scanning Electron Microscope on the cross-sectional area of cryo-fractured samples. Oil resistance of the rubber sheets was determined by measuring the mass change before and after ASTM IRM 903 oil immersion, while the tensile strengths were determined according to ASTM D412 standard. Low values of tensile strength obtained for the commercial alkali lignin modified rubber sheet relative to the rest of the rubber samples was attributed to poor lignin dispersion. This occurrence was substantiated by the SEM analysis of cryo-fractured samples where crazes and inhomogeneity was observed. Nonetheless, both lignin modified rubbers exhibited higher level of oil resistance compared to SMR 20. This is due to the nature of lignin as a hydrophilic component and its presence in the rubber matrix complicates the oil diffusion process into rubber.

  6. Determination of neomycin residues in pasteurized milks produced in some dairy processing establishments in East-Azarbaijan Province, Iran

    Directory of Open Access Journals (Sweden)

    M.H Movassagh

    2014-11-01

    Full Text Available Antibiotic residues in milk have a potential hazard for the consumer and may cause allergic reactions, interference in the intestinal flora that result in development of resistant populations of bacteria, thereby rendering antibiotic treatment ineffective. The aim of this study was to determine neomycin residues in pasteurized milk in East-Azarbaijan province. For this, a total of 200 samples of pasteurized milk produced by five dairy processing establishments of East Azarbaijan province was randomly collected. The samples were obtained over the spring and autumn (100 samples for each season of 2010. First, antibiotic residues were determined by Copan milk test. Afterwards, the competitive ELISA assay was used for the determination of neomycin concentration in positive samples. Of all samples, neomycin residues were observed in 9 and 13 samples and the mean neomycin residues amount were 43.20 ± 8.10 and 26.63±2.08 µg/L in spring and autumn, respectively. According to the limit of neomycin (1500 µg/l in cow raw milk in Iran, despite all the remaining drugs in pasteurized milk, in any of the samples exceeded level of neomycin was not observed.Based on the results, continuousmonitoringofantibiotic residues inmilk samples is recommended.

  7. Validation of a multi-residue method for the determination of residuals pesticides in cabbage (Brassica Oleracea var. Capitata) for gases chromatography

    International Nuclear Information System (INIS)

    Moreno, Milton Leonardo; Guerrero Dallos, Jairo Arturo

    2002-01-01

    This study describes the validation of a multi-residue method for the determination of most used organo chlorine, organophosphorus and organonitrogen pesticides in cabbage in the Cundinamarca Department (Colombia). The extraction process includes blending of small sample quantity with ethyl acetate in presence of Na 2 SO 4 and NaHCO 3 , filtration and concentration. The clean up steps include GPC and mini-column chromatography using silica gel. Final determination was carried out by gas chromatography with: pulsed splitless injection, HP-5 capillary column, and a parallel detection system with micro electron capture detection (μ - ECD) and Nitrogen-Phosphorus Detection (NPD). The methodology is specific, selective, accurate and robust. Recovery values of majority of pesticides were in the range 70-120% at spiking levels ranging 0.05-10.73 mg/kg. Limits of detection were less than 0.10 mg/kg for most of the studied compounds. The distribution of the analyses in the laboratory sample was evaluated and it was found its homogeneity. The evaluation of pesticide residues was made in a specific area of municipality of Madrid-Cundinamarca, (Colombia). No residues of the studied analyses were founded

  8. UPLC-MS/MS determination of florfenicol and florfenicol amine antimicrobial residues in tilapia muscle.

    Science.gov (United States)

    Orlando, Eduardo Adilson; Costa Roque, Aline Gabriela; Losekann, Marcos Eliseu; Colnaghi Simionato, Ana Valéria

    2016-11-01

    Despite the benefits to fish farmers, the use of antimicrobials in aquaculture has concerned consumers and competent authorities. The indiscriminate use of such substances promotes the emergence of resistant microorganisms, decreases the effectiveness of treatments, and causes possible toxic effects in humans. In Brazil, florfenicol is the only antimicrobial registered for use in aquaculture and is often used in tilapia in cage creation. Thus, this study aimed to develop a method for determination of florfenicol residues and its metabolite florfenicol amine in tilapia fillet by UPLC-MS/MS. Analytes were extracted with ethyl acetate, followed by liquid-liquid partition clean-up with hexane and SPE. The sorbents C18, phenyl and HLB-Oasis were evaluated by SPE. Phenyl sorbent showed the best results, and the extraction conditions were optimized in the sample matrix with fractional factorial design 2 4-1 . The analytes were separated on a C18 chromatographic column (50×2.1mm×1.7μm) using water (A) and acetonitrile (B) as mobile phase at a flow rate of 0.3mLmin -1 with a linear gradient (in% B): 0-2.0min: 20%; 2.0-2.5min: increase to 90%; 2.5-3.5min: 90%; 3.0-3.5min: decrease to 20%; 4.0-5.0min: 20%. The analytes were monitored in a MS/MS triple quadrupole system by MRM mode with transitions at m/z 356.1>336.1 (florfenicol) and m/z 248.1>130.1 (florfenicol amine). The optimized method was validated obtaining LOQ values of 3 and 25ngg -1 for florfenicol and florfenicol amine, respectively, precision between 20 and 36%, absolute extraction efficiency between 38 and 80%, and adequate linearity. The method was applied to samples intended for human consumption, and within the 15 evaluated samples, only one showed florfenicol residue at 30ngg -1 , which is below the maximum residue limit established in Brazil. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Preparation and Analysis of Biomass Lignins

    Science.gov (United States)

    Compere, Alicia L.; Griffith, William L.

    Lignin, comprised primarily of three randomly polymerized phenylpropenyl monomers, is, arguably, the second most common organic molecule on earth. In current biorefinery applications, lignin is burned, usually in concentrated pulping or hydrolysis liquor, as a source of process steam and both internal and exported electricity. The aromatic content of lignin makes it a potentially attractive feedstock for high-value aromatic chemicals, polymers, and carbon products (graphite, activated carbon, and carbon fiber). Revenue from production of lignin-based chemicals could play a major role in biorefinery profitability if cost-effective methods for lignin separation and purification can be developed. This chapter presents descriptions of methods for assessing and purifying biorefinery lignins so that they can be evaluated for use as feedstock for production of chemical products. Areas covered are: (1) initial evaluations of as-received lignin samples (visual, microscopic, separable organics); (2) analysis of common contaminants (bulk and filterable ash and particulate contaminants in liquid and dry lignin samples); (3) preparation of lignins for experimental use as chemical feedstock (prefiltration, filtration using bench-scale chemical apparatus and larger scale bag filters, one-step lignin precipitation, two-step carbohydrate and lignin precipitation, desalting of dry powdered or precipitated lignin, and lyophilization). These methods have been used successfully at the bench scale to produce the 1-50 kg amounts of wood and grass lignins typically required for bench-scale assessment as chemical feedstocks.

  10. An efficient direct competitive nano-ELISA for residual BSA determination in vaccines.

    Science.gov (United States)

    Wang, Qian-Long; Li, Jie; Li, Xing-De; Tao, Wan-Jun; Ding, Li-Sheng; Luo, Pei; Qing, Lin-Sen

    2017-07-01

    A simple, fast, and highly sensitive direct competitive enzyme-linked immunosorbent assay (ELISA) based on bovine serum albumin (BSA) antigen labeled amine-terminated silicon dioxide (SiO 2 -NH-BSA) nanoparticles was developed to determine residual BSA in vaccines. As nano-ELISA using nanomaterials with a very high surface-to-volume ratio has emerged as a promising strategy, SiO 2 -NH-BSA nanoparticles were prepared in this study by the coupling of BSA to SiO 2 nanoparticles modified with amidogen, followed by the quantification of BSA via a direct competitive binding of BSA-antigen-labeled SiO 2 nanoparticles to anti-BSA antibody conjugated with horseradish peroxidase. The validation study showed that the linear range of this method was from 1 to 90 ng/mL (r = 0.998) and the limit of detection was 0.67 ng/mL. The intra-assay and interassay coefficients of variation were less than 10% at three concentrations (10, 40, and 70 ng/mL), and the recovery was 92.4%, indicating good specificity. As a proof of principle, this new method was applied in the analysis of residual BSA in five different vaccines. Bland-Altman plots revealed that there was no significant difference in the accuracy and precision between our new method and the most commonly used sandwich ELISA. From the results taken together, the new method developed in this study is more sensitive and facile with lower cost and thus demonstrated potential to be applied in the quality control of biological products. Graphical Abstract Illustration of the procedures of the direct competitive enzyme immunoassay.

  11. An accurate method for determining residual stresses with magnetic non-destructive techniques in welded ferromagnetic steels

    Science.gov (United States)

    Vourna, P.

    2016-03-01

    The scope of the present research work was to investigate the proper selection criteria for developing a suitable methodology for the accurate determination of residual stresses existing in welded parts. Magnetic non-destructive testing took place by the use of two magnetic non-destructive techniques: by the measurement of the magnetic Barkhausen noise and by the evaluation of the magnetic hysteresis loop parameters. The spatial distribution of residual stresses in welded metal parts by both non-destructive magnetic methods and two diffraction methods was determined. The conduction of magnetic measurements required an initial calibration of ferromagnetic steels. Based on the examined volume of the sample, all methods used were divided into two large categories: the first one was related to the determination of surface residual stress, whereas the second one was related to bulk residual stress determination. The first category included the magnetic Barkhausen noise and the X-ray diffraction measurements, while the second one included the magnetic permeability and the neutron diffraction data. The residual stresses determined by the magnetic techniques were in a good agreement with the diffraction ones.

  12. Simultaneous Determination of TetracyclinesResidues in Bovine Milk Samples by Solid Phase Extraction and HPLC-FL Method

    Directory of Open Access Journals (Sweden)

    Mehra Mesgari Abbasi

    2011-06-01

    Full Text Available Introduction:Tetracyclines (TCs are widely used in animal husbandry and their residues in milk may resultinharmful effects on human. The aim of this study was to investigate the presence of TCs residues in various bovine milk samples from local markets of Ardabil, Iran. Methods:One hundred and fourteen pasteurized, sterilized and raw milk samples were collected from markets of Ardabil. Tetracycline, Oxytetracycline and Chlortetracycline (TCs residues extraction carried out by Solid Phase Extraction method. Determination of TCs residues were performed by high performance liquid chromatography (HPLC method using Fluorescence detector.Results: The mean of total TCs residues in all samples (114 samples was 97.6 ±16.9ng/g and that of pasteurized, sterilized and raw milk samples were 87.1 ± 17.7, 112.0 ± 57.3 and 154.0 ± 66.3ng/g respectively. Twenty five point four percent of the all samples, and24.4%, 30% and 28.6% of the pasteurized, sterilized and raw milk samples, respectively had higher TCs residues than the recommended maximum levels (100ng/g. Conclusion:This study indicates the presence of tetracycline residues more than allowed amount. Regulatory authorities should ensure proper withdrawal period before milking the animals and definite supervisions are necessary on application of these drugs.

  13. Standard Test Method for Gravimetric Determination of Nonvolatile Residue from Cleanroom Gloves

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2011-01-01

    1.1 This test method covers the determination of solvent extractable nonvolatile residue (NVR) from gloves used in cleanrooms where spacecraft are assembled, cleaned, or tested. 1.2 The NVR of interest is that which can be extracted from gloves using a specified solvent that has been selected for its extracting qualities, or because it is representative of solvents used in the particular facility. Alternative solvents may be used, but since their use may result in different values being generated, they must be identified in the procedure data sheet. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  14. Thermal desorption-Gas chromatographic methodology for the determination of residual solvents in mesoporous silica.

    Science.gov (United States)

    Asfaw, Adissu Alemayehu; Wolfs, Kris; Schepdael, Ann Van; Adams, Erwin

    2017-06-02

    In this work, thermal desorption-gas chromatography-flame ionization detection (TD-GC-FID) was adapted to enable the determination of residual solvents (RS) in mesoporous silica (MPSi). MPSi is often utilized in various pharmaceutical formulations or drug delivery systems and the accurate determination of RS is an important part of pharmaceutical quality control. Seven commonly used solvents (methanol, ethanol, acetone, isopropanol, dichloromethane, tetrahydrofuran and hexafluoroisopropanol) were evaluated in combination with 3 types of MPSi having pore sizes of 2-3, 15 and 25nm. Validation results showed general recovery values >98% and good linearity over the concentration ranges studied. The limits of detection (LOD) and limits of quantification (LOQ) for the different solvents ranged from 0.03 to 0.08μg and from 0.1 to 0.2μg per tube, respectively. Verification of the accuracy of the TD method was investigated by using an alternative method based on complete dissolution of MPSi in hydrofluoric acid (HF) followed by full evaporation headspace-GC (HS-GC). The results obtained from both procedures were not statistically different (p>0.05) when applied to actual experimental drug samples consisting of itraconazole loaded on MPSi. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. Esterification and characterization of lignin aiming the synthesis of polymeric composite

    International Nuclear Information System (INIS)

    Victor, Priscilla A.; Machado, Fabricio

    2015-01-01

    Lignin is a natural polymer derived from lignocellulosic materials with high availability, presenting a huge potential for production of new materials. Due to its complex macromolecular structure, and its low compatibility with styrene, eucalyptus wood-extracted lignin method was esterified with methacrylic anhydride - exhibiting a yield of 64% - in order to ensure homogeneity in the organic phase into the reaction medium. The evaluation of both the natural and esterified lignin through infrared (IR) spectroscopy showed a decrease of the hydroxyl band, characteristic of natural lignin (3200-3400 cm -1 ) and an increase of the characteristic ester band (1720 to 1740 cm -1 ). According to nuclear magnetic resonance ( 1 H NMR) analysis on esterified lignin, intense peaks were observed in the range from 1.7 to 2.05 ppm (-CH 3 ) and 5.4 ppm to 6.2 ppm (=CH 2 ), related to methacrylic anhydride. According to the thermogravimetric analysis (TGA), the esterified lignin showed a decrease in its thermal stability when compared to natural lignin, exhibiting two main weight losses between 200 °C and 300 °C and in the interval from 550 °C to 800 °C. Comparatively, the esterified lignin also displayed an increase in its glass transition temperature (Tg = 98 °C) for, when compared to natural lignin, whose Tg value was determined to be equal to 91 °C. (author)

  16. Characteristics of Multifunctional, Eco-Friendly Lignin-Al2O3 Hybrid Fillers and Their Influence on the Properties of Composites for Abrasive Tools

    Directory of Open Access Journals (Sweden)

    Łukasz Klapiszewski

    2017-11-01

    Full Text Available The main aim of the present study was the preparation and comprehensive characterization of innovative additives to abrasive materials based on functional, pro-ecological lignin-alumina hybrid fillers. The behavior of lignin, alumina and lignin-Al2O3 hybrids in a resin matrix was explained on the basis of their surface and application properties determined by inverse gas chromatography, the degree of adhesion/cohesion between components, thermomechanical and rheological properties. On the basis of the presented results, a hypothetical mechanism of interactions between lignin and Al2O3 as well as between lignin-Al2O3 hybrids and phenolic resins was proposed. It was concluded that lignin compounds can provide new, promising properties for a phenolic binder combining the good properties of this biopolymer as a plasticizer and of alumina as a filler improving mechanical and thermal properties. The use of such materials may be relatively non-complicated and efficient way to improve the performance of bonded abrasive tools.

  17. Lignin from hydrothermally pretreated grass biomass retards enzymatic cellulose degradation by acting as a physical barrier rather than by inducing nonproductive adsorption of enzymes

    DEFF Research Database (Denmark)

    Djajadi, Demi T.; Jensen, Mads M.; Oliveira, Marlene

    2018-01-01

    Lignin is known to hinder efficient enzymatic conversion of lignocellulose in biorefining processes. In particular, nonproductive adsorption of cellulases onto lignin is considered a key mechanism to explain how lignin retards enzymatic cellulose conversion in extended reactions. Lignin.......97. The LRRs had different residual carbohydrate levels-the highest in MS; the lowest in WS. The residual carbohydrate was not traceable at the surface of the LRRs particles by ATR-FTIR analysis. The chemical properties of the lignin in the LRRs varied across the three types of biomass, but monolignols...... of the enzymes to the LRRs. Since the surface of the LRRs particles were covered by lignin, the data suggest that the retardation of enzymatic cellulose degradation during extended reaction on lignocellulosic substrates is due to physical blockage of the access of enzymes to the cellulose caused by the gradual...

  18. Impact of the homogenization process on the structure and antioxidant properties of chitosan-lignin composite films.

    Science.gov (United States)

    Crouvisier-Urion, Kevin; Lagorce-Tachon, Aurélie; Lauquin, Camille; Winckler, Pascale; Tongdeesoontorn, Wirongrong; Domenek, Sandra; Debeaufort, Frédéric; Karbowiak, Thomas

    2017-12-01

    This work investigated the impact of two homogenization treatments, High Shear (HS) and High Pressure (HP), on the structure and antioxidant activity of chitosan-lignin bio-composite films. Laser light scattering analysis revealed that smaller lignin particles were obtained after HP processing, around 0.6μm, compared to HS treatment, between 2.5 and 5μm. Moreover, these particles were more homogeneously distributed in the chitosan film matrix after HP process, while some aggregates remained after HS treatment, as highlighted by two-photon microscopy. The surface hydrophobicity of the composite films, as measured by water contact angle, increased after the two homogenization treatments. Finally, the antioxidant activity of the composite films was determined using the DPPH· assay. No significant difference in the radical scavenging activity was noticeable, neither after HS nor HP processing. However, a migration of lignin residues from the film to the extraction medium was noticed, particularly for HP process. Copyright © 2017. Published by Elsevier Ltd.

  19. Pyrolysis - gas chromatography - mass spectrometry of lignins

    Energy Technology Data Exchange (ETDEWEB)

    Martin, F.; Saiz-Jimenez, C.; Gonzalez-Vila, F.J.

    1979-01-01

    Milled wood lignins from spruce, beech and bamboo were pyrolysed. The high-boiling products of pyrolysis were studied by GLC and mass spectrometry. The forty-three products identified provide information on the structural units of lignin.

  20. Lignin poly(lactic acid) copolymers

    Energy Technology Data Exchange (ETDEWEB)

    Olsson, Johan Vilhelm; Chung, Yi-Lin; Li, Russell Jingxian; Waymouth, Robert; Sattely, Elizabeth; Billington, Sarah; Frank, Curtis W.

    2017-02-14

    Provided herein are graft co-polymers of lignin and poly(lactic acid) (lignin-g-PLA copolymer), thermoset and thermoplastic polymers including them, methods of preparing these polymers, and articles of manufacture including such polymers.

  1. Validation of an HPLC–UV method for the determination of digoxin residues on the surface of manufacturing equipment

    Directory of Open Access Journals (Sweden)

    ZORAN B. TODOROVIĆ

    2009-09-01

    Full Text Available In the pharmaceutical industry, an important step consists in the removal of possible drug residues from the involved equipments and areas. The cleaning procedures must be validated and methods to determine trace amounts of drugs have, therefore, to be considered with special attention. An HPLC–UV method for the determination of digoxin residues on stainless steel surfaces was developed and validated in order to control a cleaning procedure. Cotton swabs, moistened with methanol were used to remove any residues of drugs from stainless steel surfaces, and give recoveries of 85.9, 85.2 and 78.7 % for three concentration levels. The precision of the results, reported as the relative standard deviation (RSD, were below 6.3 %. The method was validated over a concentration range of 0.05–12.5 µg mL-1. Low quantities of drug residues were determined by HPLC–UV using a Symmetry C18 column (150´4.6 mm, 5 µm at 20 °C with an acetonitrile–water (28:72, v/v mobile phase at a flow rate of 1.1 mL min-1, an injection volume of 100 µL and were detected at 220 nm. A simple, selective and sensitive HPLC–UV assay for the determination of digoxin residues on stainless steel was developed, validated and applied.

  2. QuEChERS-based method for the determination of carbamate residues in aromatic herbs by UHPLC-MS/MS.

    Science.gov (United States)

    Nantia, Edouard Akono; Moreno-González, David; Manfo, Faustin P T; Gámiz-Gracia, Laura; García-Campaña, Ana M

    2017-02-01

    A new reliable, fast and highly sensitive method based on ultra-high performance liquid chromatography tandem mass spectrometry has been developed and validated for the determination of 28 carbamates in aromatic herbs. A modified QuEChERS-based method was optimized for the extraction of carbamate residues from a wide variety of fresh herbal products. The proposed method allowed recoveries higher than 72%, achieving quantification limits of 2μgkg(-1), therefore below maximum residue limits established for this type of samples. The combination of QuEChERS with UHPLC-MS/MS introduces a high-throughput methodology for the monitoring of these residues in this type of matrices scarcely explored. The analysis of the real samples revealed that several samples sold in the European Union and in the North West region of Cameroon contain pesticides in concentrations below the maximum residue limits. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Base-catalyzed depolymerization of lignin : separation of monomers

    Energy Technology Data Exchange (ETDEWEB)

    Vigneault, A. [Sherbrooke Univ., PQ (Canada). Dept. of Chemical Engineering; Johnson, D.K. [National Renewable Energy Laboratory, Golden, CO (United States); Chornet, E. [Sherbrooke Univ., PQ (Canada). Dept. of Chemical Engineering; National Renewable Energy Laboratory, Golden, CO (United States)

    2007-12-15

    Biofuels produced from residual lignocellulosic biomass range from ethanol to biodiesel. The use of lignin for the production of alternate biofuels and green chemicals has been studied with particular emphasis on the structure of lignin and its oxyaromatic nature. In an effort to fractionate lignocellulosic biomass and valorize specific constitutive fractions, the authors developed a strategy for the separation of 12 added value monomers produced during the hydrolytic base catalyzed depolymerization (BCD) of a Steam Exploded Aspen Lignin. The separation strategy was similar to vanillin purification to obtain pure monomers, but combining more steps after the lignin depolymerization such as acidification, batch liquid-liquid-extraction (LLE), followed by vacuum distillation, liquid chromatography (LC) and crystallization. The purpose was to develop basic data for an industrial size process flow diagram, and to evaluate both the monomer losses during the separation and the energy requirements. Experimentally testing of LLE, vacuum distillation and flash LC in the laboratory showed that batch vacuum distillation produced up to 4 fractions. Process simulation revealed that a series of 4 vacuum distillation columns could produce 5 distinct monomer streams, of which 3 require further chromatography and crystallization operations for purification. 22 refs., 4 tabs., 8 figs.

  4. Carbon Fibres from Kraft Lignin

    OpenAIRE

    Norberg, Ida

    2012-01-01

    Kraft lignin has a high potential for use in more valuable applications than its current use as fuel in pulp mills and integrated pulp and paper mills. The possibility of using kraft lignin, a green material with a carbon content of more than 60 %, for the manufacturing of carbon fibres was investigated in this thesis. The strong and lightweight carbon fibre material has many potential application areas, e.g. in cars; the main obstacle limiting its demand is the high production cost, with the...

  5. Lignin recovery. A resource to value

    International Nuclear Information System (INIS)

    Zimbardi, P.; Cardinale, G.; Demichele, M.; Nanna, F.; Viggiano, D.; Bonini, C.; D'Alessio, L.; D'Auria, M.; Teghil, R.; Tofani, D.

    1999-01-01

    In the present paper, the effects of the steam explosion (ES) pretreatment conditions on recovery and chemical structure of wheat straw lignin are reported. The experimental data of lignin recovery by caustic extraction, followed by acid precipitation, have been interpolated to obtain the dependence on the time and temperature of SE. The lignin has been characterised by using several methods. Preliminary results on the synthesis of copolymers lignin-styrene are also reported [it

  6. Lignin degradation during plant litter photodegradation

    Science.gov (United States)

    Lin, Y.; King, J. Y.

    2014-12-01

    Lignin is the second most abundant compound, after cellulose, synthesized by plants. Numerous studies have demonstrated that initial lignin concentration is negatively correlated with litter decomposition rate under both laboratory and field conditions. Thus lignin is commonly considered to be a "recalcitrant" compound during litter decomposition. However, lignin can also serve as a radiation-absorbing compound during photodegradation, the process through which solar radiation breaks down organic matter. Here, we synthesize recent studies concerning lignin degradation during litter photodegradation and report results from our study on how photodegradation changes lignin chemistry at a molecular scale. Recent field studies have found that litter with high initial lignin concentration does not necessarily exhibit high mass loss during photodegradation. A meta-analysis (King et al. 2012) even found a weak negative correlation between initial lignin concentration and photodegradation rate. Contradicting results have been reported with regard to the change in lignin concentration during photodegradation. Some studies have found significant loss of lignin during photodegradation, while others have not. In most studies, loss of lignin only accounts for a small proportion of the overall mass loss. Using NMR spectroscopy, we found significant loss of lignin structural units containing beta-aryl ether linkages during photodegradation of a common grass litter, Bromus diandrus, even though conventional forage fiber analysis did not reveal changes in lignin concentration. Both our NMR and fiber analyses supported the idea that photodegradation induced loss of hemicellulose, which was mainly responsible for the litter mass loss during photodegradation. Our results suggest that photodegradation induces degradation, but not necessarily complete breakdown, of lignin structures and consequently exposes hemicellulose and cellulose to microbial decomposition. We conclude that lignin

  7. A quantitative and qualitative comparison of aquatic and terrestrial plant lignin phenols: Critical information for paleoecological reconstructions

    Science.gov (United States)

    Thomas, E. K.; Gao, L.; Huang, Y.

    2009-12-01

    caution when using lignin phenols in sedimentary archives to reconstruct changes in terrestrial vegetation. We determined the types of lignin phenols in each plant sample and compare the lignin phenol ratios in our samples to the database of lignin phenol ratios for terrestrial plants, with the goal of identifying characteristic differences between terrestrial and aquatic lignin phenols. This is the first report of the lignin phenol composition of freshwater aquatic plants, and is important information for studies that utilize lignin phenols to reconstruct ecological conditions.

  8. Role of enthalpy-entropy compensation interactions in determining the conformational propensities of amino acid residues in unfolded peptides.

    Science.gov (United States)

    Toal, Siobhan E; Verbaro, Daniel J; Schweitzer-Stenner, Reinhard

    2014-02-06

    The driving forces governing the unique and restricted conformational preferences of amino acid residues in the unfolded state are still not well understood. In this study, we experimentally determine the individual thermodynamic components underlying intrinsic conformational propensities of these residues. Thermodynamic analysis of ultraviolet-circular dichroism (UV-CD) and (1)H NMR data for a series of glycine capped amino acid residues (i.e., G-x-G peptides) reveals the existence of a nearly exact enthalpy-entropy compensation for the polyproline II-β strand equilibrium for all investigated residues. The respective ΔHβ, ΔSβ values exhibit a nearly perfect linear relationship with an apparent compensation temperature of 295 ± 2 K. Moreover, we identified iso-equilibrium points for two subsets of residues at 297 and 305 K. Thus, our data suggest that within this temperature regime, which is only slightly below physiological temperatures, the conformational ensembles of amino acid residues in the unfolded state differ solely with respect to their capability to adopt turn-like conformations. Such iso-equilibria are rarely observed, and their existence herein indicates a common physical origin behind conformational preferences, which we are able to assign to side-chain dependent backbone solvation. Conformational effects such as differences between the number of sterically allowed side chain rotamers can contribute to enthalpy and entropy but not to the Gibbs energy associated with conformational preferences. Interestingly, we found that alanine, aspartic acid, and threonine are the only residues which do not share these iso-equilbiria. The enthalpy-entropy compensation discovered as well as the iso-equilbrium and thermodynamics obtained for each amino acid residue provide a new and informative way of identifying the determinants of amino acid propensities in unfolded and disordered states.

  9. Experimental determination of residual stress by neutron diffraction in a boiling water reactor core shroud

    International Nuclear Information System (INIS)

    Payzant, A.; Spooner, S.; Zhu, Xiaojing; Hubbard, C.R.

    1996-01-01

    Residual strains in a 51 mm (2-inch) thick 304L stainless steel plate have been measured by neutron diffraction and interpreted in terms of residual stress. The plate, measuring (300 mm) in area, was removed from a 6m (20-ft.) diameter unirradiated boiling water reactor core shroud, and included a multiple-pass horizontal weld which joined two of the cylindrical shells which comprise the core shroud. Residual stress mapping was undertaken in the heat affected zone, concentrating on the outside half of the plate thickness. Variations in residual stresses with location appeared consistent with trends expected from finite element calculations, considering that a large fraction of the residual hoop stress was released upon removal of the plate from the core shroud cylinder

  10. Iron addition to soil specifically stabilized lignin

    Science.gov (United States)

    Steven J. Hall; Whendee L. Silver; Vitaliy I. Timokhin; Kenneth E. Hammel

    2016-01-01

    The importance of lignin as a recalcitrant constituent of soil organic matter (SOM) remains contested. Associations with iron (Fe) oxides have been proposed to specifically protect lignin from decomposition, but impacts of Fe-lignin interactions on mineralization rates remain unclear. Oxygen (O2) fluctuations characteristic of humid tropical...

  11. Converting lignin to aromatics: step by step

    NARCIS (Netherlands)

    Strassberger, Z.I.

    2014-01-01

    Lignin, the glue that holds trees together, is the most abundant natural resource of aromatics. In that respect, it is a far more advanced resource than crude oil. This is because lignin already contains the aromatic functional groups. Thus, catalytic conversion of lignin to high-value aromatics is

  12. Lignin pyrolysis for profitable lignocellulosic biorefineries

    NARCIS (Netherlands)

    Wild, de P.J.; Gosselink, R.J.A.; Huijgen, W.J.J.

    2014-01-01

    Bio-based industries (pulp and paper and biorefineries) produce > 50 Mt/yr of lignin that results from fractionation of lignocellulosic biomass. Lignin is world's second biopolymer and a major potential source for production of performance materials and aromatic chemicals. Lignin valorization is

  13. Liquid Fuels from Lignins: Annual Report

    Energy Technology Data Exchange (ETDEWEB)

    Chum, H. L.; Johnson, D. K.

    1986-01-01

    This task was initiated to assess the conversion of lignins into liquid fuels, primarily of lignins relevant to biomass-to-ethanol conversion processes. The task was composed of a literature review of this area and an experimental part to obtain pertinent data on the conversion of lignins germane to biomass-to-ethanol conversion processes.

  14. Cationic electrodepositable coating composition comprising lignin

    Science.gov (United States)

    Fenn, David; Bowman, Mark P; Zawacky, Steven R; Van Buskirk, Ellor J; Kamarchik, Peter

    2013-07-30

    A cationic electrodepositable coating composition is disclosed. The present invention in directed to a cationic electrodepositable coating composition comprising a lignin-containing cationic salt resin, that comprises (A) the reaction product of: lignin, an amine, and a carbonyl compound; (B) the reaction product of lignin, epichlorohydrin, and an amine; or (C) combinations thereof.

  15. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review.

    Science.gov (United States)

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Multi-residue method for the determination of antibiotics and some of their metabolites in seafood.

    Science.gov (United States)

    Serra-Compte, Albert; Álvarez-Muñoz, Diana; Rodríguez-Mozaz, Sara; Barceló, Damià

    2017-06-01

    The presence of antibiotics in seafood for human consumption may pose a risk for consumers. A methodology for the analysis of antibiotics in seafood based on QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction, followed by detection and quantification using liquid chromatography coupled to mass spectrometry was developed. The analytical method was evaluated for the determination of 23 antibiotics (including parent compounds and some metabolites) in fish, mussels and clams. Recoveries ranged between 30% and 70% for most of the compounds and method detection and quantification limits (MDLs and MQLs) were between 0.01 and 0.31 ng/g dry weigh (dw) and 0.02-1.03 ng/g (dw) respectively. Real seafood samples were analysed using this method. Nine antibiotics were found at levels above MDLs; however none of them exceed the maximum residue limits (MRL) established by the authorities. Tetracycline was the most ubiquitous compound, presenting also the highest concentration: 5.63 ng/g (dw) in fish from Netherlands. In addition, an alternative technique based on microbial growth inhibition was explored as semiquantitative detection method of antibiotics in seafood. This methodology could be applied as a fast screening technique for the detection of macrolides and β-lactams in seafood but further research is needed for other antibiotics families. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Simultaneous determination of 38 veterinary antibiotic residues in raw milk by UPLC-MS/MS.

    Science.gov (United States)

    Han, R W; Zheng, N; Yu, Z N; Wang, J; Xu, X M; Qu, X Y; Li, S L; Zhang, Y D; Wang, J Q

    2015-08-15

    A selective and rapid method has been developed to determine, simultaneously, 38 veterinary antibiotic residues in raw milk by ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). One milliliter of raw milk was diluted with 0.5 mL water and 3 mL acetonitrile, then purified using an Oasis HLB cartridge. The eluates were evaporated by nitrogen drying and then reconstituted to 4 mL with water/acetonitrile (8:1) before being injected into the UPLC-MS/MS system. The results indicated recoveries of 68-118% for 14 β-lactams, 79-118% for eight quinolones, 71-106% for eight sulfonamides, 76-116% for four tetracyclines, 78-106% for three macrolides, and 88-103% for one lincosamides, with coefficients of variation less than 15% for intraday and interday precisions. The limit of quantification for all antibiotics was 0.03-10 μg kg(-1). This methodology was then applied to field-collected real raw milk samples and trace levels of four antibiotics were detected. Copyright © 2015 Elsevier Ltd. All rights reserved.

  18. Direct determination of the redox status of cysteine residues in proteins in vivo

    Energy Technology Data Exchange (ETDEWEB)

    Hara, Satoshi [Chemical Resources Laboratory, Tokyo Institute of Technology, Nagatsuta 4259-R1-8, Midori-ku, Yokohama 226-8503 (Japan); Tatenaka, Yuki; Ohuchi, Yuya [Dojindo Laboratories, 2025-5 Tabaru, Mashiki-machi, Kumamoto 861-2202 (Japan); Hisabori, Toru, E-mail: thisabor@res.titech.ac.jp [Chemical Resources Laboratory, Tokyo Institute of Technology, Nagatsuta 4259-R1-8, Midori-ku, Yokohama 226-8503 (Japan); Core Research for Evolutional Science and Technology (CREST), Japan Science and Technology Agency (JST), Tokyo 102-0075 (Japan)

    2015-01-02

    Highlights: • A new DNA-maleimide which is cleaved by UV irradiation, DNA-PCMal, was developed. • DNA-PCMal can be used like DNA-Mal to analyze the redox state of cysteine residues. • It is useful for detecting the thiol redox status of a protein in vivo by Western blotting method. • Thus, DNA-PCMal can be a powerful tool for redox proteomics analysis. - Abstract: The redox states of proteins in cells are key factors in many cellular processes. To determine the redox status of cysteinyl thiol groups in proteins in vivo, we developed a new maleimide reagent, a photocleavable maleimide-conjugated single stranded DNA (DNA-PCMal). The DNA moiety of DNA-PCMal is easily removed by UV-irradiation, allowing DNA-PCMal to be used in Western blotting applications. Thereby the state of thiol groups in intracellular proteins can be directly evaluated. This new maleimide compound can provide information concerning redox proteins in vivo, which is important for our understanding of redox networks in the cell.

  19. [Multi-residue method for determination of veterinary drugs and feed additives in meats by HPLC].

    Science.gov (United States)

    Chonan, Takao; Fujimoto, Toru; Ueno, Ken-Ichi; Tazawa, Teijiro; Ogawa, Hiroshi

    2007-10-01

    A simple and rapid multi-residue method was developed for the determination of 28 kinds of veterinary drugs and feed additives (drugs) in muscle of cattle, pig and chicken. The drugs were extracted with acetonitrile-water (95:5) in a homogenizer and ultrasonic generator. The extracted solution was poured into an alumina column and the drugs were eluted with acetonitrile-water (90:10). The eluate was washed with n-hexane saturated with acetonitrile and then evaporated. The drugs were separated on a Inertsil ODS-3V column (4.6 mm i.d. x 250 mm) with a gradient system of 0.1% phosphoric acid-acetonitrile as the mobile phase, with monitoring at 280 and 340 nm. The recoveries of the 26 kinds of drugs were over 60% from the meats fortified at 0.1 microg/g, and the quantification limits of most drugs were 0.01 microg/g. This proposed method was found to be effective and suitable for the screening of the above drugs in meats.

  20. Study of TATP: method for determination of residual acids in TATP.

    Science.gov (United States)

    Matyáš, Robert; Chýlková, Jaromíra

    2013-05-10

    Triacetone triperoxide (3,3,6,6,9,9-hexamethyl-1,2,4,5,7,8-hexoxonane, TATP) is nowadays one of the most commonly used improvised explosives. It is prepared by the action of hydrogen peroxide on acetone in an acidic environment. Easily available mineral acids - hydrochloric, sulfuric, nitric and perchloric - are the most often recommended on the extremist web pages dealing with improvised production of explosives. The various TATP producers' choice of acid mainly depends on the author's experiences and the local availability of the acid. A knowledge of the kind of acid used for TATP production can help in detecting the person who has made the TATP, or who has committed a criminal act using TATP. Therefore, a capillary isotachophoretic method was developed for determination of residual anions (originating from the acid used during TATP synthesis) in the resulting TATP crystals. This analytical method has proved to be reliable; the acid used for TATP synthesis was correctly identified in all samples analyzed. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

  1. Determination of oxytetracycline residues in matrixes from a freshwater recirculating aquaculture system.

    Science.gov (United States)

    Carson, Mary C; Bullock, Graham; Bebak-Williams, Julie

    2002-01-01

    This paper describes related procedures to determine the amount of oxytetracycline (OTC) present in trout tissue (muscle with skin attached), biofilter sand, sediment, and tank water from a recirculating aquaculture system. OTC was extracted from the matrixes by different techniques, depending on complexity of the matrix and desired OTC detection level in that matrix. Listed in order of increasing complexity, OTC was extracted from tank water by dilution with acidic buffer containing ethylenediaminetetraacetic acid (EDTA); from biofilter sand by shaking with 0.1 N HCl; from sediment by homogenization and shaking with buffer/EDTA; and from ground trout by homogenization and shaking with buffer/EDTA (twice), with further cleanup and concentration of the extract on a polymeric solid-phase extraction cartridge. The 4 procedures all used the same reversed-phase gradient chromatography on a polymeric column with UV detection at 350 nm. The lower limit of detection (estimated) and upper limit of validation for each of these 4 matrixes were 0.04-4.0 microg/g (ppm; trout), 0.03-20 ppm (biofilter sand), 1-6000 ppm (sediment), and 0.003-10 ppm (water). Recoveries ranged from 82 to 108%, with relative standard deviation <20% over the applicable concentration ranges. These procedures were used to monitor OTC residues resulting from medicated feed administered to rainbow trout in a recirculating aquaculture system.

  2. Characteristics of Lignin Fractions from Dilute Acid Pretreated Switchgrass and Their Effect on Cellobiohydrolase from Trichoderma longibrachiatum

    Directory of Open Access Journals (Sweden)

    Lan Yao

    2018-02-01

    Full Text Available To investigate the interactions between acid pretreated switchgrass lignin and cellobiohydrolase (CBH, three different lignin fractions were isolated from dilute acid pretreated switchgrass by (i ethanol extraction, followed by (ii dioxane/H2O extraction, and (iii cellulase treatment, respectively. Structural properties of each lignin fraction were elucidated by GPC, 13C-NMR, and 2D-HSQC NMR analyses. The adsorptions of CBH to the isolated lignin fractions were also studied by Langmuir adsorption isotherms. Ethanol-extractable lignin fraction, mainly composed of syringyl (S and guaiacyl (G units, had the lowest molecular weight, while dioxane/H2O-extracted lignin fraction had the lowest S/G ratio with higher content of p-coumaric acid (pCA unit. The residual lignin fraction after enzymatic treatment had the highest S/G ratio without hydroxyphenyl (H unit. Strong associations were found between lignin properties such as lignin composition and S/G ratio and its non-productive enzyme adsorption factors including the maximum adsorption capacity and binding strength.

  3. Catalytic Depolymerization and Upgrading of Lignin for Vanillin Production: Cooperative Research and Development Final Report, CRADA Number CRD-14-545

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg [National Renewable Energy Lab. (NREL), Golden, CO (United States)

    2017-03-31

    Examine catalytic conversion of lignin using multifunctional catalysts that are able to depolymerize and oxidize lignin to a vanillin-rich stream. Examine separation processes for isolation of vanillin from product mixtures. Conduct preliminary experiments to determine if deconstructed lignin streams can be metabolized by Pseudomonas putida.

  4. Copper Determination in Gunshot Residue by Cyclic Voltammetric and Inductive Coupled Plasma-Optical Emission Spectroscopy

    Directory of Open Access Journals (Sweden)

    Mohd Hashim Nurul’Afiqah Hashimah

    2016-01-01

    Full Text Available Analysis of gunshot residue (GSR is a crucial evidences for a forensic analyst in the fastest way. GSR analysis insists a suitable method provides a relatively simple, rapid and precise information on the spot at the crime scene. Therefore, the analysis of Cu(II in GSR using cyclic voltammetry (CV on screen printed carbon electrode (SPCE is a better choice compared to previous alternative methods such as Inductive Coupled Plasma-Optical Emission Spectroscopy (ICP-OES those required a long time for analysis. SPCE is specially designed to handle with microvolumes of sample such as GSR sample. It gives advantages for identification of copper in GSR on-site preliminary test to prevent the sample loss on the process to be analyzed in the laboratory. SPCE was swabbed directly on the shooter’s arm immediately after firing and acetate buffer was dropped on SPCE before CV analysis. For ICP-OES analysis, cotton that had been soaked in 0.5 M nitric acid was swabbed on the shooter’s arm immediately after firing and kept in a tightly closed sampling tube. Gold coated SPCE that had been through nanoparticles modification exhibits excellent performance on voltammograms. The calibration was linear from 1 to 50 ppm of copper, the limit of detection for copper was 0.3 ppm and a relative standard deviation was 6.1 %. The method was successfully applied to the determination of copper in GSR. The Cu determination on SPCE was compared and validated by ICP-OES method with 94 % accuracy.

  5. [Research on the Spectrophotometry for Determination of Flavonoids in Waste Residue of Stevia Rebaudiana].

    Science.gov (United States)

    Luo, Xu-yan; Fang, Hao-bin; Huang, Rui-yu; Zhao, Dong-fang; Zhu, Ting; Guo, Yang-yang; Zeng Yi-ping; Liu, Ren-yue; Zhu, Dong

    2015-10-01

    A spectrophotometric method for the determination of flavonoids content in Waste Residue of Stevia Rebaudiana was established by comparing the UV-Vis spectra with three spectrophotometric methods: Direct, AlCl3 and NaNO2-Al (NO3)3-NaOH method. The effects of spectrophotometric reaction were studied by analyzing the wavelength, the dosage of color development reagent, reaction time, temperature and pH. The further research was studied by analyzing linearity between the absorbance and the concentration, the stability of this color system, the recovery rate and so on. The results showed that NaNO2-Al(NO3)3-NaOH method was best. The wavelength was 500 nm. The standard sample was rutin. There was a good linear relationship in the ranges of 2 - 24 μg x mL(-1), correlation coefficient R2 = 0.999 5. The recovery of the additional sample was 96.0%-104.3%. The relative standard deviation(RSD) is respectively 3.75%. The dosages of NaNO2 and Al(NO3)3 both were 1.0 mL, both of their reaction time was 6 min. The dosage of NaOH was 15.0 mL and the reaction time was 15 min. The temperature in the whole process of the reaction must be maintained at 40 degrees C and pH is 5. The spectrophotometric condition was further improved on the determination of flavonoids content. This method, which is simple, rapid and accuracy, can be used in practical application.

  6. Substrate specificity determinants of the methanogen homoaconitase enzyme: structure and function of small subunit residues

    Energy Technology Data Exchange (ETDEWEB)

    Jeyakanthan, Jeyaraman [National Synchrotron Radiation Research Center; Drevland, Randy [University of Texas, Austin; Gayathri, Dasara [University of Madras; Velmurugan, Devadasan [University of Madras; Shinkai, Akeo [SPring8/JASRI, Mikazuki, Hyogo and RIKEN, Japan; Kuramitsu, Seiki [SPring8/JASRI, Mikazuki, Hyogo and RIKEN, Japan; Yokoyama, Shigeyuki [University of Tokyo, Tokyo, Japan; Graham, David E [ORNL

    2010-01-01

    The aconitase family of hydro-lyase enzymes includes three classes of proteins that catalyze the isomerization of -hydroxyacids to -hydroxyacids. Besides aconitase, isopropylmalate isomerase (IPMI) proteins specifically catalyze the isomerization of , -dicarboxylates with hydrophobic -chain groups, and homoaconitase (HACN) proteins catalyze the isomerization of tricarboxylates with variable chain length -carboxylate groups. These enzymes stereospecific hydro-lyase activities make them attractive catalysts to produce diastereomers from unsaturated precursors. However, sequence similarity and convergent evolution among these proteins leads to widespread misannotation and uncertainty about gene function. To find the substrate specificity determinants of homologous IPMI and HACN proteins from Methanocaldococcus jannaschii, the small-subunit HACN protein (MJ1271) was crystallized for X-ray diffraction. The structural model showed characteristic residues in a flexible loop region between 2 and 3 that distinguish HACN from IPMI and aconitase proteins. Site-directed mutagenesis of MJ1271 produced loop-region variant proteins that were reconstituted with wild-type MJ1003 large-subunit protein. The heteromers formed promiscuous hydro-lyases with reduced activity but broader substrate specificity. Both R26K and R26V variants formed relatively efficient IPMI enzymes, while the T27A variant had uniformly lower specificity constants for both IPMI and HACN substrates. The R26V T27Y variant resembles the MJ1277 IPMI small subunit in its flexible loop sequence, but demonstrated the broad substrate specificity of the R26V variant. These mutations may reverse the evolution of HACN activity from an ancestral IPMI gene, demonstrating the evolutionary potential for promiscuity in hydro-lyase enzymes. Understanding these specificity determinants enables the functional reannotation of paralogous HACN and IPMI genes in numerous genome sequences. These structural and kinetic results will

  7. Standard test method for determining the effective elastic parameter for X-ray diffraction measurements of residual stress

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    1998-01-01

    1.1 This test method covers a procedure for experimentally determining the effective elastic parameter, Eeff, for the evaluation of residual and applied stresses by X-ray diffraction techniques. The effective elastic parameter relates macroscopic stress to the strain measured in a particular crystallographic direction in polycrystalline samples. Eeff should not be confused with E, the modulus of elasticity. Rather, it is nominally equivalent to E/(1 + ν) for the particular crystallographic direction, where ν is Poisson's ratio. The effective elastic parameter is influenced by elastic anisotropy and preferred orientation of the sample material. 1.2 This test method is applicable to all X-ray diffraction instruments intended for measurements of macroscopic residual stress that use measurements of the positions of the diffraction peaks in the high back-reflection region to determine changes in lattice spacing. 1.3 This test method is applicable to all X-ray diffraction techniques for residual stress measurem...

  8. Structural variations and physical properties of lignin coke

    International Nuclear Information System (INIS)

    Otani, C.

    1986-01-01

    The studied lignin is a by-product of the process of ethanol production from eucaliptus. It was heat-treated under inert atmosphere conditions at increasing temperatures from 300 0 C up to 2600 0 C. This material has about 35 weight % of carbon yield and low ash content (0.70 w %). The structural variations were studied by wide-angle X-ray diffraction, small-angle X-ray scattering and infra-red spectroscopy. The bulk and the ''real'' density of the samples have also been determined as a function of the heat treatment temperatures. These experimental results enabled us to establish a mechanism of structure variation based on the formation of a graphite-like and porous structure within the initially amorphous lignin matrix. It has been possible to specify the adequate heat treatment temperature based upon the lignin coke applications. (author) [pt

  9. Survey of pesticide residues in table grapes: Determination of processing factors, intake and risk assessment

    DEFF Research Database (Denmark)

    Poulsen, Mette Erecius; Hansen, H.K.; Sloth, Jens Jørgen

    2007-01-01

    The differences in residue pattern between Italy and South Africa, the main exporters of table grapes to the Danish market, were investigated. The results showed no major differences with respect to the number of samples with residues, with residues being found in 54-78% of the samples. Exceedances......, no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes was 3.9 mu g day......(-1) for pesticides and 21 mu g day(-1) for copper. Correspondingly, the intakes from South African grapes were 2.6 and 5.7 mu g day(-1) respectively. When the total exposure of pesticides from grapes were related to acceptable daily intake, expressed as the sum of Hazard Quotients, the exposure were...

  10. Measurement of capillary permeability in canine heart determined by the tissue injection, residue detection method

    DEFF Research Database (Denmark)

    Svendsen, Jesper Hastrup; Paaske, W P; Haunsø, S

    1991-01-01

    In previous studies the tissue injection, residue detection method failed to provide results of diffusional capillary permeability comparable to those of other methods. For this reason we reconsidered the kinetic theory and found that it is necessary to take into account the apparent (restricted...... (apparent) interstitial volume of distribution, tev is the mean transit time of the indicator, and klo is the recorded fractional initial washout rate constant. In experiments on open chest dog hearts we examined capillary permeability for 51Cr-EDTA and 99mTc-DTPA with the tissue injection, residue...... detection method and the single injection, residue detection method. Blood flow was measured independently with local 133Xenon washout. D and D' were measured by a true transient diffusion method. We found that the tissue injection, residue detection method gave results for capillary extraction and Pd...

  11. Measurement of capillary permeability in canine heart determined by the tissue injection, residue detection method

    DEFF Research Database (Denmark)

    Svendsen, J H; Paaske, William P; Haunsø, S

    1991-01-01

    detection method and the single injection, residue detection method. Blood flow was measured independently with local 133Xenon washout. D and D' were measured by a true transient diffusion method. We found that the tissue injection, residue detection method gave results for capillary extraction and Pd......In previous studies the tissue injection, residue detection method failed to provide results of diffusional capillary permeability comparable to those of other methods. For this reason we reconsidered the kinetic theory and found that it is necessary to take into account the apparent (restricted...... (apparent) interstitial volume of distribution, tev is the mean transit time of the indicator, and klo is the recorded fractional initial washout rate constant. In experiments on open chest dog hearts we examined capillary permeability for 51Cr-EDTA and 99mTc-DTPA with the tissue injection, residue...

  12. Determination of Bulk Residual Stresses in Electron Beam Additive-Manufactured Aluminum

    Science.gov (United States)

    Brice, Craig A.; Hofmeister, William H.

    2013-11-01

    Additive-manufactured aluminum alloy deposits were analyzed using neutron diffraction to characterize the effect of intermediate stress relief anneal heat treatment on bulk residual stresses in the final part. Based on measured interplanar spacing, stresses were calculated at various locations along a single bead, stacked wall deposit. A comparison between an uninterrupted deposited wall and an interrupted, stress-relieved, and annealed deposited wall showed a measureable reduction in residual stress magnitude at the interface with a corresponding shift in stress character into the deposit. This shift changes the interface stresses from purely compressive to partially tensile. The residual stress profile varied along the length of the deposit, and the heat-treatment procedure reduced the overall magnitude of the stress at the interface by 10 through 25 MPa. These results are interpreted in terms of thermal gradients inherent to the process and compared with prior residual stress-characterization studies in additive-manufactured metallic structures.

  13. Determine metrics and set targets for soil quality on agriculture residue and energy crop pathways

    Energy Technology Data Exchange (ETDEWEB)

    Ian Bonner; David Muth

    2013-09-01

    There are three objectives for this project: 1) support OBP in meeting MYPP stated performance goals for the Sustainability Platform, 2) develop integrated feedstock production system designs that increase total productivity of the land, decrease delivered feedstock cost to the conversion facilities, and increase environmental performance of the production system, and 3) deliver to the bioenergy community robust datasets and flexible analysis tools for establishing sustainable and viable use of agricultural residues and dedicated energy crops. The key project outcome to date has been the development and deployment of a sustainable agricultural residue removal decision support framework. The modeling framework has been used to produce a revised national assessment of sustainable residue removal potential. The national assessment datasets are being used to update national resource assessment supply curves using POLYSIS. The residue removal modeling framework has also been enhanced to support high fidelity sub-field scale sustainable removal analyses. The framework has been deployed through a web application and a mobile application. The mobile application is being used extensively in the field with industry, research, and USDA NRCS partners to support and validate sustainable residue removal decisions. The results detailed in this report have set targets for increasing soil sustainability by focusing on primary soil quality indicators (total organic carbon and erosion) in two agricultural residue management pathways and a dedicated energy crop pathway. The two residue pathway targets were set to, 1) increase residue removal by 50% while maintaining soil quality, and 2) increase soil quality by 5% as measured by Soil Management Assessment Framework indicators. The energy crop pathway was set to increase soil quality by 10% using these same indicators. To demonstrate the feasibility and impact of each of these targets, seven case studies spanning the US are presented

  14. Lignin depletion enhances the digestibility of cellulose in cultured xylem cells.

    Directory of Open Access Journals (Sweden)

    Catherine I Lacayo

    Full Text Available Plant lignocellulose constitutes an abundant and sustainable source of polysaccharides that can be converted into biofuels. However, the enzymatic digestion of native plant cell walls is inefficient, presenting a considerable barrier to cost-effective biofuel production. In addition to the insolubility of cellulose and hemicellulose, the tight association of lignin with these polysaccharides intensifies the problem of cell wall recalcitrance. To determine the extent to which lignin influences the enzymatic digestion of cellulose, specifically in secondary walls that contain the majority of cellulose and lignin in plants, we used a model system consisting of cultured xylem cells from Zinniaelegans. Rather than using purified cell wall substrates or plant tissue, we have applied this system to study cell wall degradation because it predominantly consists of homogeneous populations of single cells exhibiting large deposits of lignocellulose. We depleted lignin in these cells by treating with an oxidative chemical or by inhibiting lignin biosynthesis, and then examined the resulting cellulose digestibility and accessibility using a fluorescent cellulose-binding probe. Following cellulase digestion, we measured a significant decrease in relative cellulose content in lignin-depleted cells, whereas cells with intact lignin remained essentially unaltered. We also observed a significant increase in probe binding after lignin depletion, indicating that decreased lignin levels improve cellulose accessibility. These results indicate that lignin depletion considerably enhances the digestibility of cellulose in the cell wall by increasing the susceptibility of cellulose to enzymatic attack. Although other wall components are likely to contribute, our quantitative study exploits cultured Zinnia xylem cells to demonstrate the dominant influence of lignin on the enzymatic digestion of the cell wall. This system is simple enough for quantitative image analysis

  15. Multi-residue methods for confirmatory determination of antibiotics in milk.

    Science.gov (United States)

    Samanidou, Victoria; Nisyriou, Styliani

    2008-06-01

    The prevalent use of antibiotics, e. g. sulphonamides, tetracyclines, beta-lactams, macrolides, aminoglycosides, etc., in dairy farming to prevent and treat microbial infections e. g. mastitis, can be a potential source of veterinary drug residues in milk. Antibiotic residues constitute a risk to human health, since they can cause allergic reactions in hypersensitive individuals or they may lead to the appearance of drug-resistant bacteria. Analysis of these residues plays a key role in ensuring food safety. Regulatory agencies in the European Union and in other countries have established maximum residue limits and requirements concerning the performance of analytical methods and the interpretation of the results. This review describes the state of the art in the analytical strategies concerning the multi-class as well as the multi-residue analysis of antibiotics in milk. Since milk is a complex matrix due to its high protein and fat content, which often interfere in analytical procedures, special focus has been placed on sample preparation: extraction and clean-up. Confirmation of antibiotic residues according to European Decision 657/2002/EC has been also discussed.

  16. Computational design, construction, and characterization of a set of specificity determining residues in protein-protein interactions.

    Science.gov (United States)

    Nagao, Chioko; Izako, Nozomi; Soga, Shinji; Khan, Samia Haseeb; Kawabata, Shigeki; Shirai, Hiroki; Mizuguchi, Kenji

    2012-10-01

    Proteins interact with different partners to perform different functions and it is important to elucidate the determinants of partner specificity in protein complex formation. Although methods for detecting specificity determining positions have been developed previously, direct experimental evidence for these amino acid residues is scarce, and the lack of information has prevented further computational studies. In this article, we constructed a dataset that is likely to exhibit specificity in protein complex formation, based on available crystal structures and several intuitive ideas about interaction profiles and functional subclasses. We then defined a "structure-based specificity determining position (sbSDP)" as a set of equivalent residues in a protein family showing a large variation in their interaction energy with different partners. We investigated sequence and structural features of sbSDPs and demonstrated that their amino acid propensities significantly differed from those of other interacting residues and that the importance of many of these residues for determining specificity had been verified experimentally. Copyright © 2012 Wiley Periodicals, Inc.

  17. Transient and residual stresses in a pressable glass-ceramic before and after resin-cement coating determined using profilometry.

    LENUS (Irish Health Repository)

    2011-05-01

    The effect of heat-pressing and subsequent pre-cementation (acid-etching) and resin-cementation operative techniques on the development of transient and residual stresses in different thicknesses of a lithium disilicate glass-ceramic were characterised using profilometry prior to biaxial flexure strength (BFS) determination.

  18. Pretreatment and enzymatic hydrolysis of wheat straw (Triticum aestivum L.) – The impact of lignin relocation and plant tissues on enzymatic accessibility

    DEFF Research Database (Denmark)

    Hansen, Mads Anders Tengstedt; Kristensen, Jan Bach; Felby, Claus

    2011-01-01

    , after 144 h of enzymatic hydrolysis the cortex had vanished, exposing the heavier lignified vascular tissue. Accumulation of lignin droplets and exposure of residual lignin could be part of the explanation for the decreasing hydrolysis rate. Flattening of macrofibrils after pretreatment together...

  19. Drugs’ maximal residual limits determination methodology and waiting period’s establishing, in the light of E.U. regulations

    Directory of Open Access Journals (Sweden)

    Cristina , T. Romeo

    2008-12-01

    Full Text Available Communitary concept’s related to the drug residues assumption is essential to Romania’s full integration amongst the countries where alimentary security and human consumer’s security have had become national policy. In this respect a concise enumeration of E.U. basic legislative notions, with the specific terminology and of technicalpremises presentation, it is proposed in the aim of Communitary veterinary medicinal product’s residues evaluation as well the MRL’s determination phases in the light of 2377/90 EU Regulation’s understanding.

  20. Residual life assessment of overhead transmission lines 110 kV and above and determination of their reconstruction terms

    Directory of Open Access Journals (Sweden)

    Uteuliyev Bauyrzhan

    2017-01-01

    Full Text Available In this article is given a method for assessment the residual life of overhead transmission lines on reinforced concrete supports with centrifuged poles. Reinforced concrete poles of supports, wires and lightning protection cables are adopted as the main elements. The intensity of change in the actual state parameters of these elements is determined by the laws of random variables distribution that allow predicting the residual life and the timing of repairs and reconstruction of overhead transmission lines. The parameters of natural climatic conditions and other external factors are considered by including of coefficients into the formula for changing the actual state parameters.

  1. Lignin solubilization and aqueous phase reforming for the production of aromatic chemicals and hydrogen.

    Science.gov (United States)

    Zakzeski, Joseph; Weckhuysen, Bert M

    2011-03-21

    The solubilization and aqueous phase reforming of lignin, including kraft, soda, and alcell lignin along with sugarcane bagasse, at low temperatures (T≤498 K) and pressures (P≤29 bar) is reported for the first time for the production of aromatic chemicals and hydrogen. Analysis of lignin model compounds and the distribution of products obtained during the lignin aqueous phase reforming revealed that lignin was depolymerized through disruption of the abundant β-O-4 linkages and, to a lesser extent, the 5-5' carbon-carbon linkages to form monomeric aromatic compounds. The alkyl chains contained on these monomeric compounds were readily reformed to produce hydrogen and simple aromatic platform chemicals, particularly guaiacol and syringol, with the distribution of each depending on the lignin source. The methoxy groups present on the aromatic rings were subject to hydrolysis to form methanol, which was also readily reformed to produce hydrogen and carbon dioxide. The composition of the isolated yields of monomeric aromatic compounds and overall lignin conversion based on these isolated yields varied from 10-15% depending on the lignin sample, with the balance consisting of gaseous products and residual solid material. Furthermore, we introduce the use of a high-pressure autoclave with optical windows and an autoclave with ATR-IR sentinel for on-line in situ spectroscopic monitoring of biomass conversion processes, which provides direct insight into, for example, the solubilization process and aqueous phase reforming reaction of lignin. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Development of lignin in Themeda triandra, Cymbopogon plurinodis ...

    African Journals Online (AJOL)

    The amount and distribution of lignin in three grass species was determined. Two climax species, Themeda triandra and Cymbopogon plurinodis and one pioneer species, Eragrostis lehmanniana were used in the investigation. Leaf samples of the three grass species were taken at four stages of growth and samples of the ...

  3. The determination, by x-ray-fluorescence spectrometry, of noble and base metals in matte-leach residues

    International Nuclear Information System (INIS)

    Austen, C.E.

    1977-01-01

    An accurate and precise method is described for the determination of noble and base metals in matte-leach residues. Preparation of the samples essentially involves fusion with sodium peroxide in a zirconium crucible and leaching with hydrochloric and nitric acids. Matrix correction and calibration are achieved by use of the single-standard calibration method with reference solutions prepared from pure metals or from compounds of the element to be determined

  4. The natural catalytic function of CuGE glucuronoyl esterase in hydrolysis of genuine lignin-carbohydrate complexes from birch

    DEFF Research Database (Denmark)

    Mosbech, Caroline; Holck, Jesper; Meyer, Anne S.

    2018-01-01

    Glucuronoyl esterases belong to carbohydrate esterase family 15 and catalyze de-esterification. Their natural function is presumed to be cleavage of ester linkages in lignin-carbohydrate complexes particularly those linking lignin and glucuronoyl residues in xylans in hardwood. Here, we show...... for the first time a detailed product profile of aldouronic acids released from birchwood lignin by a glucuronoyl esterase from the white-rot fungus Cerrena unicolor (CuGE). CuGE releases substrate for GH10 endo-xylanase which results in significantly increased product release compared to the action of endo...... with lignin and we propose that this is a direct result of enzymatic cleavage of the ester bonds connecting glucuronoxylan to lignin via 4-O-methyl glucuronoyl-ester linkages. This function appears important for the fungal organism's ability to effectively utilize all available carbohydrates...

  5. Covalent bond formation between amino acids and lignin: cross-coupling between proteins and lignin.

    Science.gov (United States)

    Cong, Fang; Diehl, Brett G; Hill, Joseph Lee; Brown, Nicole R; Tien, Ming

    2013-12-01

    The present study characterized the products formed from the reaction of amino acids and in turn, proteins, with lignin resulting in cross-coupling. When added to reaction mixtures containing coniferyl alcohol, horseradish peroxidase and H2O2, three amino acids (Cys, Tyr, and Thr) are able to form adducts. The low molecular weight products were analyzed by HPLC and from each reaction mixture, one product was isolated and analyzed by LC/MS. LC/MS results are consistent with bond formation between the polar side-chain of these amino acids with Cα. These results are consistent with the cross-coupling of Cys, Tyr and Thr through a quinone methide intermediate. In addition to the free amino acids, it was found that the cross-coupling of proteins with protolignin through Cys or Tyr residues. The findings provide a mechanism by which proteins and lignin can cross-couple in the plant cell wall. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Determination of residual stresses and natural frequencies of roll-tensioned disc by a dynamic simulation of the rolling process

    Science.gov (United States)

    Skordaris, G.; Bouzakis, K.-D.; Tasoulas, D.

    2017-02-01

    Roll tensioning is a common method for increasing locally the superficial strength of thin circular saws and in this way their dynamic stability. Through roll tensioning, residual stresses are induced into the disc material leading to a significant enhancement of its dynamic stiffness. In this paper, a FEM-methodology is proposed for determining the developed residual stresses in the discs after rolling and for investigating their effects on the circular saw natural frequencies. More specifically, a 3D-FEM model was developed for the dynamic simulation of the rolling process on circular saws, using the LS-DYNA software. This model enables the explicit determination of the developed residual stresses in the roll-tensioned discs. Furthermore, the natural frequencies of the pre-stressed circular saws were calculated by the ANSYS software. In these calculations, the already determined residual stresses were taken into consideration. Different distances of the roll-tensioned zone from the disc centre were taken into account for estimating their effect on the disc’s natural frequencies. By the proposed methodology, optimum roll-tensioning conditions can be predicted for improving the dynamic behaviour of thin circular saws during cutting.

  7. Determination of the Ability to Measure Traces of Water in Dehydrated Residues of Waste Water by IR Diffuse Reflectance Spectra

    Science.gov (United States)

    Pratsenka, S. V.; Voropai, E. S.; Belkin, V. G.

    2018-01-01

    Rapid measurement of the moisture content of dehydrated residues is a critical problem, the solution of which will increase the efficiency of treatment facilities and optimize the process of applying flocculants. The ability to determine the moisture content of dehydrated residues using a meter operating on the IR reflectance principle was confirmed experimentally. The most suitable interference filters were selected based on an analysis of the obtained diffuse reflectance spectrum of the dehydrated residue in the range 1.0-2.7 μm. Calibration curves were constructed and compared for each filter set. A measuring filter with a transmittance maximum at 1.19 μm and a reference filter with a maximum at 1.3 μm gave the best agreement with the laboratory measurements.

  8. Fast Curing Bio-Based Phenolic Resins via Lignin Demethylated under Mild Reaction Condition

    Directory of Open Access Journals (Sweden)

    Jiongjiong Li

    2017-09-01

    Full Text Available Demethylation technique has been used to enhance lignin reactivity for preparation of phenolic resins. However, the demethylation efficiency and the demethylated lignin (DL reactivity were still unsatisfactory. To improve the demethylation efficiency, alkali lignin was demethylated under different mild conditions using sodium sulfite as a catalyst. Lignin and DL were characterized by 1H-NMR (nuclear magnetic resonance and Fourier transform infrared (FT-IR spectroscopy to determine the demethylation mechanism. With the demethylation of lignin, the methoxyl group content decreased from 1.93 m mol/g to 1.09 m mol/g, and the phenolic hydroxyl group content increased from 0.56 m mol/g to 0.82 m mol/g. These results revealed that methoxyl groups were attacked by SO32−, and some methoxyl groups were converted to phenolic hydroxyl groups by a nucleophilic substitution reaction, generating DL with high reactivity. The chemical properties of lignin-based phenolic resins were studied by 13C-NMR and FT-IR spectroscopy, and their physical properties were also investigated. The results indicated that lignin-based phenolic resins exhibited faster curing rate and shorter gel time. In addition, the bonding strength increased from 0.92 MPa to 1.07 MPa, and the formaldehyde emission decreased from 0.58 mg/L to 0.22 mg/L after lignin demethylated at the optimum condition.

  9. Determination of the residue levels of nicarbazin and combination nicarbazin-narasin in broiler chickens after oral administration

    Science.gov (United States)

    da Silva, Guilherme Resende; de Assis, Débora Cristina Sampaio; Cançado, Silvana de Vasconcelos

    2017-01-01

    The depletion times of the anticoccidial nicarbazin administered individually and of nicarbazin and narasin administered in combination were evaluated by determining the presence and levels of 4,4'-dinitrocarbanilide (DNC), the marker residue for nicarbazin, and narasin residues in the muscle tissues of broiler chickens subjected to a pharmacological treatment. A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was used. The results showed the presence of all anticoccidial residues; however, the DNC levels were higher when the nicarbazin was administered individually than when it was used in association with narasin throughout the experimental period. After six days of withdrawal, the DNC level following nicarbazin administration alone was lower than the maximum residue level (MRL) of 200 μg kg-1. However, when the nicarbazin was co-administered with narasin, the concentrations of DNC were lower than the MRL after four days of withdrawal. These results may be justified because the dosage of nicarbazin, when administrated individually, is greater than when it is used in combination with narasin. The levels of narasin were lower than the MRL of 15 μg kg-1 throughout the evaluation period. It was concluded that nicarbazin is rapidly metabolized from the broiler muscles up to six days of withdrawal since the DNC levels were lower than the maximum residue level (MRL) and the concentrations of narasin were lower than the MRL throughout the evaluation period. PMID:28750013

  10. TCR-contacting residues orientation and HLA-DRβ* binding preference determine long-lasting protective immunity against malaria

    International Nuclear Information System (INIS)

    Alba, Martha P.; Suarez, Carlos F.; Varela, Yahson; Patarroyo, Manuel A.; Bermudez, Adriana; Patarroyo, Manuel E.

    2016-01-01

    Fully-protective, long-lasting, immunological (FPLLI) memory against Plasmodium falciparum malaria regarding immune protection-inducing protein structures (IMPIPS) vaccinated into monkeys previously challenged and re-challenged 60 days later with a lethal Aotus monkey-adapted P. falciparum strain was found to be associated with preferential high binding capacity to HLA-DRβ1* allelic molecules of the major histocompatibility class II (MHC-II), rather than HLA-DRβ3*, β4*, β5* alleles. Complete PPII L 3D structure, a longer distance (26.5 Å ± 1.5 Å) between residues perfectly fitting into HLA-DRβ1*PBR pockets 1 and 9, a gauche − rotamer orientation in p8 TCR-contacting polar residue and a larger volume of polar p2 residues was also found. This data, in association with previously-described p3 and p7 apolar residues having gauche + orientation to form a perfect MHC-II-peptide-TCR complex, determines the stereo-electronic and topochemical characteristics associated with FPLLI immunological memory. - Highlights: • Stereo-electronic and topochemical rules associated with FPLLI immunological memory. • Presence of very high long-lasting antibody titres against Plasmodium falciparum Spz. • Protective memory induction associated with a binding capacity to HLA-DRβ1*. • gauche − rotamer orientation in p8 polar residue is related to is related to immunological memory.

  11. Determination of the residue levels of nicarbazin and combination nicarbazin-narasin in broiler chickens after oral administration.

    Science.gov (United States)

    Lima, Arina Lopes de; Barreto, Fabiano; Rau, Renata Batista; Silva, Guilherme Resende da; Lara, Leonardo José Camargos; Figueiredo, Tadeu Chaves de; Assis, Débora Cristina Sampaio de; Cançado, Silvana de Vasconcelos

    2017-01-01

    The depletion times of the anticoccidial nicarbazin administered individually and of nicarbazin and narasin administered in combination were evaluated by determining the presence and levels of 4,4'-dinitrocarbanilide (DNC), the marker residue for nicarbazin, and narasin residues in the muscle tissues of broiler chickens subjected to a pharmacological treatment. A high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was used. The results showed the presence of all anticoccidial residues; however, the DNC levels were higher when the nicarbazin was administered individually than when it was used in association with narasin throughout the experimental period. After six days of withdrawal, the DNC level following nicarbazin administration alone was lower than the maximum residue level (MRL) of 200 μg kg-1. However, when the nicarbazin was co-administered with narasin, the concentrations of DNC were lower than the MRL after four days of withdrawal. These results may be justified because the dosage of nicarbazin, when administrated individually, is greater than when it is used in combination with narasin. The levels of narasin were lower than the MRL of 15 μg kg-1 throughout the evaluation period. It was concluded that nicarbazin is rapidly metabolized from the broiler muscles up to six days of withdrawal since the DNC levels were lower than the maximum residue level (MRL) and the concentrations of narasin were lower than the MRL throughout the evaluation period.

  12. TCR-contacting residues orientation and HLA-DRβ* binding preference determine long-lasting protective immunity against malaria

    Energy Technology Data Exchange (ETDEWEB)

    Alba, Martha P.; Suarez, Carlos F. [Fundación Instituto de Inmunología de Colombia (FIDIC), Bogotá D. C. (Colombia); Universidad del Rosario, Bogotá D. C. (Colombia); Universidad de Ciencias Aplicadas y Ambientales (UDCA), Bogotá (Colombia); Varela, Yahson [Fundación Instituto de Inmunología de Colombia (FIDIC), Bogotá D. C. (Colombia); Patarroyo, Manuel A.; Bermudez, Adriana [Fundación Instituto de Inmunología de Colombia (FIDIC), Bogotá D. C. (Colombia); Universidad del Rosario, Bogotá D. C. (Colombia); Patarroyo, Manuel E., E-mail: mepatarr@gmail.com [Fundación Instituto de Inmunología de Colombia (FIDIC), Bogotá D. C. (Colombia); Universidad Nacional de Colombia, Bogotá D. C. (Colombia)

    2016-09-02

    Fully-protective, long-lasting, immunological (FPLLI) memory against Plasmodium falciparum malaria regarding immune protection-inducing protein structures (IMPIPS) vaccinated into monkeys previously challenged and re-challenged 60 days later with a lethal Aotus monkey-adapted P. falciparum strain was found to be associated with preferential high binding capacity to HLA-DRβ1* allelic molecules of the major histocompatibility class II (MHC-II), rather than HLA-DRβ3*, β4*, β5* alleles. Complete PPII{sub L} 3D structure, a longer distance (26.5 Å ± 1.5 Å) between residues perfectly fitting into HLA-DRβ1*PBR pockets 1 and 9, a gauche{sup −} rotamer orientation in p8 TCR-contacting polar residue and a larger volume of polar p2 residues was also found. This data, in association with previously-described p3 and p7 apolar residues having gauche{sup +} orientation to form a perfect MHC-II-peptide-TCR complex, determines the stereo-electronic and topochemical characteristics associated with FPLLI immunological memory. - Highlights: • Stereo-electronic and topochemical rules associated with FPLLI immunological memory. • Presence of very high long-lasting antibody titres against Plasmodium falciparum Spz. • Protective memory induction associated with a binding capacity to HLA-DRβ1*. • gauche{sup −} rotamer orientation in p8 polar residue is related to is related to immunological memory.

  13. DETERMINACIÓN DE FENOLES TOTALES EN DERIVADOS LÍGNICOS OBTENIDOS DEL “LICOR NEGRO” COMO ALTERNATIVA DE PRODUCCIÓN // DETERMINATION OF TOTAL PHENOL DERIVATIVES OBTAINED FROM LIGNIN "BLACK LIQUOR" AS ALTERNATIVE TO PRODUCTION

    Directory of Open Access Journals (Sweden)

    María José López Villalobos

    2015-06-01

    Full Text Available Lignin is an industrial waste being worthless in papermaking byproduct of black liquor obtained from the pulping process in some Venezuelan plants. The black liquor is obtained from the Kraft pulping process to extract lignin sulphite by acid precipitation and quantify the amount of total phenols in such lignin products used in this study. Spectrophotometry Molecular absorption in the UV-Visible and Infrared Spectroscopy (FTIR region were used to carry out these study techniques. The products obtained in the study had the same signs than commercial lignin (LA, along with the extracted lignin present little degradation HCl, confirmed by infrared spectra. Also, the amount of total phenols was quantified in derivative lignin obtained using the Folin-Ciocalteu. In the sulphite process extracted lignin with acetic acid derivative contains more phenols, and in the Kraft process, the derivative lignin extracted with fewer nitric acid present. The amount of total phenolics present in these derivatives are good for making antiseptics, detergents, nylon, resin and many industrial products. // RESUMEN La lignina es un subproducto del licor negro obtenido del proceso de despulpado en algunas plantas de Venezuela, siendo un desecho industrial que carece de valor en la fabricación de papel. En este estudio se utilizó el licor negro obtenido de los procesos de pulpado Kraft y Sulfito para extraer la lignina mediante precipitaciones ácidas y cuantificar la cantidad de fenoles totales en dichos productos lígnicos. Para llevar a cabo este estudio, se utilizaron las técnicas de Espectrofotometría de Absorción Molecular en la región UV-Visible y la Espectroscopia de Infrarrojo (FTIR. Los productos obtenidos en el estudio presentaron señales similares que la lignina comercial (LA, además la lignina extraída con HCl presentó poca degradación, corroborado por los espectros infrarrojos. Asimismo, se cuantificó la cantidad de fenoles totales en los

  14. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Masiá, Ana [Food and Environmental Safety Research Group, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); Research Center on Desertification (CIDE, UV-CSIC-GV), Carretera Moncada-Náquera, Moncada (Spain); Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin [Unit of Public Health, Hygiene and Environmental Health, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); CIBER Epidemiología y Salud Pública (CIBERESP), Madrid (Spain); Center for Advanced Research in Public Health (CSISP-FISABIO), Valencia (Spain); Picó, Yolanda, E-mail: Yolanda.Pico@uv.es [Food and Environmental Safety Research Group, Department of Preventive Medicine and Public Health, Food Science, Toxicology and Legal Medicine, University of Valencia, Valencia (Spain); Research Center on Desertification (CIDE, UV-CSIC-GV), Carretera Moncada-Náquera, Moncada (Spain); CIBER Epidemiología y Salud Pública (CIBERESP), Madrid (Spain)

    2016-09-14

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. - Highlights: • An overview of status and future trends in this field. • Analytical method's compliance with guidelines to ensure reliability. • QuEChERS platform is a referent to extract both, pesticides and veterinary drugs in food. • The progress that liquid chromatography has shown in recent years is revised. • Determination of target, non-target and unknowns is

  15. Determination of pesticides and veterinary drug residues in food by liquid chromatography-mass spectrometry: A review

    International Nuclear Information System (INIS)

    Masiá, Ana; Suarez-Varela, Maria Morales; Llopis-Gonzalez, Agustin; Picó, Yolanda

    2016-01-01

    Monitoring of pesticides and veterinary drug residues is required to enforce legislation and guarantee food safety. Liquid chromatography-mass spectrometry (LC-MS) is the prevailing technique for assessing both types of residues because LC offers a versatile and universal separation mechanism suitable for non-gas chromatography (GC) amenable and the majority of GC-amenable compounds. This characteristic becomes more relevant when LC is coupled to MS because the high sensitivity and specificity of the detector allows to apply generic sample preparation procedures, which simultaneously extract a wide variety of residues with different physico-chemical properties. Determination of metabolites and degradation products, non-target suspected screening of an increasing number of residues, and even unknowns identification are also becoming inherent LC-MS advantages thanks to the latest advances. For routine analysis and, in particular, for official surveillance purposes in food control, analytical methods properly validated following strict guidelines are needed. After a brief introduction and an outline of the legislation applicable around the world, aspects such as improvement of specificity of high-throughput methods, resolution and mass accuracy of identification strategies and quantitative accuracy are critically reviewed in this article. In them, extraction, separation and determination are emphasized. The main objective is to offer an assessment of the state of the art and identify research needs and future trends in determining pesticide and veterinary drug residues in food by LC-MS. - Highlights: • An overview of status and future trends in this field. • Analytical method's compliance with guidelines to ensure reliability. • QuEChERS platform is a referent to extract both, pesticides and veterinary drugs in food. • The progress that liquid chromatography has shown in recent years is revised. • Determination of target, non-target and unknowns is

  16. Photography - Determination of thiosulphate and other residual chemicals in processed photographic films, plates and papers - Methylene blue photometric method and silver sulphide densitometric method

    CERN Document Server

    International Organization for Standardization. Geneva

    1977-01-01

    Photography - Determination of thiosulphate and other residual chemicals in processed photographic films, plates and papers - Methylene blue photometric method and silver sulphide densitometric method

  17. Determination of caprolactam and residual vinyl caprolactam monomer in soluplus by mixed mode gel permeation chromatography.

    Science.gov (United States)

    Soman, Ashish; Jerfy, Madhuri

    2014-01-01

    Soluplus, a graft copolymer of polyethylene glycol, vinyl caprolactam and vinyl acetate, is designed to solubilize poorly soluble active pharmaceutical ingredients. A straightforward aqueous gel permeation chromatography method that exploits both size exclusion and adsorption modes of separation was used to separate and quantify the related residual vinyl caprolactam monomer and caprolactam impurity present in Soluplus. This methodology offers a single step analysis of caprolactam and the residual vinyl caprolacatam monomer, yielding similar results to reversed-phase chromatography measurements, which are time-consuming and may involve multi-step sample preparation. The results of this study demonstrate that gel permeation chromatography provides a viable option to traditional reversed-phase chromatography in the quantitative analysis of residual caprolactam and vinyl caprolactam monomers and can be extended to other monomer-polymeric systems.

  18. Determination of pesticide residues in fruits of Nawabshah district, Sindh, Pakistan

    International Nuclear Information System (INIS)

    Anwar, T.; Ahmad, I.; Tahir, S.

    2011-01-01

    Eight fruit samples of apple, guava, orange, grapes, pear, persimmon, banana and pear purchased from the local markets of Nawabshah district, Sindh and residues of pesticide of organophosphate (OP), pyrethroid and organochlorine (OC) (i.e., dichlorvos, fenvalerate, dimethoate, methyl parathion, fenitrothion, cypermethrin, endosulfan, deltamethrin, mevinphos, chlorpyriphos, profenofos and dicofol) were monitored in fruit samples by Gas Chromatography (GC). All the fruit samples were found contaminated except banana and among these only apple samples were found exceeding the maximum residue limits (MRL) of Codex Alimentarius Commission. (author)

  19. Multi-residue determination of plant growth regulators in apples and tomatoes by liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Xue, Jiaying; Wang, Suli; You, Xiangwei; Dong, Jiannan; Han, Lijun; Liu, Fengmao

    2011-11-15

    A sensitive and rapid multi-residue analytical method for plant growth regulators (PGRs) (i.e., chlormequat, mepiquat, paclobutrazol, uniconazole, ethephon and flumetralin) in apples and tomatoes was developed using high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). A homogenised sample was extracted with a mixture of methanol/water (90:10, v/v) and adjusted to pH <3 with formic acid. Primary secondary amine (PSA) adsorbent was used to clean up the sample. The determination was performed using electrospray ionisation (ESI) and a triple quadrupole (QqQ) analyser. Under the optimised method, the results showed that, except for ethephon, the recoveries were 81.8-98.1% in apples and tomatoes at the spiked concentrations of 0.005 to 2 mg/kg, with relative standard deviations (RSDs) of less than 11.7%. The limits of quantification (LOQs) were lower than their maximum residue limits (MRLs). The procedure was concluded as a practical method to determine the PGR residues in fruit and vegetables and is also suitable for the simultaneous analysis of the amounts of samples for routine monitoring. The analytical method described herein demonstrates a strong potential for its application in the field of PGR multi-residue analysis to help assure food safety. Copyright © 2011 John Wiley & Sons, Ltd.

  20. Determination of the energy potential of the Urban Solid Residuals in three municipalities of the county of Luanda. Angola

    International Nuclear Information System (INIS)

    González Diaz, Yudith; Gato Clavell, Tania; Girón Guillot, Rosa L.; Pires Araújo, Luis

    2015-01-01

    The biological conversion of the Urban Solid Residuals (USR) for energy purposes comes winning importance every day, once the urban residuals became considered a source of alternative energy. To foresee the generation of resulting biogas of the process of biological decomposition of the solid residuals of organic origin in the sanitary fillers is fundamental to estimate the energy and economic balance of facilities of recovery of gas. For the appropriate determination of the potential of generation of gases you employment the calculation methodology presented by the Agency of Environmental Protection of United States. In this context, the objective of this article is to quantify the potential of electric power generation coming from the gas methane originating of the Urban Solid Residuals of the municipalities Belas, Cacuaco and Viana of the County of Luanda in Angola. The available energy power was determined annually of the three municipalities. The instinct demonstrates that the biogas flow arrives at the maximum level and it possesses the maximum available Power in the year 2037, obtaining stops the municipalities Belas, Cacuaco and Viana 3330 · 103, 1206.13 · 103 and 2809.23 · 103m 3 /year of profitable methane respectively whose calculated energy potential was respectively of 2316.52, 1358.88 and 3165,02 kW. The carried out calculations not allow alone to evaluate the energy potential of the filler, but also to evaluate, in certain way, the environmental impact for the mitigation of emissions of gases of effect hothouse. (author)

  1. Lignin Biodegradation in Pulp-and-Paper Mill Wastewater by Selected White Rot Fungi

    Directory of Open Access Journals (Sweden)

    Stefania Costa

    2017-12-01

    Full Text Available An investigation has been carried out to explore the lignin-degrading ability of white rot fungi, as B. adusta and P. crysosporium, grown in different media containing (i glucose and mineral salts; (ii a dairy residue; (iii a dairy residue and mineral salts. Both fungi were then used as inoculum to treat synthetic and industrial pulp-and-paper mill wastewater. On synthetic wastewater, up to 97% and 74% of lignin degradation by B. adusta and P. crysosporium, respectively, have been reached. On industrial wastewater, both fungal strains were able to accomplish 100% delignification in 8–10 days, independent from pH control, with a significant reduction of total organic carbon (TOC of the solution. Results have confirmed the great biotechnological potential of both B. adusta and P. crysosporium for complete lignin removal in industrial wastewater, and can open the way to next industrial applications on large scale.

  2. Survey of pesticide residues in table grapes: Determination of processing factors, intake and risk assessment

    DEFF Research Database (Denmark)

    Poulsen, Mette Erecius; Hansen, H.K.; Sloth, Jens Jørgen

    2007-01-01

    , no significant effect was found for organophosphorus pesticides and pyrethroids, whereas the number of samples with residues of benzilates, phenylamids and triazoles was insufficient to demonstrate any significant effects. An intake calculation showed that the average intake from Italian grapes was 3.9 mu g day...

  3. Residual dipolar couplings : a new technique for structure determination of proteins in solution

    NARCIS (Netherlands)

    van Lune, Frouktje Sapke

    2004-01-01

    The aim of the work described in this thesis was to investigate how residual dipolar couplings can be used to resolve or refine the three-dimensional structure of one of the proteins of the phosphoenol-pyruvate phosphotransferase system (PTS), the main transport system for carbohydrates in

  4. Interference of Helix pomatia extracts on the determination of methandriol in veterinary residue control analysis

    OpenAIRE

    LEYSSENS, Luc; VAN PUYMBROECK, Mark; RAUS, Jef

    1998-01-01

    Aqueous solutions containing methandriol (MAD) were incubated with Succus helix pomatia (SHP) or beta-glucuronidase from Escherichia coli (EC). SHP, used for enzymatic hydrolysis of urinary steroid conjugates for residue analysis of anabolic agents, caused transformation of MAD into methyltestosterone. No conversion occurred when bacterial beta-glucuronidase from E. coli was used.

  5. Deamidation of asparagine and glutamine residues in proteins and peptides: structural determinants and analytical methodology

    NARCIS (Netherlands)

    Bischoff, Rainer; Kolbe, H.V.

    1994-01-01

    Non-enzymatic deamidation of asparagine and glutamine residues in proteins and peptides are reviewed by first outlining the well-described reaction mechanism involving cyclic imide intermediates, followed by a discussion of structural features which influence the reaction rate. The second and major

  6. Residual stresses determination by neutron diffraction in a 100Cr6 chromium steel bearing ring

    Czech Academy of Sciences Publication Activity Database

    Rogante, M.; Martinat, G.; Mikula, Pavol; Vrána, Miroslav

    2013-01-01

    Roč. 51, č. 5 (2013), s. 275-281 ISSN 0023-432X R&D Projects: GA MŠk(XE) LM2011019 Institutional support: RVO:61389005 Keywords : 100Cr6 steel * rings * martensitic hardening * tempering * residual stress es * neutron diffraction Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.546, year: 2013

  7. Experimental determination and theoretical analysis of local residual stress at grain scale

    NARCIS (Netherlands)

    Basu, Indranil; Ocelík, Václav; De Hosson, Jeff Th M.

    2017-01-01

    Grain/phase boundaries contribute significantly to build up of residual stresses, owing to varied plastic/thermal response of different grain orientations or phases during thermomechanical treatment. Hence, accurate quantification of such local scale stress gradients in commercial components is

  8. Determination of residual oil in diesel oil by spectrofluorimetric and chemometric analysis.

    Science.gov (United States)

    Corgozinho, Camila N C; Pasa, Vânya M D; Barbeira, Paulo J S

    2008-07-15

    Multivariate calibration (PLS), principal components analysis (PCA) and linear discriminant analysis (LDA), associated to synchronous spectrofluorimetry, were used to identify and quantify non-transesterified residual vegetable oil in diesel oil with the addition of 2% of biodiesel (B2). The addition of residual oil, one of the easiest ways of adultering fuel, damages engines and leads to tax evasion. Using this method, the samples of diesel oil, B2, and B2 contaminated with residual oil were classified correctly and separated into three well-defined groups. The quantification of residual oil in B2 was carried out in the 0-25% (w/w) band, RMSEC and RMSEP values ranging from 0.26 to 0.48% (w/w) and 1.6-2.6% (w/w), respectively. The method is highly sensitive and efficient to identify and quantify this type of adulterant in which 100% of the samples were correctly classified and the average relative error was approximately 4% in the range 0.5-25% (w/w).

  9. Lignin-Retaining Transparent Wood.

    Science.gov (United States)

    Li, Yuanyuan; Fu, Qiliang; Rojas, Ramiro; Yan, Min; Lawoko, Martin; Berglund, Lars

    2017-09-11

    Optically transparent wood, combining optical and mechanical performance, is an emerging new material for light-transmitting structures in buildings with the aim of reducing energy consumption. One of the main obstacles for transparent wood fabrication is delignification, where around 30 wt % of wood tissue is removed to reduce light absorption and refractive index mismatch. This step is time consuming and not environmentally benign. Moreover, lignin removal weakens the wood structure, limiting the fabrication of large structures. A green and industrially feasible method has now been developed to prepare transparent wood. Up to 80 wt % of lignin is preserved, leading to a stronger wood template compared to the delignified alternative. After polymer infiltration, a high-lignin-content transparent wood with transmittance of 83 %, haze of 75 %, thermal conductivity of 0.23 W mK -1 , and work-tofracture of 1.2 MJ m -3 (a magnitude higher than glass) was obtained. This transparent wood preparation method is efficient and applicable to various wood species. The transparent wood obtained shows potential for application in energy-saving buildings. © 2017 The Authors. Published by Wiley-VCH Verlag GmbH & Co. KGaA.

  10. The impact of alterations in lignin deposition on cellulose organization of the plant cell wall

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Jiliang; Kim, Jeong Im; Cusumano, Joanne C.; Chapple, Clint; Venugopalan, Nagarajan; Fischetti, Robert F.; Makowski, Lee

    2016-06-17

    Background: Coordination of synthesis and assembly of the polymeric components of cell walls is essential for plant growth and development. Given the degree of co-mingling and cross-linking among cell wall components, cellulose organization must be dependent on the organization of other polymers such as lignin. Here we seek to identify aspects of that codependency by studying the structural organization of cellulose fibrils in stems from Arabidopsis plants harboring mutations in genes encoding enzymes involved in lignin biosynthesis. Plants containing high levels of G-lignin, S-lignin, H-lignin, aldehyde-rich lignin, and ferulic acid-containing lignin, along with plants with very low lignin content were grown and harvested and longitudinal sections of stem were prepared and dried. Scanning X-ray microdiffraction was carried out using a 5-micron beam that moved across the sections in 5-micron steps and complete diffraction patterns were collected at each raster point. Approximately, 16,000 diffraction patterns were analyzed to determine cellulose fibril orientation and order within the tissues making up the stems. Results: Several mutations-most notably those exhibiting (1) down-regulation of cinnamoyl CoA reductase which leads to cell walls deficient in lignin and (2) defect of cinnamic acid 4-hydroxylase which greatly reduces lignin content-exhibited significant decrease in the proportion of oriented cellulose fibrils in the cell wall. Distinctions between tissues were maintained in all variants and even in plants exhibiting dramatic changes in cellulosic order the trends between tissues (where apparent) were generally maintained. The resilience of cellulose to degradative processes was investigated by carrying out the same analysis on samples stored in water for 30 days prior to data collection. This treatment led to significant loss of cellulosic order in plants rich in aldehyde or H-lignin, less change in wild type, and essentially no change in samples with

  11. Dataset on the structural characterization of organosolv lignin obtained from ensiled Poaceae grass and load-dependent molecular weight changes during thermoplastic processing.

    Science.gov (United States)

    Dörrstein, Jörg; Scholz, Ronja; Schwarz, Dominik; Schieder, Doris; Sieber, Volker; Walther, Frank; Zollfrank, Cordt

    2018-04-01

    This article presents experimental data of organosolv lignin from Poacea grass and structural changes after compounding and injection molding as presented in the research article "Effects of high-lignin-loading on thermal, mechanical, and morphological properties of bioplastic composites" [1]. It supplements the article with morphological (SEM), spectroscopic ( 31 P NMR, FT-IR) and chromatographic (GPC, EA) data of the starting lignin as well as molar mass characteristics (mass average molar mass (M w ) and Polydispersity (D)) of the extracted lignin. Refer to Schwarz et al. [2] for a detailed description of the production of the organosolv residue and for further information on the raw material used for lignin extraction. The dataset is made publicly available and can be useful for extended lignin research and critical analyzes.

  12. Determination of crop residues and the physical and mechanical properties of soil in different tillage systems

    Directory of Open Access Journals (Sweden)

    P Ahmadi Moghaddam

    2016-04-01

    Full Text Available Introduction: Monitoring and management of soil quality is crucial for sustaining soil function in ecosystem. Tillage is one of the management operations that drastically affect soil physical quality. Conservation tillage methods are one of the efficient solutions in agriculture to reduce the soil erosion, air pollution, energy consumption, and the costs, if there is a proper management on the crop residues. One of the serious problems in agriculture is soil erosion which is rapidly increased in the recent decades as the intensity of tillage increases. This phenomenon occurs more in sloping lands or in the fields which are lacking from crop residues and organic materials. The conservation tillage has an important role in minimizing soil erosion and developing the quality of soil. Hence, it has attracted the attention of more researchers and farmers in the recent years. Materials and Methods: In this study, the effect of different tillage methods has been investigated on the crop residues, mechanical resistance of soil, and the stability of aggregates. This research was performed on the agricultural fields of Urmia University, located in Nazloo zone in 2012. Wheat and barley were planted in these fields, consecutively. The soil texture of these fields was loamy clay and the factorial experiments were done in a completely randomized block design. In this study, effect of three tillage systems including tillage with moldboard (conventional tillage, tillage with disk plow (reduced tillage, chisel plow (minimum tillage and control treatment on some soil physical properties was investigated. Depth is second factor that was investigated in three levels including 0-60, 60-140, and 140-200 mm. Moreover, the effect of different percentages of crop residues on the rolling resistance of non-driving wheels was studied in a soil bin. The contents of crop residues have been measured by using the linear transects and image processing methods. In the linear

  13. Can laccases catalyze bond cleavage in lignin?

    DEFF Research Database (Denmark)

    Munk, Line; Sitarz, Anna Katarzyna; Kalyani, Dayanand

    2015-01-01

    Modification of lignin is recognized as an important aspect of the successful refining of lignocellulosic biomass, and enzyme-assisted processing and upcycling of lignin is receiving significant attention in the literature. Laccases (EC 1.103.2) are taking the centerstage of this attention, since...... these enzymes may help degrading lignin, using oxygen as the oxidant. Laccases can catalyze polymerization of lignin, but the question is whether and how laccases can directly catalyze modification of lignin via catalytic bond cleavage. Via a thorough review of the available literature and detailed...... illustrations of the putative laccase catalyzed reactions, including the possible reactions of the reactive radical intermediates taking place after the initial oxidation of the phenol-hydroxyl groups, we show that i) Laccase activity is able to catalyze bond cleavage in low molecular weight phenolic lignin...

  14. Chemicals from Lignin: An Interplay of Lignocellulose Fractionation, Depolymerisation, and Upgrading

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Schutyser, Wouter [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Renders, Tom [KU Leuven; Van den Bosch, Sander [KU Leuven; Koelewijn, Steven-Friso [KU Leuven; Sels, Bert F. [KU Leuven

    2018-01-01

    In pursuit of more sustainable and competitive biorefineries, the effective valorisation of lignin is key. An alluring opportunity is the exploitation of lignin as a resource for chemicals. Three technological biorefinery aspects will determine the realisation of a successful lignin-to-chemicals valorisation chain, namely (i) lignocellulose fractionation, (ii) lignin depolymerisation, and (iii) upgrading towards targeted chemicals. This review provides a summary and perspective of the extensive research that has been devoted to each of these three interconnected biorefinery aspects, ranging from industrially well-established techniques to the latest cutting edge innovations. To navigate the reader through the overwhelming collection of literature on each topic, distinct strategies/topics were delineated and summarised in comprehensive overview figures. Upon closer inspection, conceptual principles arise that rationalise the success of certain methodologies, and more importantly, can guide future research to further expand the portfolio of promising technologies. When targeting chemicals, a key objective during the fractionation and depolymerisation stage is to minimise lignin condensation (i.e. formation of resistive carbon-carbon linkages). During fractionation, this can be achieved by either (i) preserving the (native) lignin structure or (ii) by tolerating depolymerisation of the lignin polymer but preventing condensation through chemical quenching or physical removal of reactive intermediates. The latter strategy is also commonly applied in the lignin depolymerisation stage, while an alternative approach is to augment the relative rate of depolymerisation vs. condensation by enhancing the reactivity of the lignin structure towards depolymerisation. Finally, because depolymerised lignins often consist of a complex mixture of various compounds, upgrading of the raw product mixture through convergent transformations embodies a promising approach to decrease the

  15. Enzymatic depolymerization of lignin by laccases

    OpenAIRE

    Hamidi, Nor Hanimah

    2013-01-01

    More than half of platform petrochemicals are aromatic, whereas the only large-scale, naturally-occurring, renewable source of aromatics is lignin. Chemical depolymerization of lignin requires extreme conditions, and results in extensive destruction of the aromatic rings and/or char formation. By contrast, enzymatic lignin depolymerization occurs under mild conditions with retention of the aromatic nuclei. Therefore, laccase from Agaricus bisporus (LAB) and from Trametes versicolor (LTV) with...

  16. Red Xylem and Higher Lignin Extractability by Down-Regulating a Cinnamyl Alcohol Dehydrogenase in Poplar.

    Science.gov (United States)

    Baucher, M.; Chabbert, B.; Pilate, G.; Van Doorsselaere, J.; Tollier, M. T.; Petit-Conil, M.; Cornu, D.; Monties, B.; Van Montagu, M.; Inze, D.; Jouanin, L.; Boerjan, W.

    1996-12-01

    Cinnamyl alcohol dehydrogenase (CAD) catalyzes the last step in the biosynthesis of the lignin precursors, the monolignols. We have down-regulated CAD in transgenic poplar (Populus tremula X Populus alba) by both antisense and co-suppression strategies. Several antisense and sense CAD transgenic poplars had an approximately 70% reduced CAD activity that was associated with a red coloration of the xylem tissue. Neither the lignin amount nor the lignin monomeric composition (syringyl/guaiacyl) were significantly modified. However, phloroglucinol-HCl staining was different in the down-regulated CAD plants, suggesting changes in the number of aldehyde units in the lignin. Furthermore, the reactivity of the cell wall toward alkali treatment was altered: a lower amount of lignin was found in the insoluble, saponified residue and more lignin could be precipitated from the soluble alkali fraction. Moreover, large amounts of phenolic compounds, vanillin and especially syringaldehyde, were detected in the soluble alkali fraction of the CAD down-regulated poplars. Alkaline pulping experiments on 3-month-old trees showed a reduction of the kappa number without affecting the degree of cellulose degradation. These results indicate that reducing the CAD activity in trees might be a valuable strategy to optimize certain processes of the wood industry, especially those of the pulp and paper industry.

  17. Structural characterization of lignin from leaf sheaths of "dwarf cavendish" banana plant.

    Science.gov (United States)

    Oliveira, Lúcia; Evtuguin, Dmitry V; Cordeiro, Nereida; Silvestre, Armando J D; Silva, Artur M S; Torres, Isabel C

    2006-04-05

    Dioxane lignin (DL) isolated from leaf sheaths of banana plant (Musa acuminata Colla var. cavendish) and in situ lignin were submitted to a comprehensive structural characterization employing spectroscopic (UV, FTIR, solid state 13C CP-MAS NMR, liquid state 13C and 1H NMR) and chemical degradation techniques (permanganate and nitrobenzene oxidation). Results obtained showed that banana plant leaf sheath lignin is of HGS type with a molar proportion of p-hydroxyphenyl (H)/guaiacyl (G)/syringyl (S) units of 12:25:63. Most of the H units in DL are terminal phenolic coumarates linked to other lignin substructures by benzyl and Cgamma-ester bonds in contrast to ferulates that are mainly ether linked to bulk lignin. It is proposed that banana plant leaf sheath lignin is chemically bonded to suberin-like components of cell tissues by ester linkages via essentially hydroxycinnamic acid residues. beta-O-4 structures (0.31/C6), the most abundant in DL, comprise mainly S units, whereas a significant proportion of G units is bonded by beta-5, 5-5', and 4-O-5' linkages contributing to ca. 80% of condensed structures in DL.

  18. Bio-based polyurethane prepared from Kraft lignin and modified castor oil

    Directory of Open Access Journals (Sweden)

    L. B. Tavares

    2016-11-01

    Full Text Available Current challenges highlight the need for polymer research using renewable natural sources as a substitute for petroleum-based polymers. The use of polyols obtained from renewable sources combined with the reuse of industrial residues such as lignin is an important agent in this process. Different compositions of polyurethane-type materials were prepared by combining technical Kraft lignin (TKL with castor oil (CO or modified castor oil (MCO1 and MCO2 to increase their reactivity towards diphenylmethane diisocyanate (MDI. The results indicate that lignin increases the glass transition temperature, the crosslinking density and improves the ultimate stress especially for those prepared from MCO2 and 30% lignin content from 8.2 MPa (lignin free to 23.5 MPa. Scanning electron microscopy (SEM micrographs of rupture surface after uniaxial tensile tests show ductile-to-brittle transition. The results show the possibility to develop polyurethane-type materials, varying technical grade Kraft lignin content, which cover a wide range of mechanical properties (from large elastic/low Young modulus to brittle/high Young modulus polyurethanes.

  19. Multi-residue determination of 115 veterinary drugs and pharmaceutical residues in milk powder, butter, fish tissue and eggs using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Dasenaki, Marilena E; Thomaidis, Nikolaos S

    2015-06-23

    A simple and sensitive multi-residue method for the determination of 115 veterinary drugs and pharmaceuticals, belonging in more than 20 different classes, in butter, milk powder, egg and fish tissue has been developed. The method involves a simple generic solid-liquid extraction step (solvent extraction, SE) with 0.1% formic acid in aqueous solution of EDTA 0.1% (w/v)-acetonitrile (ACN)-methanol (MeOH) (1:1:1, v/v) with additional ultrasonic-assisted extraction. Precipitation of lipids and proteins was promoted by subjecting the extracts at very low temperature (-23°C) for 12h. Further cleanup with hexane ensures fat removal from the matrix. Analysis was performed by liquid chromatography coupled with electrospray ionization and tandem mass spectrometry (LC-ESI-MS/MS). Two separate runs were performed for positive and negative ionization in multiple reaction monitoring mode (MRM). Particular attention was devoted to extraction optimization: different sample-to-extracting volume ratios, different concentrations of formic acid in the extraction solvent and different ultrasonic extraction temperatures were tested in butter, egg and milk powder samples. The method was also applied in fish tissue samples. It was validated, on the basis of international guidelines, for all four matrices. Quantitative analysis was performed by means of standard addition calibration. For over 80% of the analytes, the recoveries were between 50% and 120% in all matrices studied, with RSD values in the range of 1-18%. Limits of detection (LODs) and quantification (LOQs) ranged from 0.008 μg kg(-1) (oxfendazole in butter) to 3.15 μg kg(-1) (hydrochlorthiazide in egg). The evaluated method provides reliable screening, quantification, and identification of 115 veterinary drug and pharmaceutical residues in foods of animal origin and has been successfully applied in real samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  20. Determination of Thermal Properties and Morphology of Eucalyptus Wood Residue Filled High Density Polyethylene Composites

    Directory of Open Access Journals (Sweden)

    Ayse Kabakci

    2008-02-01

    Full Text Available Thermal behaviors of eucalyptus wood residue (EWR filled recycled high density polyethylene (HDPE composites have been measured applying the thermogravimetric analysis (TGA and differential scanning calorimetry (DSC. Morphology of the materials was also studied using scanning electron microscope (SEM. Addition of the EWR into the recycled HDPE matrix reduced the starting of degradation temperature. EWR filled recycled HDPE had two main decomposition peaks, one for EWR around 350 °C and one for recycled HDPE around 460 °C. Addition of EWR did not affect the melting temperature of the recycled HDPE. Morphological study showed that addition of coupling agent improved the compatibility between wood residue and recycled HDPE.

  1. Air temperature determination inside residual heat removal pump room of Angra-1 nuclear power plant after a design basic accident

    International Nuclear Information System (INIS)

    Siniscalchi, Marcio Rezende

    2005-01-01

    This work develops heat transfer theoretical models for determination of air temperature inside the Residual Heat Removal Pump Room of Angra 1 Nuclear Power Plant after a Design Basis Accident without forced ventilation. Two models had been developed. The differential equations are solved by analytical methods. A software in FORTRAN language are developed for simulations of temperature inside rooms for different geometries and materials. (author)

  2. Aromatic residue position on the nonpolar face of class a amphipathic helical peptides determines biological activity.

    Science.gov (United States)

    Datta, Geeta; Epand, Raquel F; Epand, Richard M; Chaddha, Manjula; Kirksey, Matthew A; Garber, David W; Lund-Katz, Sissel; Phillips, Michael C; Hama, Susan; Navab, Mohamad; Fogelman, Alan M; Palgunachari, Mayakonda N; Segrest, Jere P; Anantharamaiah, G M

    2004-06-18

    The apolipoprotein A-I mimetic peptide 4F (Ac-DWFKAFYDKVAEKFKEAF-NH(2)), with four Phe residues on the nonpolar face of the amphipathic alpha-helix, is strongly anti-inflammatory, whereas two 3F analogs (3F(3) and 3F(14)) are not. To understand how changes in helix nonpolar face structure affect function, two additional 3F analogs, Ac-DKLKAFYDKVFEWAKEAF-NH(2) (3F-1) and Ac-DKWKAVYDKFAEAFKEFL-NH(2) (3F-2), were designed using the same amino acid composition as 3F(3) and 3F(14). The aromatic residues in 3F-1 and 3F-2 are near the polar-nonpolar interface and at the center of the nonpolar face of the helix, respectively. Like 4F, but in contrast to 3F(3) and 3F(14), these peptides effectively inhibited lytic peptide-induced hemolysis, oxidized phospholipid-induced monocyte chemotaxis, and scavenged lipid hydroperoxides from low density lipoprotein. High pressure liquid chromatography retention times and monolayer exclusion pressures indicated that there is no direct correlation of peptide function with lipid affinity. Fluorescence studies suggested that, although the peptides bind phospholipids similarly, the Trp residue in 4F, 3F-1, and 3F-2 is less motionally restricted than in 3F(3) and 3F(14). Based on these results and molecular modeling studies, we propose that the arrangement of aromatic residues in class A amphipathic helical molecules regulates entry of reactive oxygen species into peptide-phospholipid complexes, thereby reducing the extent of monocyte chemotaxis, an important step in atherosclerosis.

  3. Determination of spallation residues in thin target: toward an hybrid reactor lead target simulation

    International Nuclear Information System (INIS)

    Audouin, L.; Tassan-Got, L.; Bernas, M.; Rejmund, F.; Stephan, C.; Taieb, J.; Boudard, A.; Fernandez, B.; Legrain, R.; Leray, S.; Volant, C.; Wlazlo, W.; Benlliure, J.; Casajeros, E.; Pereira, J.; Czajkowski, S.

    2001-01-01

    The production of spallation primary residual nuclei in thin target has been studied by measurement of isotopic yields distributions for several systems. Issues relevant for the design of accelerator-driven systems are presented. Monte-Carlo code abilities to reproduce data are studied in details; it is shown that calculations do not reproduce data in a satisfactory way. Future work orientations leading to an improvement of thin targets calculations and ultimately to a thick target simulation are discussed. (author)

  4. Residual Stress in Sprayed Ni+5% Al Coatings Determined by Neutron Diffraction

    Czech Academy of Sciences Publication Activity Database

    Matějíček, Jiří; Sampath, S.; Gnaupel-Herold, T.; Prask, H. J.

    2002-01-01

    Roč. 74, supplement 8 (2002), s. S1692-S1694 ISSN 0947-8396 R&D Projects: GA ČR GA106/01/0094 Grant - others:NSF DMR(US) 6932570 Institutional research plan: CEZ:AV0Z2043910 Keywords : residual stress, thermal spray coatings, neutron diffraction Subject RIV: JK - Corrosion ; Surface Treatment of Materials Impact factor: 2.231, year: 2002

  5. Determination of residual manganese in Mn porphyrin-based superoxide dismutase (SOD) and peroxynitrite reductase mimics

    OpenAIRE

    Rebouças, Júlio S.; Kos, Ivan; Batinić-Haberle, Ines

    2009-01-01

    The awareness of the beneficial effects of Mn porphyrin-based superoxide dismutase (SOD) mimics and peroxynitrite scavengers on decreasing oxidative stress injuries has increased the use of these compounds as mechanistic probes and potential therapeutics. Simple Mn2+ salts, however, have SOD-like activity in their own right both in vitro and in vivo. Thus, quantification/removal of residual Mn2+ species in Mn-based therapeutics is critical to an unambiguous interpretation of biological data. ...

  6. DETERMINATION OF RESIDUAL VALUE WITHIN THE COST BENEFIT ANALYSIS FOR THE PROJECTS FINANCED BY THE EUROPEAN UNION

    Directory of Open Access Journals (Sweden)

    Droj Laurentiu

    2011-12-01

    Full Text Available This paper will be later used within the Doctoral thesis: The Mechanism of Financing Investment Projects by Usage of European Structural Funds, which is currently under development at the University Babes Bolyai Cluj Napoca, Faculty of Economics and Business Management, under the coordination of the prof. univ. dr. Ioan Trenca. An increasing debate is rising recently between the academic community, the business community, the private lending institutions(banks, investment funds, etc. and the officials of the Romanian Government and of the European Union regarding the proposed method for calculation of the residual value in the European financed investment projects. Several methods of calculation of the Residual Value were taken into consideration and contested by different parties in order to prepare and to submit financial analysis studies for investment projects proposed to be financed within the European Regional Development Fund(ERDF. In this context, the present paper proposes to address the three main methods of calculation of the residual value and later to study its impact over the indicators, especially over the Internal Rate of Return, obtained in the financial analysis for an investment project proposed by a Romanian medium sized company. In order to establish the proper method which should be used for selection and calculation of the residual value previously published studies and official documentations were analyzed. The main methods for calculation of the residual values were identified as being the following: A. the residual market value of fixed assets, as if it were to be sold, B. accounting economic depreciation formula and C. by using the net present value of the cash flows. Based on these methods the research model was elaborated, and using the financial data of the proposed infrastructure investment was created a case study. According to the realized study a pattern was established for proper determination of residual value

  7. Polyoxometalate (POM) catalyst systems : chemical principles and reactions with lignin and oxygen

    Science.gov (United States)

    I.A. Weinstock; R.H. Atalla; J.S. Bond; E.M.G. Barbuzzi; V.A. Grigoriev; Y. Gueletii; J.J. Cowan; D.M. Sonnen; R.S. Reiner; S.E. Reichel; R.A. Heintz; C.J. Houtman; A.J. Bailey; C.L. Hill

    2000-01-01

    Chemical data pertinent to most-recently developed POM delignification systems will be presented. These data will be used to demonstrate the fundamental basis for the stability, self-buffering properties, versatility and high selectivity of these systems when used in combination with oxygen to convert native or residual lignin in wood or wood-pulp fibers to CO2 and H2O...

  8. Determination of Residual Stresses and Mechanical Properties using Neutron, X-ray Diffraction, Micro- and Nanoindentation Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Larsson, Cecilia

    2003-12-01

    The existence of residual stresses in engineering materials can significantly affect subsequent lifetime by augmenting or impeding failure. Consequently, for an accurate assessment of engineering lifetimes, there is a need to quantify residual stresses. Furthermore, knowledge of the origin of these stresses in conjunction with mechanical properties such as hardness and fracture toughness, among others, can be used to improve functionality by tailoring the microstructure through processing. In this work, neutron, x-ray diffraction, micro- and nanoindentation techniques were used for residual stress determination and mechanical characterization of WC-Co functionally graded composites, a Co-based Haynes 25 alloy weld, compressed steel and compacted Fe-brass powders. The neutron and x-ray diffraction techniques were used to assess residual strains and stresses while the instrumented indentation techniques were used to determine hardness, fracture toughness and elastic modulus. In each of these engineering materials, valuable insight relating to the overall mechanical performance was obtained. X-ray diffraction was used to determine thermal residual stresses that develop in a functionally graded WC-Co composite, commonly used as tool bits. Microstresses in the graded zone were attributed to the thermal mismatch between WC and the Co phase. The compressive macrostresses were determined to be a result of the compositional gradient. Micro- and nanoindentation experiments were used to determine hardness as a function of depth in two WC-Co functionally graded materials (FGMs). A relationship between hardness and Co phase content was established and explained for the two graded and five homogeneous samples. An experimental and simulation study of residual stresses was made in the vicinity of a gas tungsten arc weld in a Co-based Haynes 25 alloy used in a satellite component. The experimental measurements were made by neutron diffraction on the recently commissioned

  9. Can laccases catalyze bond cleavage in lignin?

    Science.gov (United States)

    Munk, Line; Sitarz, Anna K; Kalyani, Dayanand C; Mikkelsen, J Dalgaard; Meyer, Anne S

    2015-01-01

    Modification of lignin is recognized as an important aspect of the successful refining of lignocellulosic biomass, and enzyme-assisted processing and upcycling of lignin is receiving significant attention in the literature. Laccases (EC 1.10.3.2) are taking the centerstage of this attention, since these enzymes may help degrading lignin, using oxygen as the oxidant. Laccases can catalyze polymerization of lignin, but the question is whether and how laccases can directly catalyze modification of lignin via catalytic bond cleavage. Via a thorough review of the available literature and detailed illustrations of the putative laccase catalyzed reactions, including the possible reactions of the reactive radical intermediates taking place after the initial oxidation of the phenol-hydroxyl groups, we show that i) Laccase activity is able to catalyze bond cleavage in low molecular weight phenolic lignin model compounds; ii) For laccases to catalyze inter-unit bond cleavage in lignin substrates, the presence of a mediator system is required. Clearly, the higher the redox potential of the laccase enzyme, the broader the range of substrates, including o- and p-diphenols, aminophenols, methoxy-substituted phenols, benzenethiols, polyphenols, and polyamines, which may be oxidized. In addition, the currently available analytical methods that can be used to detect enzyme catalyzed changes in lignin are summarized, and an improved nomenclature for unequivocal interpretation of the action of laccases on lignin is proposed. Copyright © 2015 Elsevier Inc. All rights reserved.

  10. Recovering hydrocarbons with surfactants from lignin

    Energy Technology Data Exchange (ETDEWEB)

    Naae, D.G.; Whittington, L.E.; Ledoux, W.A.; Debons, F.E.

    1988-11-29

    This patent describes a method of recovering hydrocarbons from an underground hydrocarbon formation penetrated by at least one injection well and at least one production well, which comprises: injecting into the formation through an injection well a surfactant slug comprising about 0.1% to about 10% by weight of surfactants produced from lignin, the surfactants produced by placing lignin in contact with water, converting the lignin into low molecular weight lignin phenols by reducing the lignin in the presence of a reducing agent of carbon monoxide or hydrogen creating a reduction reaction mixture comprising oil soluble lignin phenols, the reduction occurring at a temperature greater than about 200/sup 0/C and a pressure greater than about 100 psi, recovering the oil soluble lignin phenols from the reduction mixture, and converting the lignin phenols into lignin surfactants by a reaction selected from the group consisting of alkoxylation, sulfonation, sulfation, aklylation, sulfomethylation, and alkoxysulfation; injecting into the formation through the injection well a drive fluid to push the surfactant slug towards a production well; and recovering hydrocarbons at the production well.

  11. Simultaneous determination of organochlorine and pyrethriod pesticide residues in the Chinese patent medicines by gas chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Mao, Xue J; Zhong, Yao; Yan, Ai P; Wang, Bin; Wang, Yuan X; Wan, Yi Q

    2018-02-01

    A simple, sensitive, reliable method was developed for the simultaneous determination of organochlorine and pyrethriod pesticide residues in Chinese patent medicines Six ingredient rehmannia pills and Xiaoyao pills. These pesticides were extracted by ethyl acetate. The extraction time and volume of ethyl acetate were optimized. Cleanup of extracts was performed with dispersive-solid phase extraction using graphitized carbon black as the sorbent. The determination of pesticides in the final extracts was carried out by gas chromatography-tandem mass spectrometry in multiple reaction monitoring mode (GC-MS/MS, MRM). The linearity of the calibration curves is good in matrix-matched standard and yields the coefficients of determination (R 2 ) ≥0.99 for all of the target analytes. Under optimized conditions, the average recoveries (five replicates) for most pesticides range from 75.5% to 114.6%, and RSDs are less than 10.0%. The LODs of 18 pesticides in Six ingredient rehmannia pill and Xiaoyao pills are in the range of 0.01-8.82 μg kg -1 . The developed method meets the requirements of pesticide residue analysis and could be effectively used for routine analysis of the organochlorine and pyrethriod pesticide residues in Six ingredient rehmannia pills and Xiaoyao pills.

  12. Structural characterization of alkaline hydrogen peroxide pretreated grasses exhibiting diverse lignin phenotypes

    Directory of Open Access Journals (Sweden)

    Li Muyang

    2012-06-01

    Full Text Available Abstract Background For cellulosic biofuels processes, suitable characterization of the lignin remaining within the cell wall and correlation of quantified properties of lignin to cell wall polysaccharide enzymatic deconstruction is underrepresented in the literature. This is particularly true for grasses which represent a number of promising bioenergy feedstocks where quantification of grass lignins is particularly problematic due to the high fraction of p-hydroxycinnamates. The main focus of this work is to use grasses with a diverse range of lignin properties, and applying multiple lignin characterization platforms, attempt to correlate the differences in these lignin properties to the susceptibility to alkaline hydrogen peroxide (AHP pretreatment and subsequent enzymatic deconstruction. Results We were able to determine that the enzymatic hydrolysis of cellulose to to glucose (i.e. digestibility of four grasses with relatively diverse lignin phenotypes could be correlated to total lignin content and the content of p-hydroxycinnamates, while S/G ratios did not appear to contribute to the enzymatic digestibility or delignification. The lignins of the brown midrib corn stovers tested were significantly more condensed than a typical commercial corn stover and a significant finding was that pretreatment with alkaline hydrogen peroxide increases the fraction of lignins involved in condensed linkages from 88–95% to ~99% for all the corn stovers tested, which is much more than has been reported in the literature for other pretreatments. This indicates significant scission of β-O-4 bonds by pretreatment and/or induction of lignin condensation reactions. The S/G ratios in grasses determined by analytical pyrolysis are significantly lower than values obtained using either thioacidolysis or 2DHSQC NMR due to presumed interference by ferulates. Conclusions It was found that grass cell wall polysaccharide hydrolysis by cellulolytic enzymes for grasses

  13. Epoxy resin synthesis using low molecular weight lignin separated from various lignocellulosic materials.

    Science.gov (United States)

    Asada, Chikako; Basnet, Sunita; Otsuka, Masaya; Sasaki, Chizuru; Nakamura, Yoshitoshi

    2015-03-01

    A low molecular weight lignin from various lignocellulosic materials was used for the synthesis of bio-based epoxy resins. The lignin extracted with methanol from steam-exploded samples (steaming time of 5 min at steam pressure of 3.5 MPa) from different biomasses (i.e., cedar, eucalyptus, and bamboo) were functionalized by the reaction with epichlorohydrin, catalyzed by a water-soluble phase transfer catalyst tetramethylammonium chloride, which was further reacted with 30 wt% aqueous NaOH for ring closure using methyl ethyl ketone as a solvent. The glycidylated products of the lignin with good yields were cured to epoxy polymer networks with bio-based curing agents i.e., lignin itself and a commercial curing agent TD2131. Relatively good thermal properties of the bio-based epoxy network was obtained and thermal decomposition temperature at 5% weight loss (Td5) of cedar-derived epoxy resin was higher than that derived from eucalyptus and bamboo. The bio-based resin satisfies the stability requirement of epoxy resin applicable for electric circuit boards. The methanol-insoluble residues were enzymatically hydrolyzed to produce glucose. This study indicated that the biomass-derived methanol-soluble lignin may be a promising candidate to be used as a substitute for petroleum-based epoxy resin derived from bisphenol A, while insoluble residues may be processed to give a bioethanol precursor i.e., glucose. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Cost and greenhouse gas emission tradeoffs of alternative uses of lignin for second generation ethanol

    Science.gov (United States)

    Pourhashem, Ghasideh; Adler, Paul R.; McAloon, Andrew J.; Spatari, Sabrina

    2013-06-01

    Second generation ethanol bioconversion technologies are under demonstration-scale development for the production of lignocellulosic fuels to meet the US federal Renewable Fuel Standards (RFS2). Bioconversion technology utilizes the fermentable sugars generated from the cellulosic fraction of the feedstock, and most commonly assumes that the lignin fraction may be used as a source of thermal and electrical energy. We examine the life cycle greenhouse gas (GHG) emission and techno-economic cost tradeoffs for alternative uses of the lignin fraction of agricultural residues (corn stover, and wheat and barley straw) produced within a 2000 dry metric ton per day ethanol biorefinery in three locations in the United States. We compare three scenarios in which the lignin is (1) used as a land amendment to replace soil organic carbon (SOC); (2) separated, dried and sold as a coal substitute to produce electricity; and (3) used to produce electricity onsite at the biorefinery. Results from this analysis indicate that for life cycle GHG intensity, amending the lignin to land is lowest among the three ethanol production options (-25 to -2 g CO2e MJ-1), substituting coal with lignin is second lowest (4-32 g CO2e MJ-1), and onsite power generation is highest (36-41 g CO2e MJ-1). Moreover, the onsite power generation case may not meet RFS2 cellulosic fuel requirements given the uncertainty in electricity substitution. Options that use lignin for energy do so at the expense of SOC loss. The lignin-land amendment option has the lowest capital cost among the three options due to lower equipment costs for the biorefinery’s thermal energy needs and use of biogas generated onsite. The need to purchase electricity and uncertain market value of the lignin-land amendment could raise its cost compared to onsite power generation and electricity co-production. However, assuming a market value (50-100/dry Mg) for nutrient and soil carbon replacement in agricultural soils, and potentially

  15. Reactivity of syringyl and guaiacyl lignin units and delignification kinetics in the kraft pulping of Eucalyptus globulus wood using Py-GC-MS/FID.

    Science.gov (United States)

    Lourenço, Ana; Gominho, Jorge; Marques, António Velez; Pereira, Helena

    2012-11-01

    Eucalyptus globulus sapwood and heartwood showed no differences in lignin content (23.0% vs. 23.7%) and composition: syringyl-lignin (17.9% vs. 18.0%) and guaiacyl-lignin (4.8% vs. 5.2%). Delignification kinetics of S- and G-units in heartwood and sapwood was investigated by Py-GC-MS/FID at 130, 150 and 170°C and modeled as double first-order reactions. Reactivity differences between S and G-units were small during the main pulping phase and the higher reactivity of S over G units was better expressed in the later pulping stage. The residual lignin composition in pulps was different from wood or from samples in the initial delignification stages, with more G and H-units. S/G ratio ranged from 3 to 4.5 when pulp residual lignin was higher than 10%, decreasing rapidly to less than 1. The S/H was initially around 20 (until 15% residual lignin), decreasing to 4 when residual lignin was about 3%. Copyright © 2012 Elsevier Ltd. All rights reserved.

  16. Rheological properties of disperse systems based on hydrolyzed lignin and oil

    Science.gov (United States)

    Savitskaya, T. A.; Reznikov, I. V.; Shcheglov, V. A.; Tsygankova, N. G.; Telysheva, G. M.; Grinshpan, D. D.

    2012-05-01

    The rheological properties of oil dispersions of hydrophobized hydrolyzed lignin, which is an effective sorbent of oil and oil products, have been studied. It has been shown that at a lignin concentration of over 10%, free-disperse systems with Newton flow go over to coagulation thixotropic structures, demonstrating the pseudoplastic character of flow. The structural-mechanical characteristics of highly filled (lignin content of 40-45%) dispersions have been determined and the concentration region of existence of an oil-saturated sorbent in the form of a solid product easily removed from the water surface has been established.

  17. Determination of pesticide residue transfer rates (percent) from dried tea leaves to brewed tea.

    Science.gov (United States)

    Wang, Jian; Cheung, Wendy; Leung, Daniel

    2014-01-29

    This paper presents a study on pesticide residue transfer rates (%) from dried tea leaves to brewed tea. In the study, a brewing procedure simulated the preparation of a hot tea drink as in routine. After brewing, pesticide residues were extracted from brewed tea using a method known as QuEChERS (quick, easy, cheap, effective, rugged, and safe). An UHPLC/ESI-MS/MS method was developed and validated to identify and quantify up to 172 pesticides in both tea leaves and brewed tea samples. Quantification was achieved using matrix-matched standard calibration curves with isotopically labeled standards or a chemical analogue as internal standards, and the calibration curves consisted of six points (0.4, 2.0, 8.0, 16.0, 24.0, and 40.0 μg/L equivalent in sample). The method was validated at four concentration levels (4.0, 12, 20.0, and 32.0 μg/L equivalent in sample) using five different brewed tea matrices on two separate days per matrix. Method performance parameters included overall recovery, intermediate precision, and measurement uncertainty, which were evaluated according to a nested experimental design. Approximately, 95% of the pesticides studied had recoveries between 81 and 110%, intermediate precision ≤20%, and measurement uncertainty ≤40%. From a pilot study of 44 incurred tea samples, pesticide residues were examined for their ability to transfer from dried tea leaves to brewed tea. Each sample, both tea leaves and brewed tea, was analyzed in duplicate. Pesticides were found to have different transfer rates (%). For example, imidacloprid, methomyl, and carbendazim had transfer rates of 84.9, 83.4, and 92.4%, respectively.

  18. Determining the release of radionuclides from tank waste residual solids. FY2015 report

    Energy Technology Data Exchange (ETDEWEB)

    King, William D. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hobbs, David T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2015-09-11

    Methodology development for pore water leaching studies has been continued to support Savannah River Site High Level Waste tank closure efforts. For FY2015, the primary goal of this testing was the achievement of target pH and Eh values for pore water solutions representative of local groundwater in the presence of grout or grout-representative (CaCO3 or FeS) solids as well as waste surrogate solids representative of residual solids expected to be present in a closed tank. For oxidizing conditions representative of a closed tank after aging, a focus was placed on using solid phases believed to be controlling pH and Eh at equilibrium conditions. For three pore water conditions (shown below), the target pH values were achieved to within 0.5 pH units. Tank 18 residual surrogate solids leaching studies were conducted over an Eh range of approximately 630 mV. Significantly higher Eh values were achieved for the oxidizing conditions (ORII and ORIII) than were previously observed. For the ORII condition, the target Eh value was nearly achieved (within 50 mV). However, Eh values observed for the ORIII condition were approximately 160 mV less positive than the target. Eh values observed for the RRII condition were approximately 370 mV less negative than the target. Achievement of more positive and more negative Eh values is believed to require the addition of non-representative oxidants and reductants, respectively. Plutonium and uranium concentrations measured during Tank 18 residual surrogate solids leaching studies under these conditions (shown below) followed the general trends predicted for plutonium and uranium oxide phases, assuming equilibrium with dissolved oxygen. The highest plutonium and uranium concentrations were observed for the ORIII condition and the lowest concentrations were observed for the RRII condition. Based on these results, it is recommended that these test methodologies be used to

  19. Determination of sugar structures in solution from residual dipolar coupling constants: methodology and application to methyl beta-D-xylopyranoside.

    Science.gov (United States)

    Pham, Tran N; Hinchley, Sarah L; Rankin, David W H; Liptaj, Tibor; Uhrín, Dusan

    2004-10-13

    We have developed methodology for the determination of solution structures of small molecules from residual dipolar coupling constants measured in dilute liquid crystals. The power of the new technique is demonstrated by the determination of the structure of methyl beta-d-xylopyranoside (I) in solution. An oriented sample of I was prepared using a mixture of C(12)E(5) and hexanol in D(2)O. Thirty residual dipolar coupling constants, ranging from -6.44 to 4.99 Hz, were measured using intensity-based J-modulated NMR techniques. These include 15 D(HH), 4 (1)D(CH), and 11 (n)D(CH) coupling constants. The accuracy of the dipolar coupling constants is estimated to be Comparison with the neutron diffraction structure showed larger differences attributable to crystal packing effects. Reducing the degree of order by using dilute liquid crystalline media in combination with precise measurement of small residual dipolar coupling constants, as shown here, is a way of overcoming the limitation of strongly orienting liquid crystals associated with the complexity of (1)H NMR spectra for molecules with more than 12 protons.

  20. Determination of residual moisture in lyophilized protein pharmaceuticals using a rapid and non-invasive method: near infrared spectroscopy.

    Science.gov (United States)

    Lin, Tanya P; Hsu, Chung C

    2002-01-01

    This study examined the application of near-infrared (NIR) spectroscopy to analyze residual moisture in lyophilized protein pharmaceuticals sealed in glass vials. We demonstrated that NIR was able to determine residual moisture in five marketed and clinical products with the same precision as Karl Fischer titration. We further investigated how changes in product configuration and protein formulation affected NIR measurement accuracy using a lyophilized monoclonal antibody rhuMAb E25 containing 1% to 5% residual moisture. The results indicated that the lyophilized cake porosity and dimensions had no effect on NIR measurement when the cake height and diameter exceeded the NIR penetration depth. In addition, changing the buffer and surfactant concentrations in the formulation did not affect moisture determination by NIR. However, doubling or halving the concentration of a disaccharide, which was used as a lyoprotectant, caused significant deviation between the NIR and Karl Fischer data because the NIR absorbance of the disaccharide overlapped with the moisture signal. Furthermore, complete removal of the disaccharide resulted in alteration of the protein NIR spectra, suggesting that NIR may be used to evaluate solid-state protein structure. The disaccharide concentration must be kept constant in this formulation to obtain accurate moisture results by NIR.

  1. Determination of Effective Criteria for location Selection of WPC Plants from agricultural residues in Iran by AHP Technique

    Directory of Open Access Journals (Sweden)

    hasan alizadeh

    2017-02-01

    Full Text Available This study was aimed at determining the effective criteria for location selection of WPC Plants from agricultural residues in Iran. For this purpose, after review and studies papers and books, Six criteria" products and materials, regulations, technical and human, economic, infrastructure and environmental and also 30 sub-criteria were identified. The priority rates of these criteria and sub-criteria were evaluated by AHP technique. The results indicated that among 30 effective sub-criteria in location selection of the WPC plants from agricultural residues, amount of wastes supply (0.087, continuity of wastes supply, cost of wastes supply, amount of sales and export, granted facilities and less Hazards for the environment and forest had the highest priorities, which were rated as 0.071, 0.067, 0.065, 0.064 and 0.062 respectively.

  2. A method to determine residue levels of persistent organochlorine pesticides in human milk from Indonesian women.

    Science.gov (United States)

    Burke, Emma R; Holden, Alexis J; Shaw, Ian C

    2003-01-01

    A method has been developed for the analysis of organochlorine pesticides in human milk using solvent extraction, Florisil solid phase extraction clean-up and analysis by gas chromatography with an electron capture detector. The recovery of analytes from spiked milk samples was in the range 53 +/- 1% to 109 +/- 7% (n = 9). A small number of samples were obtained from women in a rural and an urban area of Indonesia and analysed using the developed method. The results are reported on a milk fat basis. All samples contained detectable residues of p,p'-DDT (urban mean 0.11 +/- 0.18 mgkg(-1) (n = 5), rural mean 0.07 +/- 0.03 mg kg(-1) (n = 5)) and p,p'-DDE (urban mean 0.05 +/- 0.04 m kg(-1) (n = 5), rural mean 0.76 +/- 1.46 mg kg(-1) (n = 5)). Residues of HCB, betaHCH, alpha-endosulfan and dieldrin were also detected in some samples. There was no significant difference (at the 95% confidence level) in levels of pesticides between urban and rural areas. The levels of organochlorine pesticides in milk from Indonesian women were lower than those reported from Indonesian women exposed to DDT through malaria eradication schemes and were similar to levels reported from UK and Japan.

  3. Determination of residual monomers released from soft lining materials with the use of HPLC

    International Nuclear Information System (INIS)

    Sofou, A.; Tsoupi, I.; Karayannia, M.

    2007-01-01

    A study was carried out to examine the post polymerized leachability of three non phthalic and four phthalic residual monomers, from twelve commercially available soft lining materials, using HPLC. Specimens of equal: dimensions were constructed from each brand of material following a standardized procedure and were stored in three different conditions of storage i.e. distilled water, artificial saliva and a binary mixture of ethanol-water with the resulting liquids providing samples for analysis in the HPLC apparatus. Three different experiments were performed for each brand of material and each condition of storage, in order to examine the parameters time and temperature. The results obtained from this study suggest that a wide spectrum of residues is diffusing out of the twelve examined soft lining materials. The non phthalic compounds were leaching at high concentrations while all the phthalates examined exhibited different degrees of elusion commensurate with the storage condition, brand of material and type of experiment. The main non phthalic component extracted from all the materials was methyl methacrylate, while the mainly extracted phthalic compound was different from each material. The level of elusion seems to be increasing dependent on time, medium of storage and temperature as well. (author)

  4. Determination of Residual Monomers Released from Soft Lining Materials with the use of HPLC

    Directory of Open Access Journals (Sweden)

    Afrodite Sofou

    2007-12-01

    Full Text Available A study was carried out to examine the post polymerized leachability of three non phthalic and four phthalic residual monomers, from twelve commercially available soft lining materials, using HPLC. Specimens of equal dimensions were constructed from each brand of material following a standardized procedure and were stored in three different conditions of storage i.e. distilled water, artificial saliva and a binary mixture of ethanol-water, with the resulting liquids providing samples for analysis in the HPLC apparatus. Three different experiments were performed for each brand of material and each condition of storage, in order to examine the parameters time and temperature. The results obtained from this study suggest that a wide spectrum of residues is diffusing out of the twelve examined soft lining materials. The non phthalic compounds were leaching at high concentrations while all the phthalates examined exhibited different degrees of elusion commensurate with the storage condition, brand of material and type of experiment. The main non phthalic component extracted from all the materials was methyl methacrylate, while the mainly extracted phthalic compound was different from each material. The level of elusion seems to be increasing dependent on time, medium of storage, and temperature as well.

  5. Multi-residue fluorescent microspheres immunochromatographic assay for simultaneous determination of macrolides in raw milk.

    Science.gov (United States)

    Li, Xiangmei; Shen, Jianzhong; Wang, Qi; Gao, Shuxia; Pei, Xingyao; Jiang, Haiyang; Wen, Kai

    2015-12-01

    A rapid, reliable, sensitive, and quantitative multi-residue fluorescent microspheres immunochromatographic assay (FMCA) was developed for simultaneous detection of four macrolides in raw milk. The IC50 value of the optimized FMCA was 1.36, 1.22, 1.01, and 1.39 ng/mL for erythromycin (ERY), spiramycin (SPI), tilmicosin (TIM), and tylosin (TYL), respectively. The limits of detection (LODs) for the four macrolides was 0.13 ng/mL. The recoveries of ERY, SPI, TIM, and TYL from spiked raw milk ranged from 91.8-109.2, 89.6-114.4, 84.8-111.6, and 85.8-115.2%, respectively, with coefficients of variation (CVs) of 5.4-11.3, 7.9-15.7, 6.2-13.7, and 3.2-14.9%, respectively. The whole testing process was completed within 20 min. The antibody-mixed labeled method was successfully applied to the FMCA, which greatly simplified the operation steps and saved a lot of time. Compared with the immunogold chromatographic assay (IGCA), the FMCA is more sensitive and stable and has less antibody consumption. A parallel analysis in blind raw milk samples was conducted by liquid chromatography-tandem mass spectrometry (LC-MS/MS); the results showed good correlation (r(2) = 0.99) between the two methods. Therefore, the developed multi-residue FMCA is reliable and can be easily applied to other antibiotics or other contaminants.

  6. [Comparison of pretreatment methods for the simultaneous determination of diclazuril and toltrazuril residues in chicken tissues].

    Science.gov (United States)

    Shi, Zuhao; Ge, Qinglian; Lu, Junxian; Liu, Xuexian; Gong, Jiansen; Zhu, Liangqiang; Qi, Kezong; Chen, Dingding; Peng, Kaisong

    2009-05-01

    The effects of four pretreatment methods (acetonitrile extraction-evaporation concentration, acetonitrile extraction-solid phase extraction (SPE), matrix solid-phase dispersion (MSPD) extraction and MSPD-SPE) for the simultaneous analysis of diclazuril and toltrazuril residues in chicken tissues were compared. The average recovery of 70% for the former three methods as achieved. In comparison with other methods, the MSPD method saved more than 60% in time and solvent. So, MSPD as the sample pretreatment method, an MSPD-high performance liquid chromatography with ultraviolet detection (MSPD-HPLC/UV) method was established for the analysis. Under the optimal chromatographic conditions, the linear range was between 50 and 1,000 microg/kg. At the added levels of 50, 500, 1,000 ng/g, the recoveries of diclazuril and toltrazuril in chicken tissues ranged from 71.13% - 84.02% with the relative standard deviations (RSD) in the range of 3.76% - 12.11%, and the RSDs of intra- and interday analyses ranged from 3.70% - 6.77%. The detection limits of diclazuril and toltrazuril were less than 10 microg/kg. The quantitative limits of diclazuril and toltrazuril were less than 20 microg/kg. The method meet the requirements of the residue analysis on accuracy and precision.

  7. Supervised multivariate analysis of sequence groups to identify specificity determining residues

    Directory of Open Access Journals (Sweden)

    Higgins Desmond G

    2007-04-01

    Full Text Available Abstract Background Proteins that evolve from a common ancestor can change functionality over time, and it is important to be able identify residues that cause this change. In this paper we show how a supervised multivariate statistical method, Between Group Analysis (BGA, can be used to identify these residues from families of proteins with different substrate specifities using multiple sequence alignments. Results We demonstrate the usefulness of this method on three different test cases. Two of these test cases, the Lactate/Malate dehydrogenase family and Nucleotidyl Cyclases, consist of two functional groups. The other family, Serine Proteases consists of three groups. BGA was used to analyse and visualise these three families using two different encoding schemes for the amino acids. Conclusion This overall combination of methods in this paper is powerful and flexible while being computationally very fast and simple. BGA is especially useful because it can be used to analyse any number of functional classes. In the examples we used in this paper, we have only used 2 or 3 classes for demonstration purposes but any number can be used and visualised.

  8. Molecular-Level Transformations of Lignin During Photo-Oxidation and Biodegradation

    Science.gov (United States)

    Feng, X.; Hills, K.; Simpson, A. J.; Simpson, M. J.

    2009-05-01

    As the second most abundant component of terrestrial plant residues, lignin plays a key role in regulating plant litter decomposition, humic substance formation, and dissolved organic matter (OM) production from terrestrial sources. Biodegradation is the primary decomposition process of lignin on land. However, photo- oxidation of lignin-derived compounds has been reported in aquatic systems and is considered to play a vital role in arid and semiarid regions. With increasing ultraviolet (UV) radiation due to ozone depletion, it is important to understand the biogeochemical fate of lignin exposed to photo-oxidation in terrestrial environments. This study examines and compares the transformation of lignin in a three-month laboratory simulation of biodegradation and photo-oxidation using molecular-level techniques. Lignin-derived monomers extracted by copper oxidation were analyzed by gas chromatography/mass spectrometry (GC/MS) from the water-soluble and insoluble OM of 13C-labeled corn leaves. Biodegradation increased the solubility of lignin monomers in comparison to the control samples, and the acid-to-aldehyde (Ad/Al) ratios increased in both the water-soluble and insoluble OM, indicating a higher degree of side-chain lignin oxidation. Photo-oxidation did not produce a significant change on the solubility or Ad/Al ratios of lignin from corn leaves. However, the ratios of trans-to-cis isomers of both cinnamyl units (p-coumaric acid and ferulic acid) increased with photo-oxidation and decreased with biodegradation in the insoluble OM. We also investigated the role of photo-oxidation in lignin transformation in soils cropped with 13C-labeled corn. Interestingly, the organic carbon content increased significantly with time in the water-soluble OM from soil/corn residues under UV radiation. An increase in the concentration of lignin monomers and dimers and the Ad/Al ratios was also observed with photo-oxidation. Iso-branched fatty acids of microbial origin remained in

  9. High-value utilization of lignin to synthesize Ag nanoparticles with detection capacity for Hg²⁺.

    Science.gov (United States)

    Shen, Zuguang; Luo, Yuqiong; Wang, Qun; Wang, Xiaoying; Sun, Runcang

    2014-09-24

    This study reports the rapid preparation of silver nanoparticles (AgNPs) from Tollens' reagent under microwave irradiation. In the synthesis, lignin with reducing groups and spatial three-dimensional structure was used as reducing and stabilizing agents without other chemical reagents, and the effects of the ratio of lignin to Ag(+), reaction temperature, and heating time on the synthesis of AgNPs were investigated. The obtained AgNPs were further characterized by UV-vis, Malvern particle size, TEM, XRD, and XPS analyses. The structural changes of lignin before and after reaction were also studied by FT-IR, (1)H NMR, (13)C NMR, and GC-MS. The results revealed that the obtained AgNPs were mostly spherical with diameters of around 24 nm. The optimum reaction conditions were a ratio 50 mg of lignin to 0.3 mM of Ag(+), a microwave irradiation temperature of 60 °C, and a heating time of 10 min. Moreover, AgNPs redispersed well in water and ethanol after centrifugation for the removal of lignin. During the formation of AgNPs, lignin was oxidized, and the side chains of lignin were partly disrupted into small molecules, such as hydrocarbon and alcohol. The resultant lignin-AgNPs showed highly selective sensing detection for Hg(2+), and the color of the lignin-AgNP solution containing Hg(2+) decreased gradually with increasing amounts of Hg(2+) within seconds, but the other 19 metal ions had little effect on the color and surface plasmon absorption band of the lignin-AgNPs. Also, there was a linear relationship between the absorbance and Hg(2+) concentration, with a limit of detection concentration of 23 nM. This study provides not only a new way to take advantage of agricultural and forestry residues, but also a green and rapid method for the synthesis of AgNPs to detect the toxic ion Hg(2+) selectively and sensitively.

  10. Determination of Florfenicol Residues in the Muscle and Liver of Cultured Rainbow Trout in Iran by ELISA

    Directory of Open Access Journals (Sweden)

    Firooz Fadaeifard

    2015-09-01

    Full Text Available Florfenicol is a broad-spectrum antibiotic, widely used in veterinary medicine. The aim of this study was to determine florfenicol residues in the muscle and liver of cultured rainbow trout in Iran by ELISA. The samples were collected from three areas (Kiar, Ardal, and Koohrang, considered as areas with high production of trout in the western part of Iran. Sampling was completed during the spring and summer of 2011. All of the samples were categorized into three weight groups (below 50g, 50 to150g and over 150g and five individuals were randomly selected from fish belonged to each weigh group, and then collected samples sent for determination of antibiotic residues. The highest and the lowest antibiotic residues were 31.42±53.52 ng g-1 (>150 g fish and 10.35±2.33 ng g-1 (<50 g fish for liver samples and 48.84±50.36 ng g-1 (50-150 g fish and 18.20±15.41 ng g-1 (> 150 g fish for muscle samples, respectively. In different areas, the highest antibiotic levels were found in Koohrang and Ardal with mean of 37.00±63.61 and 15.33±10.45 ng g-1 for liver samples and 40.74±40.80 and 28.24±45.91ng g-1 for muscle samples. The results indicated that florfenicol residues are lower than the maximum permissible level has been announced by the European Union.

  11. Changes of Lignin Molecular Structures in a Modification of Kraft Lignin Using Acid Catalyst.

    Science.gov (United States)

    Kim, Sunghoon; Oh, Seungtaek; Lee, Jungmin; Roh, Hyun-Gyoo; Park, Jongshin

    2016-08-05

    The purpose of this study is to modify lignin for better blending with general purpose synthetic polymers. The possible advantages by using this modification would be cost reduction, better physical properties, and biodegradability. In this study, butyrolactone-modified lignin (BLL) and tetrahydrofuran-modified lignin (THFL) were used for aliphatic chain modification of lignin using an acid-catalyzed esterification method in order to mimic the relation of lignin-carbohydrate-complex (LCC) and cellulose. The results of several analyses indicated that lignin was well modified. It was confirmed that the lignin was modified as expected and the reaction sites of the modification, as well as the reaction behaviors, were varied by the reagent types. The result of X-ray diffraction analysis (XRD) analysis indicated that modified lignin/polymer blends increased the crystallinity due to their good compatibility. It can be confirmed that the type of alkyl chain and the miscibility gap between the alkyl chain-matrix affected the mechanical properties enormously in the fungi-degradable environment. From this study, a new method of lignin modification is proposed, and it is found that modified lignin retains the property of the substituted aliphatic chain well. This method could be a proper lignin modification method.

  12. Changes of Lignin Molecular Structures in a Modification of Kraft Lignin Using Acid Catalyst

    Directory of Open Access Journals (Sweden)

    Sunghoon Kim

    2016-08-01

    Full Text Available The purpose of this study is to modify lignin for better blending with general purpose synthetic polymers. The possible advantages by using this modification would be cost reduction, better physical properties, and biodegradability. In this study, butyrolactone-modified lignin (BLL and tetrahydrofuran-modified lignin (THFL were used for aliphatic chain modification of lignin using an acid-catalyzed esterification method in order to mimic the relation of lignin-carbohydrate-complex (LCC and cellulose. The results of several analyses indicated that lignin was well modified. It was confirmed that the lignin was modified as expected and the reaction sites of the modification, as well as the reaction behaviors, were varied by the reagent types. The result of X-ray diffraction analysis (XRD analysis indicated that modified lignin/polymer blends increased the crystallinity due to their good compatibility. It can be confirmed that the type of alkyl chain and the miscibility gap between the alkyl chain-matrix affected the mechanical properties enormously in the fungi-degradable environment. From this study, a new method of lignin modification is proposed, and it is found that modified lignin retains the property of the substituted aliphatic chain well. This method could be a proper lignin modification method.

  13. Studies of the molecular interaction between cellulose and lignin as a model for the hierarchical structure of wood

    Science.gov (United States)

    Wolfgang G. Glasser; Timothy G. Rials; Stephen S. Kelly; Vipul. Dave

    1998-01-01

    Wood and dietary fiber products all belong to a class of biomolecular composites that are rich in cellulose and lignin. The interaction between cellulose and lignin determines such properties as mechanical strength (wood); creep, durability, and aging; cellulose purity (pulp); and digestibility (nutrients). The understanding of the interaction between cellulose and...

  14. Development of Lignin-Based Polyurethane Thermoplastics

    Energy Technology Data Exchange (ETDEWEB)

    Saito, Tomonori [ORNL; Perkins, Joshua H [ORNL; Jackson, Daniel C [ORNL; Trammell, Neil E [ORNL; Hunt, Marcus A [ORNL; Naskar, Amit K [ORNL

    2013-01-01

    In our continued effort to develop value-added thermoplastics from lignin, here we report utilizing a tailored feedstock to synthesize mechanically robust thermoplastic polyurethanes at very high lignin contents (75 65 wt %). The molecular weight and glass transition temperature (Tg) of lignin were altered through cross-linking with formaldehyde. The cross-linked lignin was coupled with diisocyanate-based telechelic polybutadiene as a network-forming soft segment. The appearance of two Tg s, around 35 and 154 C, for the polyurethanes indicates the existence of two-phase morphology, a characteristic of thermoplastic copolymers. A calculated Flory-Huggins interaction parameter of 7.71 also suggests phase immiscibility in the synthesized lignin polyurethanes. An increase in lignin loading increased the modulus, and an increase in crosslink-density increased the modulus in the rubbery plateau region of the thermoplastic. This path for synthesis of novel lignin-based polyurethane thermoplastics provides a design tool for high performance lignin-based biopolymers.

  15. Environmental economics of lignin derived transport fuels

    NARCIS (Netherlands)

    Obydenkova, Svetlana V.; Kouris, Panos D.; Hensen, Emiel J. M.; Heeres, Hero J.; Boot, Michael D.

    2017-01-01

    This paper explores the environmental and economic aspects of fast pyrolytic conversion of lignin, obtained from 2G ethanol plants, to transport fuels for both the marine and automotive markets. Various scenarios are explored, pertaining to aggregation of lignin from several sites, alternative

  16. Isolation and Physicochemical Characterization of Lignin from ...

    African Journals Online (AJOL)

    The isolated lignins were characterized by some physico-chemical parameters and spectroscopy methods like Futran Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy (SEM). Lignin from Chromolaena odorata was found to be more pure than the one from Tithonia diversifolia as evident from the ...

  17. Bacterial enzymes involved in lignin degradation

    NARCIS (Netherlands)

    de Gonzalo, Gonzalo; Colpa, Dana I; Habib, Mohamed H M; Fraaije, Marco W

    2016-01-01

    Lignin forms a large part of plant biomass. It is a highly heterogeneous polymer of 4-hydroxyphenylpropanoid units and is embedded within polysaccharide polymers forming lignocellulose. Lignin provides strength and rigidity to plants and is rather resilient towards degradation. To improve the

  18. Structural elucidation of inhomogeneous lignins from bamboo.

    Science.gov (United States)

    Wen, Jia-Long; Sun, Shao-Long; Xue, Bai-Liang; Sun, Run-Cang

    2015-01-01

    A better understanding of the inhomogeneous molecular structure of lignin from bamboo is a prerequisite for promoting the "biorefinery" technologies of the bamboo feedstock. A mild and successive method for fractionating native lignin from bamboo species was proposed in the present study. The molecular structure and structural inhomogeneity of the isolated lignin polymers were comprehensively investigated by elemental analysis, carbohydrate analysis, state-of-the-art NMR and analytical pyrolysis techniques (quantitative (13)C NMR, (13)C-DEPT 135 NMR, 2D-HSQC NMR, (31)P NMR, and pyrolysis-GC-MS). The results showed that the proposed method is effective for extracting lignin from bamboo. NMR results showed that syringyl (S) was the predominant unit in bamboo lignin over guaiacyl (G) and p-hydroxyphenyl (H) units. In addition, the lignin was associated with p-coumarates and ferulates via ester and ether bonds, respectively. Moreover, various substructures, such as β-O-4, β-β, β-5, β-1, and α,β-diaryl ether linkages, were identified and quantified by NMR techniques. Based on the results obtained, a proposed schematic diagram of structural heterogeneity of the lignin polymers extracted from the bamboo is presented. In short, well-defined inhomogeneous structures of native lignin from bamboo will facilitate further applications of bamboo in current biorefineries. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Lignin biomass conversion into chemicals and fuels

    DEFF Research Database (Denmark)

    Melián Rodríguez, Mayra

    Second-generation biomass or lignocellulosic biomass, which is mainly composed of cellulose, hemicellulose and lignin, is a very important and promising feedstock for the renewable production of fuels and chemicals of the future. Lignin is the second most abundant natural polymer, representing 30...

  20. Determining the Release of Radionuclides from Tank 18F Waste Residual Solids: FY2016 Report

    Energy Technology Data Exchange (ETDEWEB)

    King, William D. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Hobbs, David T. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-08-12

    Pore water leaching studies were conducted on actual Savannah River Site (SRS) Tank 18F residual waste solids to support Liquid Waste tank closure efforts. A test methodology was developed during previous simulant testing to produce slurries of tank residual solids and grout-representative solids in grout pore water solutions (based on SRS groundwater compositions) with pH and Eh values expected during the aging of the closed waste tank. The target conditions are provided below where the initial pore water has a reducing potential and a relatively high pH (Reducing Region II). The pore water is expected to become increasingly oxidizing with time (Oxidizing Region II) and during the latter stages of aging (Oxidizing Region III) the pH is expected to decrease. For the reducing case, tests were conducted with both unwashed and washed Tank 18F residual solids. For the oxidizing cases (Oxidizing Regions II and III), all samples were washed with simulated grout pore water solutions prior to testing, since it is expected that these conditions will occur after considerable pore water solution has passed through the system. For the reducing case, separate tests were conducted with representative ground grout solids and with calcium carbonate reagent, which is the grout phase believed to be controlling the pH. Ferrous sulfide (FeS) solids were also added to the reducing samples to lower the slurry Eh value. Calcium carbonate solids were used as the grout-representative solid phase for each of the oxidizing cases. Air purge-gas with and without CO2 removed was transferred through the oxidizing test samples and nitrogen purge-gas was transferred through the reducing test samples during leach testing. The target pH values were achieved to within 0.5 pH units for all samples. Leaching studies were conducted over an Eh range of approximately 0.7 V. However, the highest and lowest Eh values achieved of ~+0.5 V and ~-0.2 V were

  1. Enzymatic conversion of lignin into renewable chemicals.

    Science.gov (United States)

    Bugg, Timothy D H; Rahmanpour, Rahman

    2015-12-01

    The aromatic heteropolymer lignin is a major component of plant cell walls, and is produced industrially from paper/pulp manufacture and cellulosic bioethanol production. Conversion of lignin into renewable chemicals is a major unsolved problem in the development of a biomass-based biorefinery. The review describes recent developments in the understanding of bacterial enzymes for lignin breakdown, such as DyP peroxidases, bacterial laccases, and beta-etherase enzymes. The use of pathway engineering methods to construct genetically modified microbes to convert lignin to renewable chemicals (e.g. vanillin, adipic acid) via fermentation is discussed, and the search for novel applications for lignin (e.g. carbon fibre). Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Photocatalytic Based Degradation Processes of Lignin Derivatives

    Directory of Open Access Journals (Sweden)

    Colin Awungacha Lekelefac

    2015-01-01

    Full Text Available Photocatalysis, belonging to the advanced oxidation processes (AOPs, is a potential new transformation technology for lignin derivatives to value added products (e.g., phenol, benzene, toluene, and xylene. Moreover, lignin represents the only viable source to produce aromatic compounds as fossil fuel alternative. This review covers recent advancement made in the photochemical transformation of industrial lignins. It starts with the photochemical reaction principle followed by results obtained by varying process parameters. In this context, influences of photocatalysts, metal ions, additives, lignin concentration, and illumination intensity and the influence of pH are presented and discussed. Furthermore, an overview is given on several used process analytical methods describing the results obtained from the degradation of lignin derivatives. Finally, a promising concept by coupling photocatalysis with a consecutive biocatalytic process was briefly reviewed.

  3. Lignin Biodegradation with Laccase-Mediator Systems

    International Nuclear Information System (INIS)

    Christopher, Lew Paul; Yao, Bin; Ji, Yun

    2014-01-01

    Lignin has a significant and largely unrealized potential as a source for the sustainable production of fuels and bulk high-value chemicals. It can replace fossil-based oil as a renewable feedstock that would bring about socio-economic and environmental benefits in our transition to a biobased economy. The efficient utilization of lignin however requires its depolymerization to low-molecular weight phenolics and aromatics that can then serve as the building blocks for chemical syntheses of high-value products. The ability of laccase to attack and degrade lignin in conjunction with laccase mediators is currently viewed as one of the potential “breakthrough” applications for lignin valorization. Here, we review the recent progress in lignin biodegradation with laccase-mediator systems, and research needs that need to be addressed in this field.

  4. Determination of drug residues by CLAR-MS/MS in animal tissues

    International Nuclear Information System (INIS)

    Brenes Jimenez, Jose Eduardo

    2009-01-01

    Produced food of animal origin, present the possibility of occurrence of any contact with substances that have negative effects on the health of people who consume them. The use of drugs in veterinary medicine is one of the possible sources of such waste; so, the conditions for the analysis of some classes of antibiotics in animal tissues are based on the study. Costa Rica and the countries that are export destination, have regulation and programs for control before to be distributed in local markets, or post if it is received any complaint of pollution. The high resolution liquid chromatography coupled to mass spectrometers (CLAR-MS/MS) allows the analysis of analytes monitored, according to the specifications required by the legislation. The cases of two laboratories in Costa Rica are presented as the only ones who have the ability to perform the analysis of drug residues CLAR-MS/MS. (author) [es

  5. The determination of residual perchlorate after the controlled ignition of selected fireworks compositions

    Energy Technology Data Exchange (ETDEWEB)

    Armstrong, K.; Ridley, W.; Guilbeault, R.; Duff, B.

    2008-04-15

    This study investigated perchlorate releases into the atmosphere caused by fireworks displays. Five perchlorate-based compositions were ignited in a sealed stainless steel vessel. The interior of the vessel and the exhaust filters were then washed with hot de-ionized water. Ion chromatography was then used to analyzed the water solutions. Amounts of perchlorate ion measured in the solution were then used to calculate the percentage of residual perchlorate based on the original mass of perchlorate contained within the samples. The study showed that 99.98 to 99.999 per cent of the initial mass of perchlorate in the samples was consumed during ignition. It was concluded that the incomplete combustion of fireworks caused by defective article construction will cause higher amounts of perchlorate releases into the environment. Stricter quality controls are needed to reduce the environmental impacts of fireworks. 14 refs., 4 tabs., 3 figs.

  6. Neutron diffraction measurements for the determination of residual stresses in MMC tensile and fatigue specimens

    DEFF Research Database (Denmark)

    Fiori, F.; Girardin, E.; Giuliani, A.

    2000-01-01

    The experiments here described have been carried out in the framework of a more general research, aiming to develop a set of complementary models to predict the in-service performances of particle reinforced MMC automotive and aeronautical components. As MMCs are highly heterogeneous materials......, residual stresses are present in both the matrix and the particles microstructure, prior to any macroscopic loading. They vary with the temperature and with the type and level of loading imposed to the material, having a strong influence on the mechanical behaviour of MMCs. Neutron diffraction measurements...... and thermal mismatch microstresses. The results show that, in general, the main contribution to the stress state of both matrix and reinforcement is given by the thermal microstresses, already existing due to heat treatment prior to mechanical tests. (C) 2000 Elsevier Science B.V. All rights reserved....

  7. Comparison of Methods for Bifenthrin Residues Determination in Fermented Wheat Samples

    Directory of Open Access Journals (Sweden)

    Tijana Đorđević

    2012-01-01

    Full Text Available Efficiency of three different sample preparation methods for GC/MS determinationof bifenthrin residues in wheat (Triticum spelta samples fermented by Lactobacillusplantarum was tested. The first method was based on a methanol:acetone=1:1 extractionfolowed by a purification on columns containing mixture of aluminium oxide and activatedcharcoal slurry-packed and eluted with dichlormethane, the second was based onmethanol:acetone=1:1 extraction folowed by the purification on florisil column and elutionby ethil acetate:acetone=4:1, while the third tested method was based on a combinationof the first two mentioned methods, thus methanol:acetone=1:1 extraction and clean-upthrought columns filled with a mixture of aluminum oxide and activated charcoal slurrypackedand eluted with ethil acetate:acetone=4:1. The second method was the most effectivefor obtaining satisfactory recoveries for bifenthrin in a range of 79-83% for four fortificationlevels, with good reproducibility i.e. RSD% in a range of 2.2-7.4%. The chosen methodwas further optimized by assessing the optimum volume of elution solvent used duringthe clean-up procedures. The highest recovery of 82.1% was obtained after elution with25 ml of solvent. Overall, two-step extraction with 25 ml of methanol:acetone=1:1 solventmix for 30 min, followed by clean-up procedure through a glass column with florisil coupledwith elution with 25 ml of ethyl acetate: acetone=4:1, allows simple, efficient and reliableGC/MS detection of bifenthrin residues from wheat grain fermented by L. plantarum.

  8. Ouabain affinity determining residues lie close to the Na/K pump ion pathway.

    Science.gov (United States)

    Artigas, Pablo; Gadsby, David C

    2006-08-15

    The Na/K pump establishes essential ion concentration gradients across animal cell membranes. Cardiotonic steroids, such as ouabain, are specific inhibitors of the Na/K pump. We exploited the marine toxin, palytoxin, to probe both the ion translocation pathway through the Na/K pump and the site of its interaction with ouabain. Palytoxin uncouples the pump's gates, which normally open strictly alternately, thus allowing both gates to sometimes be open, so transforming the pump into an ion channel. Palytoxin therefore permits electrophysiological analysis of even a single Na/K pump. We used outside-out patch recording of Xenopus alpha1beta3 Na/K pumps, which were made ouabain-resistant by point mutation, after expressing them in Xenopus oocytes. Endogenous, ouabain-sensitive, Xenopus alpha1beta3 Na/K pumps were silenced by continuous exposure to ouabain. We found that side-chain charge of two residues at either end of the alpha subunit's first extracellular loop, known to make a major contribution to ouabain affinity, strongly influenced conductance of single palytoxin-bound pump-channels by an electrostatic mechanism. The effects were mimicked by modification of cysteines introduced at those two positions with variously charged methanethiosulfonate reagents. The consequences of these modifications demonstrate that both residues lie in a wide vestibule near the mouth of the pump's ion pathway. Bound ouabain protects the site with the strongest influence on conductance from methanethiosulfonate modification, while leaving the site with the weaker influence unprotected. The results suggest a method for mapping the footprint of bound cardiotonic steroid on the extracellular surface of the Na/K pump.

  9. Opportunities and challenges in biological lignin valorization

    Energy Technology Data Exchange (ETDEWEB)

    Beckham, Gregg T.; Johnson, Christopher W.; Karp, Eric M.; Salvachúa, Davinia; Vardon, Derek R.

    2016-12-01

    Lignin is a primary component of lignocellulosic biomass that is an underutilized feedstock in the growing biofuels industry. Despite the fact that lignin depolymerization has long been studied, the intrinsic heterogeneity of lignin typically leads to heterogeneous streams of aromatic compounds, which in turn present significant technical challenges when attempting to produce lignin-derived chemicals where purity is often a concern. In Nature, microorganisms often encounter this same problem during biomass turnover wherein powerful oxidative enzymes produce heterogeneous slates of aromatics compounds. Some microbes have evolved metabolic pathways to convert these aromatic species via ‘upper pathways’ into central intermediates, which can then be funneled through ‘lower pathways’ into central carbon metabolism in a process we dubbed ‘biological funneling’. This funneling approach offers a direct, biological solution to overcome heterogeneity problems in lignin valorization for the modern biorefinery. Coupled to targeted separations and downstream chemical catalysis, this concept offers the ability to produce a wide range of molecules from lignin. This perspective describes research opportunities and challenges ahead for this new field of research, which holds significant promise towards a biorefinery concept wherein polysaccharides and lignin are treated as equally valuable feedstocks. In particular, we discuss tailoring the lignin substrate for microbial utilization, host selection for biological funneling, ligninolytic enzyme–microbe synergy, metabolic engineering, expanding substrate specificity for biological funneling, and process integration, each of which presents key challenges. Ultimately, for biological solutions to lignin valorization to be viable, multiple questions in each of these areas will need to be addressed, making biological lignin valorization a multidisciplinary, co-design problem.

  10. UPLC-MS/MS determination of ractopamine residues in retinal tissue of treated food-producing pigs.

    Science.gov (United States)

    Vulić, Ana; Pleadin, Jelka; Perši, Nina; Milić, Dinka; Radeck, Wolfgang

    2012-05-01

    Ractopamine is a β(2)-adrenergic agonist, which reduces fat deposition and promotes muscle growth in animals for meat production. In the European Union countries, systematic monitoring and control of this contaminant residue is regularly performed by use of validated analytical methods of detection in different biological materials. The aim of the present study was to assess persistence of ractopamine in retina as a pigmented tissue by determination of its residues using UPLC-MS/MS as a quantitative confirmatory method after pig exposure to a ractopamine dose of 0.51 mg/kg b.w. Experimental group (n=9) of pigs were orally administered ractopamine for 28 days and then randomly sacrificed (n=3) on days 1, 3 and 8 of treatment discontinuation, whereas control animals (n=3) were left untreated. Study results showed mean ractopamine residue concentrations of 110.36 μg/kg, 67.11 μg/kg and 89.93 μg/kg on days 1, 3 and 8 after withdrawal, respectively, indicating high accumulation of ractopamine in retina despite a low dose applied. These data pointed to high affinity of ractopamine for binding to the pigmented segment of the eye, thus supporting the use of pigmented tissues as matrices in the regulatory monitoring of this β(2)-adrenergic agonist. Copyright © 2012 Elsevier B.V. All rights reserved.

  11. Rapid ion-pair liquid chromatographic method for the determination of fenbendazole marker residue in fermented dairy products.

    Science.gov (United States)

    Vousdouka, Venetia I; Papapanagiotou, Elias P; Angelidis, Apostolos S; Fletouris, Dimitrios J

    2017-04-15

    A simple, rapid and sensitive liquid chromatographic method that allows for the quantitative determination of fenbendazole residues in fermented dairy products is described. Samples were extracted with a mixture of acetonitrile-phosphoric acid and the extracts were defatted with hexane to be further partitioned into ethyl acetate. The organic layer was evaporated to dryness and the residue was reconstituted in mobile phase. Separation of fenbendazole and its sulphoxide, sulphone, and p-hydroxylated metabolites was carried out isocratically with a mobile phase containing both positively and negatively charged pairing ions. Overall recoveries ranged from 79.8 to 88.8%, while precision data, based on within and between days variations, suggested an overall relative standard deviation of 6.3-11.0%. The detection and quantification limits were lower than 9 and 21μg/kg, respectively. The method has been successfully applied to quantitate fenbendazole residues in Feta cheese and yoghurt made from spiked and incurred ovine milk. Copyright © 2016 Elsevier Ltd. All rights reserved.

  12. A Small Number of Residues Can Determine if Linker Histones Are Bound On or Off Dyad in the Chromatosome.

    Science.gov (United States)

    Zhou, Bing-Rui; Feng, Hanqiao; Ghirlando, Rodolfo; Li, Shipeng; Schwieters, Charles D; Bai, Yawen

    2016-10-09

    Linker histones bind to the nucleosome and regulate the structure and function of chromatin. We have previously shown that the globular domains of chicken H5 and Drosophila H1 linker histones bind to the nucleosome with on- or off-dyad modes, respectively. To explore the determinant for the distinct binding modes, we investigated the binding of a mutant globular domain of H5 to the nucleosome. This mutant, termed GH5_pMut, includes substitutions of five globular domain residues of H5 with the corresponding residues in the globular domain of Drosophila H1. The residues at these five positions play important roles in nucleosome binding by either H5 or Drosophila H1. NMR and spin-labeling experiments showed that GH5_pMut bound to the nucleosome off the dyad. We further found that the nucleosome array condensed by either the GH5_pMut or the globular domain of Drosophila H1 displayed a similar sedimentation coefficient, whereas the same nucleosome array condensed by the wild-type globular domain of H5 showed a much larger sedimentation coefficient. Moreover, NMR and spin-labeling results from the study of the nucleosome in complex with the full-length human linker histone H1.0, whose globular domain shares high sequence conservation with the corresponding globular domain of H5, are consistent with an on-dyad binding mode. Taken together, our results suggest that a small number of residues in the globular domain of a linker histone can control its binding location on the nucleosome and higher-order chromatin structure. Copyright © 2016. Published by Elsevier Ltd.

  13. Determination of temperature and residual laser energy on film fiber-optic thermal converter for diode laser surgery.

    Science.gov (United States)

    Liu, Weichao; Kong, Yaqun; Shi, Xiafei; Dong, Xiaoxi; Wang, Hong; Zhao, Jizhi; Li, Yingxin

    2017-12-01

    The diode laser was utilized in soft tissue incision of oral surgery based on the photothermic effect. The contradiction between the ablation efficiency and the thermal damage has always been in diode laser surgery, due to low absorption of its radiation in the near infrared region by biological tissues. Fiber-optic thermal converters (FOTCs) were used to improve efficiency for diode laser surgery. The purpose of this study was to determine the photothermic effect by the temperature and residual laser energy on film FOTCs. The film FOTC was made by a distal end of optical fiber impacting on paper. The external surface of the converter is covered by a film contained amorphous carbon. The diode laser with 810 nm worked at the different rated power of 1.0 W, 1.5 W, 2.0 W, 3.0 W, 4.0 W, 5.0 W, 6.0 W, 7.0 W, 8.0 W in continuous wave (CW)and pulse mode. The temperature of the distal end of optical fiber was recorded and the power of the residual laser energy from the film FOTC was measured synchronously. The temperature, residual power and the output power were analyzed by linear or exponential regression model and Pearson correlations analysis. The residual power has good linearity versus output power in CW and pulse modes (R 2  = 0.963, P fiber tip both in CW and pulsed mode while limiting the ability of the laser light to interact directly with target tissue. Film FOTCs can concentrate part of laser energy transferred to heat on distal end of optical fiber, which have the feasibility of improving efficiency and reducing thermal damage of deep tissue.

  14. Chemical composition, anatomy, lignin distribution, and cell wall structure of Malaysian plant waste fibers

    OpenAIRE

    Mohd Omar, A. K.; Siti Alwani, M.; Abdul Khalil, H. P. S.

    2006-01-01

    The chemical composition, anatomical characteristics, lignin distribution, and cell wall structure of oil palm frond (OPF), coconut (COIR), pine-apple leaf (PALF), and banana stem (BS) fibers were analyzed. The chemical composition of fiber was analyzed according to TAPPI Methods. Light microscopy (LM) and transmission electron microscopy (TEM) were used to observe and determine the cell wall structure and lignin distribution of various agro-waste fibers. The results revealed differences in a...

  15. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Marguí, Eva, E-mail: eva.margui@udg.edu [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain); Queralt, Ignasi, E-mail: iqueralt@ictja.csic.es [Laboratory of X-ray Analytical Applications, Institute of Earth Sciences “Jaume Almera”, CSIC, Solé Sabarís s/n, 08028 Barcelona (Spain); Hidalgo, Manuela, E-mail: manuela.hidalgo@udg.edu [Department of Chemistry, University of Girona, Campus Montilivi, 17071 Girona (Spain)

    2013-08-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2–4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods. - Highlights: • A TXRF method for PGM catalyst residue determination in API samples is presented. • Analysis can be performed using 10 μL of the internal standardized dissolved API. • The method is rapid, simple and suitable according to the USP requirements.

  16. Flash pyrolysis properties of algae and lignin residue

    DEFF Research Database (Denmark)

    Trinh, Ngoc Trung; Jensen, Peter Arendt; Sørensen, Hanne Risbjerg

    of macroalgae showed a promising result with on yield of 54 wt% dry ash free basis (daf) and 78% energy recovery in the bio-oil. The physiochemical properties of the bio-oils were characterized with respect to higher heating value, molecular mass distribution, viscosity, pH, density and elemental compositions...

  17. Nickel, sulfur and vanadium determination in residues from crude oil distillation by ICPOES after microwave-induced combustion

    International Nuclear Information System (INIS)

    Mello, P.A.; Pereira, J.S.F.; Dressler, V.L.; Flores, E.M.M.

    2009-01-01

    Full text: A microwave-induced combustion method is proposed for digestion of atmospheric and vacuum residues from heavy crude oil for simultaneous Ni, S and V determination by ICPOES. Ammonium nitrate solution (6 M, 50 μl) was used as igniter. Operational parameters were investigated as maximum sample mass, initial O 2 pressure, type and concentration of absorbing solutions (H 2 O, H 2 O 2 , and HNO 3 ) and the necessity of additional reflux steps. Accuracy was better than 98 %. Limits of detection were 0.2, 2 and 0.1 mg kg -1 for Ni, S and V, respectively. (author)

  18. Validation of a method for determination of amoxicillin residues applied to cleaning validation process in penicillins pharmaceutical industry

    OpenAIRE

    Gomes, Maria Luiza Pinheiro Costa; Souza, Scheilla Vitorino Carvalho de

    2010-01-01

    The aim of this work was the single-laboratory validation of a quantitative method for the determination of amoxicillin residues in support of cleaning control and validation. Linearity was demonstrated between 2.5 and 17.5 μg/mL, without matrix effects. Mean recoveries ranged from 84.00 to 103.74% and the relative standard deviation under repetitivity and within-reproducibility conditions were from 0.58 to 4.20% and from 0.79 to 4.39%, respectively. The theoretical limits of detection a...

  19. Nanoscale characterisation by SANS and residual stresses determination by neutron diffraction related to materials and components of technological interest

    Science.gov (United States)

    Rogante, Massimo; Rosta, Laszlo

    2005-06-01

    Neutron techniques, among the other non-destructive diagnostics, are becoming more and more relevant in investigating materials and components of industrial interest. In this paper, Small Angle Neutron Scattering (SANS) for microstructural characterisation-especially related to the nanoscale-and Neutron Diffraction for Residual Stresses (RS) measurements are considered. The basic theoretical aspects and some industrial applications of each technique are described. In particular, RS determination in welding, in extruded specimens and in components for energy industry is reported. SANS measurements concerning materials and components for energy and automotive industry are finally presented.

  20. Residual solvent determination by head space gas chromatography with flame ionization detector in omeprazole API

    Directory of Open Access Journals (Sweden)

    Saurabh Pandey

    2011-06-01

    Full Text Available Residual solvents in pharmaceutical samples are monitored using gas chromatography with head space. Based on good manufacturing practices, measuring residual solvents is mandatory for the release testing of all active pharmaceutical ingredients (API. The analysis of residual organic solvents (methanol, acetone, cyclohexane, dichloromethane, toluene in Omeprazole, an active pharmaceutical ingredient was investigated. Omeprazole is a potent reversible inhibitor of the gastric proton pump H+/K+-ATPase. The Head space gas chromatography (HSGC method described in this investigation utilized a SPB TM-624, Supelco, 30 m long x 0.25 mm internal diameter, 1.4µm-thick column. Since Omeprazole is a thermally labile compound, the selection of the proper injector temperature is critical to the success of the analysis. The injector temperature was set at 170ºC to prevent degradation. The initial oven temperature was set at 40ºC for 12 min and programmed at a rate of 10ºC min-1 to a final temperature of 220ºC for 5 min. Nitrogen was used as a carrier gas. The sample solvent selected was N,N-dimethylacetamide. The method was validated to be specific, linear, precise, sensitive, rugged and showed excellent recovery.Solventes residuais em amostras farmacêuticas são monitoradas utilizando-se cromatografia a gás "headspace". Com base nas boas práticas de fabricação, a medida de solventes residuais é obrigatória para o teste de liberação de todos os ingredientes farmacêuticos (API. Efetuou-se a análise de solventes orgânicos residuais (metanol, acetona, cicloexano, diclorometano, tolueno em omeprazol, ingrediente farmacêutico ativo. O omeprazol é potente inibidor reversível da bomba de prótons H+/K+-ATPase. A cromatografia a gás "headspace" (HSGC descrita nessa pesquisa utilizou um SPB TM-624, Supelco, de 30 m de comprimento x 0,25 mm de diâmetro interno, e coluna de 1,4 µm de espessura. Considerando-se que o omeprazol é termicamente l

  1. Determination Residues of Penicillin G and Cloxacillin in Raw Cow Milk Using Fourier Transform Near Infrared Spectroscopy

    Directory of Open Access Journals (Sweden)

    Michaela Dračková

    2009-01-01

    Full Text Available The objective of this study was to study the use of Fourier transform near infrared spectroscopy (FTNIR combined with the partial least square (PLS method for determining the residues of penicillin and cloxacillin in raw milk. The spectra were measured in the reflectance mode with transflectance cell in the spectral range of 10,000 – 4,000 cm-1 with 100 scans. Calibration models were developed. They were assessed statistically based on correlation coefficients (R and standard errors of calibration (SEC. For penicillin, the following values were established: R = 0.951 and SEC = 0.004. For cloxacillin, they were R = 0.871 and SEC = 0.007. These calibration models were verified later with cross-validation. Better results were obtained in the calibration and validation models that were developed on milk samples coming from one farm. Using FT-NIR, the maximum residue limit (MRL of cloxacillin in milk can be determined. However, standard errors of calibration and validation for penicillin G exceed the fixed MRL. FT-NIR spectroscopy is not a suitable method for accurate determination of these substances in raw milk. Variability in milk composition has a major influence on detection of substances present at very low concentrations.

  2. Genetic Augmentation of Syringyl Lignin in Low-lignin Aspen Trees, Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Chung-Jui Tsai; Mark F. Davis; Vincent L. Chiang

    2004-11-10

    As a polysaccharide-encrusting component, lignin is critical to cell wall integrity and plant growth but also hinders recovery of cellulose fibers during the wood pulping process. To improve pulping efficiency, it is highly desirable to genetically modify lignin content and/or structure in pulpwood species to maximize pulp yields with minimal energy consumption and environmental impact. This project aimed to genetically augment the syringyl-to-guaiacyl lignin ratio in low-lignin transgenic aspen in order to produce trees with reduced lignin content, more reactive lignin structures and increased cellulose content. Transgenic aspen trees with reduced lignin content have already been achieved, prior to the start of this project, by antisense downregulation of a 4-coumarate:coenzyme A ligase gene (Hu et al., 1999 Nature Biotechnol 17: 808- 812). The primary objective of this study was to genetically augment syringyl lignin biosynthesis in these low-lignin trees in order to enhance lignin reactivity during chemical pulping. To accomplish this, both aspen and sweetgum genes encoding coniferaldehyde 5-hydroxylase (Osakabe et al., 1999 PNAS 96: 8955-8960) were targeted for over-expression in wildtype or low-lignin aspen under control of either a constitutive or a xylem-specific promoter. A second objective for this project was to develop reliable and cost-effective methods, such as pyrolysis Molecular Beam Mass Spectrometry and NMR, for rapid evaluation of cell wall chemical components of transgenic wood samples. With these high-throughput techniques, we observed increased syringyl-to-guaiacyl lignin ratios in the transgenic wood samples, regardless of the promoter used or gene origin. Our results confirmed that the coniferaldehyde 5-hydroxylase gene is key to syringyl lignin biosynthesis. The outcomes of this research should be readily applicable to other pulpwood species, and promise to bring direct economic and environmental benefits to the pulp and paper industry.

  3. Determination of flumioxazin residue in food samples through a sensitive fluorescent sensor based on click chemistry.

    Science.gov (United States)

    Lu, Lijun; Yang, Linlin; Cai, Huijian; Zhang, Lan; Lin, Zhenyu; Guo, Longhua; Qiu, Bin; Chen, Guonan

    2014-11-01

    A sensitive and selective fluorescent sensor for flumioxazin was designed based on the formation of strong fluorescence compound (1,2,3-triazole compounds) via the reaction of the alkynyl group in flumioxazin with 3-azido-7-hydroxycoumarin, a weak-fluorescent compound, through the Cu(+)-catalysed azide-alkyne cycloaddition (CuAAC) reaction. The fluorescence increase factor (represented by F/F0) of the system exhibited a good linear relationship with the concentrations of flumioxazin in the range of 0.25-6.0 μg/L with a detection limit of 0.18 μg/L (S/N=3). Also, the proposed fluorescent sensor demonstrated good selectivity for flumioxazin assay even in the presence of high concentration of other pesticides. Based on such high sensitivity and selectivity, the proposed fluorescent sensor has been applied to test the flumioxazin residue in some vegetable and water samples with satisfied results. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. A method for determining allowable residual contamination levels of radionuclide mixtures in soil

    International Nuclear Information System (INIS)

    Napier, B.A.

    1982-05-01

    An important consideration in the disposal of radioactive wastes, and consequently in the preparation of plans for remedial actions at contaminated sites, is the amount of radioactive contamination that may be allowed to remain at any particular waste site. The allowable residual contamination level (ARCL) is dependent on the radiation dose limit imposed, the physical and environmental characteristics of the waste site, and the time at which exposure to the wastes is assumed to occur. The steps in generating an ARCL are generally as follows: (1) develop plausible, credible site-specific exposure scenario; (2) calculate maximum annual radiation doses to an individual for each radionuclide based on the existing physical characteristics of the waste site and the site-specific exposure scenario; (3) calculate the ARCL for the dose limit desired, including all radionuclides present, uncorrected for site cleanup or barrier considerations; and (4) apply any corrections for proposed cleanup activity or addition of barriers to waste migration or uptake to obtain the ARCL applicable to the proposed action. Use of this method allows appropriate application of resources to achieve uniform compliance with a single regulatory standard, i.e., a radiation dose rate limit. Application and modification of the ARCL method requires appropriate models of the environmental transport and fate of radionuclides. Example calculations are given for several specific waste forms and waste site types in order to demonstrate the technique and generate comparisons with other approaches

  5. Application of capillary electrophoresis-mass spectrometry for determining organic food contaminants and residues.

    Science.gov (United States)

    Font, Guillermina; Ruiz, Maria José; Fernández, Monica; Picó, Yolanda

    2008-05-01

    Food contamination continues to be a serious problem around the world. Surveillance of chemical contaminants in foods is important not only for public health but also because of the negative economic impact of contamination. From the analytical perspective, analysis of contaminants in food is an extremely challenging area. There is a wide variety of questions, ranging from the quantification of extremely low levels of individual components to the detailed assessment and evaluation of the analytical technique possibilities. This review considers the applications of CE coupled to MS detection (CE-MS) for the analysis of organic contaminants in food. Analytical information on sample concentration techniques, as well as on the CE separation conditions and recoveries obtained from water and food are provided. Different sections include several fields of application, such as pesticides, drug residues, or toxic formed during food processing in different matrices. A number of tables report a comprehensive listing of CE-MS applications. As a result, this work presents an update overview on the principal application of CE-MS together with a discussion of their main advantages and drawbacks, and an outline of future trends on analysis of organic contaminants.

  6. Determination of structural fluctuations of proteins from structure-based calculations of residual dipolar couplings

    International Nuclear Information System (INIS)

    Montalvao, Rinaldo W.; De Simone, Alfonso; Vendruscolo, Michele

    2012-01-01

    Residual dipolar couplings (RDCs) have the potential of providing detailed information about the conformational fluctuations of proteins. It is very challenging, however, to extract such information because of the complex relationship between RDCs and protein structures. A promising approach to decode this relationship involves structure-based calculations of the alignment tensors of protein conformations. By implementing this strategy to generate structural restraints in molecular dynamics simulations we show that it is possible to extract effectively the information provided by RDCs about the conformational fluctuations in the native states of proteins. The approach that we present can be used in a wide range of alignment media, including Pf1, charged bicelles and gels. The accuracy of the method is demonstrated by the analysis of the Q factors for RDCs not used as restraints in the calculations, which are significantly lower than those corresponding to existing high-resolution structures and structural ensembles, hence showing that we capture effectively the contributions to RDCs from conformational fluctuations.

  7. Determination of activity by gamma spectrometry of radionuclides present in drums of residues generated in nuclear centrals

    International Nuclear Information System (INIS)

    Aguiar, J.C.; Fernandez, J.

    2006-01-01

    The generation of radioactive residuals in nuclear centrals as CNA I (Atucha I Nuclear Central) and CNE (Embalse Nuclear Central) makes that the measurement of those radionuclides has been a previous stage to the waste management. A method used in those nuclear centrals it is the gamma spectrometry with HPGe detectors, previous to the immobilization of the residual in a cemented matrix, with this the contact with the external agents and its possible dispersion to the atmosphere in the short term is avoided. The ARN (Nuclear Regulatory Authority) of Argentina it carries out periodically intercomparisons and evaluations of the measurement and procedures systems used in the nuclear power stations for the correct measurement and determination of activity of radioactive residuals by gamma spectrometry. In this work an independent method of measurement is exposed to the nuclear power stations. To determine the activity of the residuals by gamma spectrometry deposited in drums, it is required of the precise knowledge of the efficiency curve for such geometry and matrix. Due to the RNA doesn't have a pattern of these characteristics, a mathematical model has been used to obtain this efficiency curve. For it, it is necessary to determine previously: 1) the geometric efficiency or solid angle sustained by the source-detector system (drum-detector) applying a mathematical model described in this work. 2) To estimate the auto-attenuation factor that present the photons in the cemented matrix, these calculations are carried out with a simple equation and its are verified with the Micro Shield 6.10 program. The container commonly used by these nuclear power stations its are drums for 220 liters constructed with SAE 1010 steel and with a thickness of 0.127 cm, with an approximate weight 7.73 Kg., internal diameter of 57.1 cm, and height: 87 cm. The results obtained until the moment register a discrepancy from 5 to 10% with relationship to the measurements carried out by the

  8. Preliminary Economics for the Production of Pyrolysis Oil from Lignin in a Cellulosic Ethanol Biorefinery

    Energy Technology Data Exchange (ETDEWEB)

    Jones, Susanne B.; Zhu, Yunhua

    2009-04-01

    Cellulosic ethanol biorefinery economics can be potentially improved by converting by-product lignin into high valued products. Cellulosic biomass is composed mainly of cellulose, hemicellulose and lignin. In a cellulosic ethanol biorefinery, cellulose and hemicellullose are converted to ethanol via fermentation. The raw lignin portion is the partially dewatered stream that is separated from the product ethanol and contains lignin, unconverted feed and other by-products. It can be burned as fuel for the plant or can be diverted into higher-value products. One such higher-valued product is pyrolysis oil, a fuel that can be further upgraded into motor gasoline fuels. While pyrolysis of pure lignin is not a good source of pyrolysis liquids, raw lignin containing unconverted feed and by-products may have potential as a feedstock. This report considers only the production of the pyrolysis oil and does not estimate the cost of upgrading that oil into synthetic crude oil or finished gasoline and diesel. A techno-economic analysis for the production of pyrolysis oil from raw lignin was conducted. comparing two cellulosic ethanol fermentation based biorefineries. The base case is the NREL 2002 cellulosic ethanol design report case where 2000 MTPD of corn stover is fermented to ethanol (NREL 2002). In the base case, lignin is separated from the ethanol product, dewatered, and burned to produce steam and power. The alternate case considered in this report dries the lignin, and then uses fast pyrolysis to generate a bio-oil product. Steam and power are generated in this alternate case by burning some of the corn stover feed, rather than fermenting it. This reduces the annual ethanol production rate from 69 to 54 million gallons/year. Assuming a pyrolysis oil value similar to Btu-adjusted residual oil, the estimated ethanol selling price ranges from $1.40 to $1.48 (2007 $) depending upon the yield of pyrolysis oil. This is considerably above the target minimum ethanol selling

  9. Characterization of electrospun lignin based carbon fibers

    Science.gov (United States)

    Poursorkhabi, Vida; Mohanty, Amar; Misra, Manjusri

    2015-05-01

    The production of lignin fibers has been studied in order to replace the need for petroleum based precursors for carbon fiber production. In addition to its positive environmental effects, it also benefits the economics of the industries which cannot take advantage of carbon fiber properties because of their high price. A large amount of lignin is annually produced as the byproduct of paper and growing cellulosic ethanol industry. Therefore, finding high value applications for this low cost, highly available material is getting more attention. Lignin is a biopolymer making about 15 - 30 % of the plant cell walls and has a high carbon yield upon carbonization. However, its processing is challenging due to its low molecular weight and also variations based on its origin and the method of separation from cellulose. In this study, alkali solutions of organosolv lignin with less than 1 wt/v% of poly (ethylene oxide) and two types of lignin (hardwood and softwood) were electrospun followed by carbonization. Different heating programs for carbonization were tested. The carbonized fibers had a smooth surface with an average diameter of less than 5 µm and the diameter could be controlled by the carbonization process and lignin type. Scanning electron microscopy (SEM) was used to study morphology of the fibers before and after carbonization. Thermal conductivity of a sample with amorphous carbon was 2.31 W/m.K. The electrospun lignin carbon fibers potentially have a large range of application such as in energy storage devices and water or gas purification systems.

  10. Epigallocatechin gallate incorporation into lignin enhances the alkaline delignification and enzymatic saccharification of cell walls

    Directory of Open Access Journals (Sweden)

    Elumalai Sasikumar

    2012-08-01

    Full Text Available Abstract Background Lignin is an integral component of the plant cell wall matrix but impedes the conversion of biomass into biofuels. The plasticity of lignin biosynthesis should permit the inclusion of new compatible phenolic monomers such as flavonoids into cell wall lignins that are consequently less recalcitrant to biomass processing. In the present study, epigallocatechin gallate (EGCG was evaluated as a potential lignin bioengineering target for rendering biomass more amenable to processing for biofuel production. Results In vitro peroxidase-catalyzed polymerization experiments revealed that both gallate and pyrogallyl (B-ring moieties in EGCG underwent radical cross-coupling with monolignols mainly by β–O–4-type cross-coupling, producing benzodioxane units following rearomatization reactions. Biomimetic lignification of maize cell walls with a 3:1 molar ratio of monolignols and EGCG permitted extensive alkaline delignification of cell walls (72 to 92% that far exceeded that for lignified controls (44 to 62%. Alkali-insoluble residues from EGCG-lignified walls yielded up to 34% more glucose and total sugars following enzymatic saccharification than lignified controls. Conclusions It was found that EGCG readily copolymerized with monolignols to become integrally cross-coupled into cell wall lignins, where it greatly enhanced alkaline delignification and subsequent enzymatic saccharification. Improved delignification may be attributed to internal trapping of quinone-methide intermediates to prevent benzyl ether cross-linking of lignin to structural polysaccharides during lignification, and to the cleavage of ester intra-unit linkages within EGCG during pretreatment. Overall, our results suggest that apoplastic deposition of EGCG for incorporation into lignin would be a promising plant genetic engineering target for improving the delignification and saccharification of biomass crops.

  11. Epigallocatechin gallate incorporation into lignin enhances the alkaline delignification and enzymatic saccharification of cell walls.

    Science.gov (United States)

    Elumalai, Sasikumar; Tobimatsu, Yuki; Grabber, John H; Pan, Xuejun; Ralph, John

    2012-08-13

    Lignin is an integral component of the plant cell wall matrix but impedes the conversion of biomass into biofuels. The plasticity of lignin biosynthesis should permit the inclusion of new compatible phenolic monomers such as flavonoids into cell wall lignins that are consequently less recalcitrant to biomass processing. In the present study, epigallocatechin gallate (EGCG) was evaluated as a potential lignin bioengineering target for rendering biomass more amenable to processing for biofuel production. In vitro peroxidase-catalyzed polymerization experiments revealed that both gallate and pyrogallyl (B-ring) moieties in EGCG underwent radical cross-coupling with monolignols mainly by β-O-4-type cross-coupling, producing benzodioxane units following rearomatization reactions. Biomimetic lignification of maize cell walls with a 3:1 molar ratio of monolignols and EGCG permitted extensive alkaline delignification of cell walls (72 to 92%) that far exceeded that for lignified controls (44 to 62%). Alkali-insoluble residues from EGCG-lignified walls yielded up to 34% more glucose and total sugars following enzymatic saccharification than lignified controls. It was found that EGCG readily copolymerized with monolignols to become integrally cross-coupled into cell wall lignins, where it greatly enhanced alkaline delignification and subsequent enzymatic saccharification. Improved delignification may be attributed to internal trapping of quinone-methide intermediates to prevent benzyl ether cross-linking of lignin to structural polysaccharides during lignification, and to the cleavage of ester intra-unit linkages within EGCG during pretreatment. Overall, our results suggest that apoplastic deposition of EGCG for incorporation into lignin would be a promising plant genetic engineering target for improving the delignification and saccharification of biomass crops.

  12. Determination of the crystal structure and active residues of FabV, the enoyl-ACP reductase from Xanthomonas oryzae.

    Directory of Open Access Journals (Sweden)

    He Li

    Full Text Available Enoyl-ACP reductase (ENR catalyses the last reduction reaction in the fatty acid elongation cycle in bacteria and is a good antimicrobial target candidate. FabV is the most recently discovered class of ENR, but we lack information about the atomic structure and the key residues involved in reductase activity except for the known conserved tyrosine and lysine residues in the Y-X(8-K active site motif.Here we report the crystal structure of FabV from Xanthomonas oryzae (xoFabV. The crystal structure of this enzyme has been solved to 1.6 Å resolution in space group P2(12(12(1. The model of xoFabV consists of one monomer in the asymmetric unit which is composed of 13 α-helices and 11 β-strands, representing a canonical Rossmann fold architecture. Structural comparison presents that the locations of the conserved tyrosine (Y236 and lysine (K245 residues in the Y-X(8-K active site motif of xoFabV and the Y-X(6-K motif of ecFabI are notably similar. However, the conformations of Y236 in xoFabV and Y156 in ecFabI are distinct. Structure-based site-directed mutagenesis and enzymatic activity assays reveal that in addition to the conserved Y236 and K245 in the Y-X(8-K motif, Y53, D111 and Y226 are key residues implicated in the reductase activity, and F113 and T276 are also important for enzyme function. Moreover, a proposed active lysine located immediately after the Y-X(8-K motif in FabV from Burkholderia mallei (bmFabV is altered to an inactive V246 in xoFabV.We determine the first crystal structure of the FabV enzyme and identify several residues important for its enzymatic activity. These findings lay a solid foundation for the development of specific antibacterial inhibitors of the pathogenic bacteria, such as Vibrio cholerae, Burkholderia species and Xanthomonas species.

  13. Gasification kinetic analysis of the three pseudocomponents of biomass-cellulose, semicellulose and lignin.

    Science.gov (United States)

    Chen, Tianju; Wu, Jingli; Zhang, Jinzhi; Wu, Jinhu; Sun, Li

    2014-02-01

    The gasification kinetic analysis of the three pseudocomponents (hemicellulose, cellulose and lignin) of biomass decomposition in the agent of CO2 were investigated. The Multi-peaks method was used to fit the Gaussian distribution model of DTG curves. The Friedman method was used to estimate the effective Eα, and the master plot method was used for the determination of the kinetic model. The results showed that there were two reaction stages for semi-cellulose and lignin. The DTG curves of semicellulose and lignin cannot be fitted by Gaussian distribution model. The Eα were ranged from 80 to 220kJmol(-1) for the three pseudocomponents. The Fn model could describe the kinetic process of stage I of semi-cellulose decomposition. Both cellulose and stage II of semicellulose decomposition could be described by An model and the two reaction stages of the lignin were fitted the Rn model very well. Copyright © 2013 Elsevier Ltd. All rights reserved.

  14. Lignin solubilisation and gentle fractionation in liquid ammonia

    NARCIS (Netherlands)

    Strassberger, Z.; Prinsen, P.; Klis, van der F.; Es, van D.S.; Tanase, S.; Rothenberg, G.

    2015-01-01

    We present a simple method for solubilising lignin using liquid ammonia. Unlike water, which requires harsh conditions, ammonia can solubilise technical lignins, in particular kraft lignin. A commercial pine wood Kraft lignin (Indulin AT) was solubilized instantaneously at room temperature and 7–11

  15. The Use of Esterified Lignin for Synthesis of Durable Composites

    Science.gov (United States)

    S. Olsson; E. Ostmark; R.E. Ibach; C.M. Clemons; K.B. Segerholm; F. Englund

    2011-01-01

    Lignin is a natural polymer and one of the most abundant materials on earth. Despite this fact, lignin is often viewed as a by-product in chemical pulp processing and the use of lignin as a sustainable material is low. However, research and public awareness of sustainability have opened up new possibilities for using lignin as a material.

  16. Liquid chromatography-UV diode-array detection method for multi-residue determination of macrolide antibiotics in sheep's milk.

    Science.gov (United States)

    García-Mayor, M A; Garcinuño, R M; Fernández-Hernando, P; Durand-Alegría, J S

    2006-07-28

    A rapid, simple and sensitive liquid chromatography-UV diode-array detection method was developed for the simultaneous determination of seven macrolides (erythromycin, oleandomycin, roxithromycin, josamycin, spiramycin, tylosin and ivermectin) in sheep's milk. The column, mobile phase, temperature and flow rate were optimised to provide the best resolution of these analytes. The extraction of the antibiotic residues involves the treatment of protein-free samples with a combination of concentrated sodium hydroxide and ethyl acetate. Necessary defatting is achieved by alkaline hydrolysis. The recovery of each antibiotic was between 55% and 77%, with relative standard deviations ranging from 1% to 6.5%. The limit of quantification was 72.4 microg/kg for ivermectin, 48.3 microg/kg for roxithromycin, and 24.1 microg/kg for erythromycin, oleandomycin, spiramycin, josamycin and tylosin. The procedure was successfully used in the multi-residue determination of these macrolides at levels below the maximum concentrations legally allowed in milk samples.

  17. Validation of a new analytical procedure for determination of residual solvents in [{sup 18}F]FDG by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Flávia M.; Costa, Cassiano L.S.; Silva, Juliana B.; Ferreira, Soraya M.Z.M.D., E-mail: flaviabiomedica@yahoo.com.br [Centro de Desenvolvimento da Tecnologia Nuclear (UPPR/CDTN/CNEN-MG), Belo Horizonte, MG (Brazil). Unidade de Pesquisa e Produção de Radiofármacos

    2017-07-01

    Fludeoxyglucose F 18 ([{sup 18}F]FDG) is the most used radiopharmaceutical for positron emission tomography, especially on oncology. Organic solvents such as ether, ethanol and acetonitrile might be used in the synthesis of [{sup 18}F]FDG; however, they might not be completely removed during purification steps. The determination of residual solvents in [{sup 18}F]FDG is required in the European Pharmacopoeia (EP) and the United States Pharmacopeia (USP) monographs. While the procedure described in the EP is quite general, the one described in the USP requires a long runtime (about 13 minutes). In this work a simple and fast (4-minute) analytical procedure was developed and validated for determination of residual solvents in [{sup 18}F]FDG. Analyses were carried out in a Perkin Elmer gas chromatograph equipped with a flame ionization detector. The separation was obtained on a 0.53-mm x 30 m fused-silica column. Validation included the evaluation of various parameters, such as: specificity, linearity and range, limits of detection and quantitation, precision (repeatability and intermediate precision), accuracy, and robustness. Results were found to be within acceptable limits, indicating the developed procedure is suitable for its intended application. Considering the short half-life of fluorine-18 (109.7 minutes), this new method could be a valuable alternative for routine quality control of [{sup 18}F]FDG. (author)

  18. [Determination of avermectin, diclazuril, toltrazuril and metabolite residues in pork by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Gong, Xiaoming; Sun, Jun; Dong, Jing; Yu, Jinling; Wang, Hongtao

    2011-03-01

    A method for the determination of avermectin, ivermectin, doramectin, moxidectin, eprinomectin, diclazuril, toltrazuril and its two metabolite residues in pork was developed using QuEChERS method with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with acetonitrile and purified through QuEChERS method using ODS as the sorbent. The target compounds were separated on a Venusil ASB C18 column (150 mm x 2.1 mm, 3.0 microm) and detected by HPLC-MS/MS. The linear ranges were 0.005 - 0.2 mg/L and the correlation coefficients were all above 0.990. The average recoveries and the relative standard deviations ranged from 73.2% to 91.5% and from 12% to 17% at the spiked levels of 0.005, 0.01 and 0.02 mg/kg for the 9 analytes in pork matrix. This method is reliable, and suitable for the determination of the residues of avermectin and related compounds in pork.

  19. Determination of Two Sulfonylurea Herbicides Residues in Soil Environment Using HPLC and Phytotoxicity of These Herbicides by Lentil Bioassay.

    Science.gov (United States)

    Mehdizadeh, Mohammad; Alebrahim, Mohammad Taghi; Roushani, Mahmoud

    2017-07-01

    A HPLC-UV detection system was used for determination of sulfosulfuron and tribenuron methyl residues from soils. The soils were fortified with sulfosulfuron and tribenuron methyl at rates of 26 and 15 g a.i. ha -1 respectively and samples were taken randomly on 0 (2 h), 1, 2, 4, 10, 20, 40, 60, 90 and 120 days after treatment. The final extracts were prepared for analysis by HPLC. The results showed that degradation of both herbicides in the silty loam soil was faster than sandy loam soil. Half-life of sulfosulfuron was ranged from 5.37 to 10.82 days however this value for tribenuron methyl was ranged from 3.23 to 5.72 days on different soils. The residue of both herbicides at 120 days after application in wheat field had no toxicitic effect on lentil. It was concluded that HPLC analysis procedure was an appropriate method for determination of these herbicides from soils.

  20. Determination of platinum group metal catalyst residues in active pharmaceutical ingredients by means of total reflection X-ray spectrometry

    Science.gov (United States)

    Marguí, Eva; Queralt, Ignasi; Hidalgo, Manuela

    2013-08-01

    The control of metal catalyst residues (i.e., platinum group metals (PGMs)) in different stages of the manufacturing processes of the active pharmaceutical ingredients (APIs) and, especially, in the final product is crucial. For API specimens, there are strict guidelines to limit the levels of metal residues based on their individual levels of safety concern. For PGMs the concentration limit has been established at 10 mg/kg in the API. Therefore great effort is currently being devoted to the development of new and simple procedures to control metals in pharmaceuticals. In the present work, an analytical methodology based on benchtop total reflection X-ray fluorescence spectrometry (TXRF) has been developed for the rapid and simple determination of some PGM catalyst impurities (Rh, Pd, Ir and Pt) in different types of API samples. An evaluation of different sample treatments (dissolution and digestion of the solid pharmaceutical samples) has been carried out and the developed methodologies have been validated according to the analytical parameters to be considered and acceptance criteria for PGM determination according to the United States Pharmacopeia (USP). Limits of quantification obtained for PGM metals were in the range of 2-4 mg/kg which are satisfactory according to current legislation. From the obtained results it is shown that the developed TXRF method can be implemented in the pharmaceutical industries to increase productivity of the laboratory; offering an interesting and complementary analytical tool to other atomic spectroscopic methods.

  1. Large-Scale Transcriptome Analysis of Two Sugarcane Genotypes Contrasting for Lignin Content.

    Directory of Open Access Journals (Sweden)

    Renato Vicentini

    Full Text Available Sugarcane is an important crop worldwide for sugar and first generation ethanol production. Recently, the residue of sugarcane mills, named bagasse, has been considered a promising lignocellulosic biomass to produce the second-generation ethanol. Lignin is a major factor limiting the use of bagasse and other plant lignocellulosic materials to produce second-generation ethanol. Lignin biosynthesis pathway is a complex network and changes in the expression of genes of this pathway have in general led to diverse and undesirable impacts on plant structure and physiology. Despite its economic importance, sugarcane genome was still not sequenced. In this study a high-throughput transcriptome evaluation of two sugarcane genotypes contrasting for lignin content was carried out. We generated a set of 85,151 transcripts of sugarcane using RNA-seq and de novo assembling. More than 2,000 transcripts showed differential expression between the genotypes, including several genes involved in the lignin biosynthetic pathway. This information can give valuable knowledge on the lignin biosynthesis and its interactions with other metabolic pathways in the complex sugarcane genome.

  2. Antioxidant Activity of the Lignins Derived from Fluidized-Bed Fast Pyrolysis

    Directory of Open Access Journals (Sweden)

    Sohail S. Qazi

    2017-03-01

    Full Text Available A challenge in recent years has been the rational use of forest and agriculture residues for the production of bio-fuel, biochemical, and other bioproducts. In this study, potentially useful compounds from pyrolytic lignins were identified by HPLC-MS/MS and untargeted metabolomics. The metabolites identified were 2-(4-allyl-2-methoxyphenoxy-1-(4-hydroxy-3-methoxyphenyl-1-propanol, benzyl benzoate, fisetinidol, phenyllactic acid, 2-phenylpropionic acid, 6,3′-dimethoxyflavone, and vanillin. The 2,2-diphenyl-1-picrylhydrazyl radical scavenging activity (DPPH, trolox equivalent antioxidant capacity (TEAC, and total phenolics content (TPC per gram of pyrolytic lignin ranged from 14 to 503 mg ascorbic acid equivalents, 35 to 277 mg trolox equivalents, and 0.42 to 50 mg gallic acid equivalents, respectively. A very significant correlation was observed between the DPPH and TPC (r = 0.8663, p ≤ 0.0001, TEAC and TPC (r = 0.8044, p ≤ 0.0001, and DPPH and TEAC (r = 0.8851, p ≤ 0.0001. The polyphenolic compounds in the pyrolytic lignins which are responsible for radical scavenging activity and antioxidant properties can be readily profiled with HPLC-MS/MS combined with untargeted metabolomics. The results also suggest that DPPH, TEAC, and TPC assays are suitable methods for the measurement of antioxidant activity in a variety of pyrolytic lignins. These data show that the pyrolytic lignins can be considered as promising sources of natural antioxidants and value-added chemicals.

  3. Preparation of ractopamine-tetraphenylborate complexed nanoparticles used as sensors to rapidly determine ractopamine residues in pork

    Science.gov (United States)

    Zhang, Jing; Shao, Xintian; Yue, Jingli; Li, Donghui; Chen, Zhenhua

    2014-11-01

    In this work, we reported a simple, fast, and sensitive determination of ractopamine (RAC) residues in pork by using novel ractopamine-tetraphenylborate complexed nanoparticles (RT NPs) as sensors. The prepared RT NPs exhibited a fast response time of 10 s, a wide linear range from 0.1 to 1.0 × 10-7 mol/L, and a very low detection limit of 7.4 × 10-8 mol/L. The prepared sensor also presents a high selectivity for ractopamine under different pH conditions ranged from 2.85 to 7.18. These results reveal that the fabricated RT NPs can be used as efficient electrochemical sensors to determine ractopamine in animal productions.

  4. Exploring matrix effects in liquid chromatography-tandem mass spectrometry determination of pesticide residues in tropical fruits.

    Science.gov (United States)

    Botero-Coy, Ana María; Marín, José M; Serrano, Roque; Sancho, Juan Vicente; Hernández, Félix

    2015-05-01

    Tropical fruits are being increasingly consumed around the world because of their appreciated characteristics, particularly their high nutritional value and distinctive taste, which are different from those of traditional fruits. Owing to their introduction into international markets it is necessary to have a reliable analytical methodology available for the sensitive determination of pesticide residues in order to monitor the compliance of maximum residue limits (MRLs). From an analytical point of view, tropical fruits have generally been far less studied than other fruits frequently consumed in the European Union or USA, which are among the most important markets. In this work, LC-MS/MS-based methodology using a triple quadrupole analyzer was developed for the multi-residue determination of selected pesticides and metabolites in tropical fruits, which were selected among the most popular in Colombia, one of the most important suppliers of tropical fruits around the world. After selection of a QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)-based sample treatment, the study focused on the evaluation of matrix effects, in order to find a simple way for their correction. Twelve different food matrices were selected to perform this study: the seven Colombian tropical fruits of highest value for domestic and international markets (uchuva, tamarillo, granadilla, gulupa, maracuya, papaya, and pithaya), and five more matrices highly consumed in Colombia (lulo, carambolo, feijoa, mangostan, and guayaba). Twenty compounds, including pesticides widely applied in tropical fruits pest control and several metabolites considered in residue definition, were used as model compounds in this work. Correction factors were used on the basis of calibration graphs obtained with standards in solvent and in matrix, and their usefulness was supported by validation of the method in all the matrices tested at 0.01 and 0.1 mg/kg. The analysis of real-world samples revealed the

  5. Solvothermal conversion of technical lignins over NiMo catalysts

    DEFF Research Database (Denmark)

    Ghafarnejad Parto, Soheila; Christensen, Jakob Munkholt; Pedersen, Lars Saaby

    of the range of available technical lignins. In this work, catalytic conversion of different types of lignin using an alumina supported NiMo catalyst (provided by Haldor Topsøe A/S) is conducted in ethanol at 310 ˚C with initial hydrogen pressure of 25 barg. The reaction time was set to 3 hours. Proton...... lignin, a renewable source of valuable chemicals would be available and the economic viabilities of the relevant industries will be promoted. Most of the recent publications have targeted one type of lignin such as Kraft lignin 1. However, it is desirable to introduce a method suitable for conversion......-Lignosulfonate (H-LS, provided by Borregaard A/S in form of Sodium-Lignosulfonate), Kraft lignin, Protobind 1000 and Organosolv lignin are among the selected lignin types. Non-catalytic conversion of each type of lignin was also performed at similar reaction conditions for comparison. The catalyst: lignin: solvent...

  6. Near-infrared spectroscopic determination of residual moisture in lyophilized sucrose through intact glass vials.

    Science.gov (United States)

    Kamat, M S; Lodder, R A; DeLuca, P P

    1989-11-01

    A rapid, noninvasive, and nondestructive method for determining moisture in sealed freeze-drying vials is described. The method, based on near-infrared spectrometry, used a novel fiber-optic diffuse-reflectance probe to make remote reflectance measurements from 1100 to 2500 nm through the bottom of glass vials. The correlation of the method to results obtained by Karl Fischer analysis was good (r2 = 0.97). The moisture content of sucrose, a common cryoprotectant, was determined with an error of 0.27% using a single sample scan.

  7. Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorus detection

    NARCIS (Netherlands)

    Brinkman, J.H.W.; Dijk, A.G. van; Wagenaar, R.; Quirijns, J.K.

    1996-01-01

    A method was developed for the determination of daminozide in apples using gas chromatography (GC) with nitrogen-phosphorus detection (NPD). Daminozide is hydrolysed to 1,1-dimethylhydrazine (UDMH) by alkaline digestion. The UDMH generated is distilled from the apple matrix, derivatized with

  8. FT-Raman investigation of milled-wood lignins : softwood, hardwood, and chemically modified black spruce lignins

    Science.gov (United States)

    Umesh P. Agarwal; James D. McSweeny; Sally A. Ralph

    2011-01-01

    Raman spectroscopy is being increasingly applied to study wood and other lignin-containing biomass/biomaterials. Lignin’s contribution to the Raman spectra of such materials needs to be understood in the context of various lignin structures, substructures, and functional groups so that lignin-specific features could be identified and the spectral information could be...

  9. High performance liquid chromatographic determination of residual monomer released from heat-cured acrylic resin. An in vivo study.

    Science.gov (United States)

    Singh, Raghuwar D; Gautam, Rupali; Siddhartha, Ramashanker; Singh, Balendra P; Chand, Pooran; Sharma, Vinod P; Jurel, Sunit K

    2013-07-01

    Heat-polymerized acrylic resins are used in dentistry for complete denture fabrication. Despite the polymerization method, conversion of monomer into polymer is often incomplete with free or unreacted residual monomer remaining in the polymerized resin. The aim of this study was to determine the amount of residual monomeric methyl methacrylate (MMA) leaching in the saliva of patients wearing complete dentures in their postinsertion period. Thirty edentulous participants as first-time complete denture wearers (age 60 to 65 years) were selected. All the prostheses were fabricated using a similar standard technique with a heat-cured acrylic resin denture base material. Saliva samples were collected at time intervals of 1 hour, 1 day, and 3 days postdenture insertion. Participants were asked to discharge saliva every 30 seconds into a pre-weighed screw-capped container for a 5-minute period. MMA levels were measured using high performance liquid chromatography. Data were analyzed by ANOVA and Tukey-HSD. The maximum concentration of monomer released into saliva peaked 1 day after insertion of the complete dentures. The mean (SD) MMA content was 0.04 ± 0.01 (μg/ml) 1 hour after insertion, and 0.3 ± 0.09 (μg/ml), and 0.05 ± 0.01 (μg/ml) on the first and third days postinsertion, respectively. Although the released monomeric MMA was not at toxic levels, it could potentially sensitize complete denture patients or elicit an allergic reaction. The risk of the residual material as a primary irritant for a sensitizing reaction could be minimized by immersion of the denture in water for 24 hours before insertion. © 2012 by the American College of Prosthodontists.

  10. Synthesis and characterization of kraft lignin-based epoxy resins

    OpenAIRE

    El Mansouri, Nour-Eddine; Yuan, Qiaolong; Huang, Farong

    2011-01-01

    Epoxidization is an interesting way to develop a new application of lignin and therefore to improve its application potential. In this work, kraft lignin-based epoxy resins were obtained by the epoxidization reaction, using the kraft lignin recovered directly from pulping liquor and modified by a methylolation reaction. The methylolated lignins were obtained by the reaction of original kraft lignin with formaldehyde and glyoxal, which is a less volatile and less toxic aldehyde. 1H-NMR spectro...

  11. Development of a prototype lignin concentration sensor. Final report. Draft

    Energy Technology Data Exchange (ETDEWEB)

    Jeffers, L.A.

    1994-11-01

    The ultimate objective of the DOE-sponsored program discussed in this report is to commercialize an instrument for real-time, in-situ measurement of lignin in wood pulp at a variety of locations in the pulp process stream. The instrument will be used as a primary sensor for process control in the pulp and paper industry. Work done by B&W prior to the initiation of this program had shown: there is a functional relationship between the fluorescence intensity and the Kappa number as measured at the pulp mill laboratory. Kappa number is a standard wet chemical method for determination of the lignin concentration; the relationship is one of decreasing intensity with Kappa number, indicating operation in the quenched fluorescence regime; a great deal of scatter in the data. Because of the preliminary nature of the study, the origin of the scatter was not identified. This report documents the results of laboratory measurements made on a variety of well defined pulp samples to generate the data necessary to: determine the feasibility of an instrument for on-line lignin concentration measurement using laser fluorescence; identify the preferred measurement strategy; define the range of applicability of the instrument; and to provide background information to guide the design of a field-worthy prototype.

  12. Adsorption Properties of Lignin-derived Activated Carbon Fibers (LACF)

    Energy Technology Data Exchange (ETDEWEB)

    Contescu, Cristian I. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Gallego, Nidia C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Thibaud-Erkey, Catherine [United Technologies Research Center (UTRC), East Hartford, CT (United States); Karra, Reddy [United Technologies Research Center (UTRC), East Hartford, CT (United States)

    2016-04-01

    The object of this CRADA project between Oak Ridge National Laboratory (ORNL) and United Technologies Research Center (UTRC) is the characterization of lignin-derived activated carbon fibers (LACF) and determination of their adsorption properties for volatile organic compounds (VOC). Carbon fibers from lignin raw materials were manufactured at Oak Ridge National Laboratory (ORNL) using the technology previously developed at ORNL. These fibers were physically activated at ORNL using various activation conditions, and their surface area and pore-size distribution were characterized by gas adsorption. Based on these properties, ORNL did down-select five differently activated LACF materials that were delivered to UTRC for measurement of VOC adsorption properties. UTRC used standard techniques based on breakthrough curves to measure and determine the adsorption properties of indoor air pollutants (IAP) - namely formaldehyde and carbon dioxide - and to verify the extent of saturated fiber regenerability by thermal treatments. The results are summarized as follows: (1) ORNL demonstrated that physical activation of lignin-derived carbon fibers can be tailored to obtain LACF with surface areas and pore size distributions matching the properties of activated carbon fibers obtained from more expensive, fossil-fuel precursors; (2) UTRC investigated the LACF potential for use in air cleaning applications currently pursued by UTRC, such as building ventilation, and demonstrated their regenerability for CO2 and formaldehyde, (3) Both partners agree that LACF have potential for possible use in air cleaning applications.

  13. Organosolv Lignin-Based Wood Adhesive. Influence of the Lignin Extraction Conditions on the Adhesive Performance

    Directory of Open Access Journals (Sweden)

    Issam Dababi

    2016-09-01

    Full Text Available Ethanol organosolv alfa grass lignins were extracted in the presence of sulfuric acid or Lewis acids (Sc(OTf3, FeCl3 as catalysts and subjected to a comprehensive structural characterization by solid state 13C NMR, GPC, MALDI-TOF, and ASAP-MS/MS. The impact of the severity of the treatment and of the nature of the acid catalyst on the recovered lignin structure was investigated. The lignins isolated at high severity were highly recondensed and partly composed of regular structures composed of furan-like rings. The alfa (Stipa tenacissima L. organosolv lignins were used for the preparation of formaldehyde-free adhesives which were characterized by TMA and used for the preparation of particleboard without any addition of synthetic resin. It has been demonstrated for the first time that: (1 the addition of 10% to 30% of organosolv alfa lignin in a tannin-based adhesive improved the adhesive performance; and (2 the conditions of the lignin extraction strongly impact the lignin-based adhesive performances. The highly recondensed lignin extracted with sulfuric acid as a catalyst allowed the production of resins with improved performances. Formulations composed of 50% glyoxalated alfa lignin and 50% of Aleppo Pine tannins yielded good internal bond strength results for the panels (IB = 0.45 MPa and satisfied relevant international standard specifications for interior-grade panels.

  14. Determination of Beta-Lactam residues in milk by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Roseane Brandão de Brito

    2006-01-01

    Full Text Available A high performance liquid chromatographic method to assay beta-lactam residues in milk was developed and validated. Milk samples were spiked with standard solutions and deproteinated. The extract was cleaned-up on C18 SPE cartridge, the antibiotics eluted with acetonitrile:water (50:50 v/v and derivatized with acetic anhydride and 1-methyl-imidazole solution containing HgCl2. The chromatographic analysis was performed on C18 column using mobile phase consisting of acetonitrile and phosphate buffer (pH 6.5 in the presence of Na2S2O3 gradient and detection at 325 nm. The method was selective for ampicillin, penicillin G and penicillin V, the latter used as internal standard. Average recoveries for ampicillin and penicillin G ranged, respectively, from 60.0% to 104.9% and from 82.7% to 109.2%, with coefficients of variation from 11.1% to 24.6%, and from 2.1% to 25.2%, indicating accuracy and precision. Detection limit of 4.0 µg/L for ampicillin and 3.0 µg/L for penicillin G, and quantification limits of 4.0 µg/L for both were estimated.Um método para determinar resíduos de antibióticos beta-lactâmicos em leite por cromatografia líquida de alta eficiência (CLAE foi desenvolvido e validado. Amostras brancas foram adicionadas de padrão e desproteinizadas. O extrato foi purificado por extração em fase sólida C18, os antibióticos eluídos com acetonitrila:água (50:50 v/v e posteriormente derivatizados com anidrido acético e solução de 1-metil-imidazol contendo HgCl2. A análise cromatográfica foi realizada utilizando coluna C18, fase móvel composta por acetonitrila e tampão fosfato pH 6,5, na presença de Na2S2O3 em gradiente e detecção a 325 nm. O método foi seletivo para ampicilina, penicilina G e penicilina V, sendo este último utilizado como padrão interno. As médias de recuperação para ampicilina e penicilina G situaram-se, respectivamente, na faixa de 60,0% a 104,9% e de 82,7% a 109,2%, com coeficientes de varia

  15. Manipulation of Guaiacyl and Syringyl Monomer Biosynthesis in an Arabidopsis Cinnamyl Alcohol Dehydrogenase Mutant Results in Atypical Lignin Biosynthesis and Modified Cell Wall Structure

    Energy Technology Data Exchange (ETDEWEB)

    Anderson, Nickolas A.; Tobimatsu, Yuki; Ciesielski, Peter N.; Ximenes, Eduardo; Ralph, John; Donohoe, Bryon S.; Ladisch, Michael; Chapple, Clint

    2015-08-01

    Modifying lignin composition and structure is a key strategy to increase plant cell wall digestibility for biofuel production. Disruption of the genes encoding both cinnamyl alcohol dehydrogenases (CADs), including CADC and CADD, in Arabidopsis thaliana results in the atypical incorporation of hydroxycinnamaldehydes into lignin. Another strategy to change lignin composition is downregulation or overexpression of ferulate 5-hydroxylase (F5H), which results in lignins enriched in guaiacyl or syringyl units, respectively. Here, we combined these approaches to generate plants enriched in coniferaldehyde-derived lignin units or lignins derived primarily from sinapaldehyde. The cadc cadd and ferulic acid hydroxylase1 (fah1) cadc cadd plants are similar in growth to wild-type plants even though their lignin compositions are drastically altered. In contrast, disruption of CAD in the F5H-overexpressing background results in dwarfism. The dwarfed phenotype observed in these plants does not appear to be related to collapsed xylem, a hallmark of many other lignin-deficient dwarf mutants. cadc cadd, fah1 cadc cadd, and cadd F5H-overexpressing plants have increased enzyme-catalyzed cell wall digestibility. Given that these CAD-deficient plants have similar total lignin contents and only differ in the amounts of hydroxycinnamaldehyde monomer incorporation, these results suggest that hydroxycinnamaldehyde content is a more important determinant of digestibility than lignin content.

  16. Downregulation of caffeoyl-CoA O-methyltransferase (CCoAOMT by RNA interference leads to reduced lignin production in maize straw

    Directory of Open Access Journals (Sweden)

    Xiaoyu Li

    2013-01-01

    Full Text Available Lignin is a major cell wall component of vascular plants that provides mechanical strength and hydrophobicity to vascular vessels. However, the presence of lignin limits the effective use of crop straw in many agroindustrial processes. Here, we generated transgenic maize plants in which the expression of a lignin biosynthetic gene encoding CCoAOMT , a key enzyme involved in the lignin biosynthesis pathway was downregulated by RNA interference (RNAi. RNAi of CCoAOMT led to significantly downregulated expression of this gene in transgenic maize compared with WT plants. These transgenic plants exhibited a 22.4% decrease in Klason lignin content and a 23.3% increase in cellulose content compared with WT plants, which may reflect compensatory regulation of lignin and cellulose deposition. We also measured the lignin monomer composition of the RNAi plants by GC-MS and determined that transgenic plants had a 57.08% higher S/G ratio than WT plants. In addition, histological staining of lignin with Wiesner reagent produced slightly more coloration in the xylem and sclerenchyma than WT plants. These results provide a foundation for breeding maize with low-lignin content and reveal novel insights about lignin regulation via genetic manipulation of CCoAOMT expression.

  17. Optimized Production of Lignin Peroxidase, Manganese Peroxidase

    African Journals Online (AJOL)

    Mgina

    OPTIMIZED PRODUCTION OF LIGNIN PEROXIDASE, MANGANESE. PEROXIDASE AND LACCASE IN SUBMERGED CULTURES OF. TRAMETES TROGII USING VARIOUS GROWTH MEDIA. COMPOSITIONS. F Patrick*, G Mtui, AM Mshandete and A Kivaisi. Department of Molecular Biology and Biotechnology, College ...

  18. Composition comprising lignin and antidi arrheal component

    DEFF Research Database (Denmark)

    2008-01-01

    The present invention relates to a composition comprising lignin and at least one compound selected from the group consisting of bromelain, papain, tannin, carvacrol, thymol, alliin, allicin, fenugreek seed, egg, poppy, poppy seeds, humic acid, roots, kaolin, catechu, cellulase, flavonoid...

  19. Liquefaction of Biorefinery Lignin for Fuel Production

    DEFF Research Database (Denmark)

    Jensen, Anders

    Lignocellulosic biorefineries can be an important piece of the puzzle in fighting climate change. Present, biorefineries that produce ethanol from lignocellulose are challenged in working on market terms as the two product streams ethanol and lignin are low value products. The aim of this project...... has been to increase the value of the lignin stream. Recent regulations on shipping exhaust gasses in coastal waters dictate lower sulfur emissions which require ships to use low sulfur fuels for propulsion. This opens or expands a very large market for low sulfur fuels because a shift from...... traditional sulfur containing bunker fuel is needed. The lignin stream from lignocellulosic biorefineries could provide a source for the production of sulfur free fuels and this is what has been explored and demonstrated in this PhD project. The chemical reactions taking place in lignin during hydrothermal...

  20. Determination of pesticide residues in animal origin baby foods by gas chromatography coupled with triple quadrupole mass spectrometry.

    Science.gov (United States)

    Amendola, Graziella; Pelosi, Patrizia; Attard Barbini, Danilo

    2015-01-01

    A simple, fast and multiresidue method for the determination of pesticide residues in baby foods of animal origin has been developed in order to check the compliance with the Maximum Residue Levels (MRLs) set at a general value of 0.01 mg/kg by Commission Directive 2006/125/EC for infant foods. The main classes of organochlorine, organophosphorus and pyrethroid compounds have been considered, which are mainly fat soluble pesticides. The analytical procedure consists in the extraction of baby food samples by acetonitrile (ACN) followed by a clean up using C18 solid-phase extraction column eluted with ACN. The compounds were determined by gas chromatography-triple quadrupole mass spectrometry equipped with a Programmed Temperature Vaporizer (PTV) injection and a backflush system. In order to compensate for matrix effects PTV and matrix matched standard calibrations have been used. The method has been fully validated for 57 pesticides according to the Document SANCO/12571/2013. Accuracy and precision (repeatability) have been studied by recoveries at two spiking levels, the Limit of Quantitation (LOQ) (0.003-0.008 mg/kg) and 10 time greater (0.03-0.08 mg/kg), and the results were in the acceptable range of 70-120% with Relative Standards Deviations (RSD) ≤20%. Selectivity, linearity, LOQ and uncertainty of measurement were also determined for all the compounds. The method has been also applied for the analysis of 18 baby food animal origin samples, bought form the local market in Rome (Italy), and no pesticide in the scope of the method has been found above the MRL or the LOQ.

  1. [Determination of paraquat residue in plant-derived foodstuffs by high performance liquid chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Bo, Haibo

    2011-02-01

    A sensitive and selective method is presented for the determination of paraquat residue in fruits, vegetables, beans and grain by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Paraquat in samples was extracted with water and cleaned-up with a weak cation exchange (WCX) column to obtain an extract suitable for analysis using HPLC-MS/MS. The paraquat was separated by a CAPCELL PAK ST column (150 mm x 2.0 mm) and with acetonitrile-10 mmol/L ammonium acetate solution (adjusted to pH 4.0 by formic acid) as the mobile phase, and multiple reaction monitoring (MRM) was used with electrospray ionization in the positive ion mode. The calibration curve was linear between the peak area and the mass concentration of paraquat from 0.01 to 0.1 mg/L with the correlation coefficient of 0.993. Recoveries of paraquat spiked in samples at three levels ranged from 84.0% to 106.0% with the relative standard deviations of 7.8% - 18.8%. The limits of detection (LODs) of paraquat were 0.01 mg/kg in fruits and vegetables and 0.05 mg/kg in beans and grain. The LODs can meet the requirements of international maximum residue limit.

  2. Determination of chlorantraniliprole residues in crops by liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry/mass spectrometry.

    Science.gov (United States)

    Grant, Joann; Rodgers, Carol A; Chickering, Clark D; Hill, Sidney J; Stry, James J

    2010-01-01

    An analytical method is presented for the determination of chlorantraniliprole residues in crops. Chlorantraniliprole residues were extracted from crop matrixes with acetonitrile after a water soak. The extracts were passed through a strong anion-exchange (SAX) SPE cartridge stacked on top of a reversed-phase (RP) polymer cartridge. After both cartridges were rinsed and vacuum-dried, the SAX cartridge was removed, and chlorantraniliprole was eluted from the RP polymer cartridge with acetonitrile. The acetonitrile eluate was evaporated to dryness, reconstituted, and analyzed using an LC/MS/MS instrument equipped with an atmospheric pressure chemical ionization source. The method was successfully validated at 0.010, 0.10, and 10 mg/kg for the following crop matrixes: potatoes, sugar beets (tops), lettuce, broccoli, soybeans, soybean forage, tomatoes, cucumbers, oranges, apples, pears, peaches, almonds (nutmeat), rice grain, wheat grain, wheat hay, corn stover, alfalfa forage, cottonseed, grapes, and corn grain. The average recoveries from all crop samples fortified at the method LOQ ranged from 91 to 108%, with an overall average recovery of 97%. The average recoveries from all crop samples fortified at 10 times the method LOQ ranged from 89 to 115%, with an overall average recovery of 101%. For all of the fortified control samples analyzed in this study, the overall average recovery was 99%.

  3. T Cell Determinants Incorporating [beta]-Amino Acid Residues Are Protease Resistant and Remain Immunogenic In Vivo

    Energy Technology Data Exchange (ETDEWEB)

    Webb, Andrew I.; Dunstone, Michelle A.; Williamson, Nicholas A.; Price, Jason D.; Kauwe, Andreade; Chen, Weisan; Oakley, Aaron; Perlmutter, Patrick; McCluskey, James; Aguilar, Marie-Isabel; Rossjohn, Jamie; Purcell, Anthony W. (Monash); (Melbourne); (ANU)

    2010-07-20

    A major hurdle in designing successful epitope-based vaccines resides in the delivery, stability, and immunogenicity of the peptide immunogen. The short-lived nature of unmodified peptide-based vaccines in vivo limits their therapeutic application in the immunotherapy of cancers and chronic viral infections as well as their use in generating prophylactic immunity. The incorporation of {beta}-amino acids into peptides decreases proteolysis, yet its potential application in the rational design of T cell mimotopes is poorly understood. To address this, we have replaced each residue of the SIINFEKL epitope individually with the corresponding {beta}-amino acid and examined the resultant efficacy of these mimotopes. Some analogs displayed similar MHC binding and superior protease stability compared with the native epitope. Importantly, these analogs were able to generate cross-reactive CTLs in vivo that were capable of lysing tumor cells that expressed the unmodified epitope as a surrogate tumor Ag. Structural analysis of peptides in which anchor residues were substituted with {beta}-amino acids revealed the basis for enhanced MHC binding and retention of immunogenicity observed for these analogs and paves the way for future vaccine design using {beta}-amino acids. We conclude that the rational incorporation of {beta}-amino acids into T cell determinants is a powerful alternative to the traditional homologous substitution of randomly chosen naturally occurring {alpha}-amino acids, and these mimotopes may prove particularly useful for inclusion in epitope-based vaccines.

  4. VALIDATION HPLC METHOD FOR THE DETERMINATION OF CLONIDINE HYDROCHLORIDE RESIDUES FROM PHARMACEUTICAL MANUFACTURING EQUIPMENT

    Directory of Open Access Journals (Sweden)

    A. V. Yegorova

    2015-04-01

    Full Text Available Highly sensitive HPLC method of determination of clonidine hydrochloride trace amounts for validation cleaning process of the pharmaceutical equipment has been proposed. The developed method has been validated on the following parameters: specificity, linearity, precision, limit of detection and limit of quantification. The calibration curve was linear over the concentration range of 0.1-6.0 mg / ml, the limit of detection is 0.026 μg/ml. It has been found that clonidine hydrochloride solutions are stable for 48 hours. Effectiveness of the method of sampling is more than 95%.

  5. Enzymes in Commercial Cellulase Preparations Bind Differently to Dioxane Extracted Lignins

    Energy Technology Data Exchange (ETDEWEB)

    Yarbrough, John M.; Mittal, Ashutosh; Katahira, Rui; Mansfield, Elisabeth; Taylor, Larry E.; Decker, Stephen R.; Himmel, Michael E.; Vinzant, Todd

    2017-04-24

    Commercial fungal cellulases used in biomass-to-biofuels processes can be grouped into three general classes: native, augmented, and engineered. To evaluate lignin binding affinities of different enzyme activities in various commercial cellulase formulations in order to determine if enzyme losses due to lignin binding can be modulated by using different enzymes of the same activity We used water:dioxane (1:9) to extract lignin from pretreated corn stover. Commercial cellulases were incubated with lignin and the unbound supernatants were evaluated for individual enzyme loss by SDS=PAGE and these were correlated with activity loss using various pNP-sugar substrates. Colorimetric assays for general glycosyl hydrolase activities showed distinct differences in enzyme binding to lignin for each enzyme activity. Native systems demonstrated low binding of endo- and exo-cellulases, high binding of xylanase, and moderate ..beta..-glucosidase binding. Engineered cellulase mixtures exhibited low binding of exo-cellulases, very strong binding of endocellulases and ..beta..- glucosidase, and mixed binding of xylanase activity. The augmented cellulase had low binding of exocellulase, high binding of endocellulase and xylanase, and moderate binding of ..beta..-glucosidase activities. Bound and unbound activities were correlated with general molecular weight ranges of proteins as measured by loss of proteins bands in bound fractions on SDS-PAGE gels. Lignin-bound high molecular weight bands correlated with binding of ..beta..-glucosidase activity. While ..beta..-glucosidases demonstrated high binding in many cases, they have been shown to remain active. Bound low molecular weight bands correlated with xylanase activity binding. Contrary to other literature, exocellulase activity did not show strong lignin binding. The variation in enzyme activity binding between the three classes of cellulases preparations indicate that it is certainly possible to alter the binding of specific

  6. A Tomato Peroxidase Involved in the Synthesis of Lignin and Suberin1

    Science.gov (United States)

    Quiroga, Mónica; Guerrero, Consuelo; Botella, Miguel A.; Barceló, Araceli; Amaya, Iraida; Medina, María I.; Alonso, Francisco J.; de Forchetti, Silvia Milrad; Tigier, Horacio; Valpuesta, Victoriano

    2000-01-01

    The last step in the synthesis of lignin and suberin has been proposed to be catalyzed by peroxidases, although other proteins may also be involved. To determine which peroxidases are involved in the synthesis of lignin and suberin, five peroxidases from tomato (Lycopersicon esculentum) roots, representing the majority of the peroxidase activity in this organ, have been partially purified and characterized kinetically. The purified peroxidases with isoelectric point (pI) values of 3.6 and 9.6 showed the highest catalytic efficiency when the substrate used was syringaldazine, an analog of lignin monomer. Using a combination of transgenic expression and antibody recognition, we now show that the peroxidase pI 9.6 is probably encoded by TPX1, a tomato peroxidase gene we have previously isolated. In situ RNA hybridization revealed that TPX1 expression is restricted to cells undergoing synthesis of lignin and suberin. Salt stress has been reported to induce the synthesis of lignin and/or suberin. This stress applied to tomato caused changes in the expression pattern of TPX1 and induced the TPX1 protein. We propose that the TPX1 product is involved in the synthesis of lignin and suberin. PMID:10759507

  7. Metagenomic scaffolds enable combinatorial lignin transformation.

    Science.gov (United States)

    Strachan, Cameron R; Singh, Rahul; VanInsberghe, David; Ievdokymenko, Kateryna; Budwill, Karen; Mohn, William W; Eltis, Lindsay D; Hallam, Steven J

    2014-07-15

    Engineering the microbial transformation of lignocellulosic biomass is essential to developing modern biorefining processes that alleviate reliance on petroleum-derived energy and chemicals. Many current bioprocess streams depend on the genetic tractability of Escherichia coli with a primary emphasis on engineering cellulose/hemicellulose catabolism, small molecule production, and resistance to product inhibition. Conversely, bioprocess streams for lignin transformation remain embryonic, with relatively few environmental strains or enzymes implicated. Here we develop a biosensor responsive to monoaromatic lignin transformation products compatible with functional screening in E. coli. We use this biosensor to retrieve metagenomic scaffolds sourced from coal bed bacterial communities conferring an array of lignin transformation phenotypes that synergize in combination. Transposon mutagenesis and comparative sequence analysis of active clones identified genes encoding six functional classes mediating lignin transformation phenotypes that appear to be rearrayed in nature via horizontal gene transfer. Lignin transformation activity was then demonstrated for one of the predicted gene products encoding a multicopper oxidase to validate the screen. These results illuminate cellular and community-wide networks acting on aromatic polymers and expand the toolkit for engineering recombinant lignin transformation based on ecological design principles.

  8. Evaluating spectral indices for determining conservation and conventional tillage systems in a vetch-wheat rotation

    Directory of Open Access Journals (Sweden)

    Iraj Eskandari

    2016-06-01

    CAI had a linear relationship with crop residue cover, which the comparative intensity of cellulose and lignin absorption features near 2100 nm can be measure by it. Coefficients of determination (r2 for crop residue cover as a function of CAI and LCA were 0.89 and 0.79 respectively. Absorption specifications near 2.1 and 2.3 µm in the reflectance spectra of crop residues in minimum and no- tillage systems were related to cellulose and lignin. These specifications were not evident in the spectra of conventional tillage system. In this study the best index to use was CAI, which showed complete separation tillage systems, followed by LCA and NDTI. Four tillage intensity classes, corresponding to intensive (60% cover tillage, were recognized in this study.

  9. The use of natural abundance stable isotopic ratios to indicate the presence of oxygen-containing chemical linkages between cellulose and lignin in plant cell walls.

    Science.gov (United States)

    Zhou, Youping; Stuart-Williams, Hilary; Farquhar, Graham D; Hocart, Charles H

    2010-06-01

    Qualitative and quantitative understanding of the chemical linkages between the three major biochemical components (cellulose, hemicellulose and lignin) of plant cell walls is crucial to the understanding of cell wall structure. Although there is convincing evidence for chemical bonds between hemicellulose and lignin and the absence of chemical bonds between hemicellulose and cellulose, there is no conclusive evidence for the presence of covalent bonds between cellulose and lignin. This is caused by the lack of selectivity of current GC/MS-, NMR- and IR-based methods for lignin characterisation as none of these techniques directly targets the possible ester and ether linkages between lignin and cellulose. We modified the widely-accepted "standard" three-step extraction method for isolating cellulose from plants by changing the order of the steps for hemicellulose and lignin removal (solubilisation with concentrated NaOH and oxidation with acetic acid-containing NaClO(2), respectively) so that cellulose and lignin could be isolated with the possible chemical bonds between them intact. These linkages were then cleaved with NaClO(2) reagent in aqueous media of contrasting (18)O/(16)O ratios. We produced cellulose with higher purity (a lower level of residual hemicellulose and no detectable lignin) than that produced by the "standard" method. Oxidative artefacts may potentially be introduced at the lignin removal stage; but testing showed this to be minimal. Cellulose samples isolated from processing plant-derived cellulose-lignin mixtures in media of contrasting (18)O/(16)O ratios were compared to provide the first quantitative evidence for the presence of oxygen-containing ester and ether bonds between cellulose and lignin in Zea mays leaves. However, no conclusive evidence for the presence or lack of similar bonds in Araucaria cunninghamii wood was obtained. Copyright 2010 Elsevier Ltd. All rights reserved.

  10. Gas chromatographic determination of residual hydrazine and morpholine in boiler feed water and steam condensates

    International Nuclear Information System (INIS)

    Vatsala, S.; Bansal, V.; Tuli, D.K.; Rai, M.M.; Jain, S.K.; Srivastava, S.P.; Bhatnagar, A.K.

    1994-01-01

    Hydrazine, an oxygen scavenger in boiler water, was derivatised to the corresponding acetone azine and determined at the ng ml -1 level by gas chromatography. Morpholine, a corrosion inhibitor used in steam boilers, was estimated either directly (if >2.0 μg ml -1 ) or by quantitative preconcentration (0.1 ng-2.0 μg ml -1 ). To obtain symmetrical peaks for these amines, the column packing was coated with KOH. Use of a nitrogen-specific detector improved accuracy of estimation of hydrazine and morpholine, giving a RSD of 1.9-3.6%. Chromatographic analysis of these amines in boiler feed water and steam condensate samples collected from boilers servicing a pertroleum refinery is described. Environmental safety regulations calls for monitoring of hydrazine and the methods developed can easily be adapted for this purpose. (orig.)

  11. Valorization of Furfural Residue by Hydrothermal Carbonization

    DEFF Research Database (Denmark)

    Yue, Fen; Zhang, Jia; Pedersen, Christian Marcus

    2017-01-01

    Furfural residue (FR) is a low-cost by-product generated in the furfural production from corncobs, which is mainly composed of cellulose and lignin. In this report, hydrothermal carbonization (HTC) of deashed FR was conducted at various reaction temperatures (200, 220 and 240 °C) and reaction tim...

  12. Preparation of ractopamine-tetraphenylborate complexed nanoparticles used as sensors to rapidly determine ractopamine residues in pork

    OpenAIRE

    Zhang, Jing; Shao, Xintian; Yue, Jingli; Li, Donghui; Chen, Zhenhua

    2014-01-01

    In this work, we reported a simple, fast, and sensitive determination of ractopamine (RAC) residues in pork by using novel ractopamine-tetraphenylborate complexed nanoparticles (RT NPs) as sensors. The prepared RT NPs exhibited a fast response time of 10 s, a wide linear range from 0.1 to 1.0 × 10−7 mol/L, and a very low detection limit of 7.4 × 10−8 mol/L. The prepared sensor also presents a high selectivity for ractopamine under different pH conditions ranged from 2.85 to 7.18. These result...

  13. Polychlorinated biphenyl residues in food and human milk: determination of co-planar and mono-ortho substituted congeners

    International Nuclear Information System (INIS)

    Boehm, V.; Schulte, E.; Thier, H.P.

    1993-01-01

    An analytical method is described for determining the residues of coplanar as well as mono-ortho substituted PCB congeners both exhibiting toxicological relevance, in foods of animal origin and in human milk. The unsophisticated procedure, convenient for routine analyses, includes the extraction of lipids, clean-up steps using liquid/liquid partition and column chromatography, fractionation of the congeners using HPLC on a special carbon column with an optimal gradient elution, and capillary column gas chromatography with electron capture or mass spectrometric detection. As preliminary results indicate, the low-chlorinated PCB technical products contribute more to the actual contamination of environment and foods than has been estimated so far. Obviously the co-planar congeners are accumulated during the food chain in a portion different from that found for the other congeners. (orig.)

  14. Ultra performance liquid chromatography-tandem mass spectrometry for the determination of amicarthiazol residues in soil and water samples.

    Science.gov (United States)

    Gui, Wen-jun; Tian, Jie; Tian, Chun-xia; Li, Shu-ying; Ma, You-ning; Zhu, Guo-nian

    2014-12-01

    A reliable and rapid method has been optimized to determine the residue of amicarthiazol in soil and environmental water samples. After extraction and evaporation, the extraction was carried out with solid phase extraction (SPE) cleanup using HLB cartridge (only soil samples) and for the quantitative determination by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The resulting residues of amicarthiazol were analyzed by a gradient separation performed on a UPLC system with a C18 column, methanol and water containing 0.1% (v v(-1)) formic acid as the mobile phase in the mode of electrospray positive ionization (ESI(+)) and multiple reaction monitoring (MRM). Results showed that the recoveries for spiked samples were 74.4-97.1% and 72.1-109.9% for soil and water, respectively, with the relative standard deviation (RSD) less than 10.2% when fortified at 10, 100 and 1000μgL(-1). The limits of detection (LODs) and the limits of quantification (LOQs) for matrix matched standards ranged from 0.073-0.425μgL(-1) and 0.243-1.42μgL(-1). The intra-day precision (n=5) and the inter-day precision over 10 days (n=10) for the amicarthiazol in soils and water samples spiked at 100μgL(-1) was 7.9% and 15.9%, respectively. Results indicated that the developed method could be a helpful tool for the controlling and monitoring of the risks posed by amicarthiazol to human health and environment safety. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Valuation of solid phase extraction disks in the determination of pesticide residues in surface and groundwater in Panama

    International Nuclear Information System (INIS)

    Jimenez, V.; Ramos de Jimenez, J.; Rojas, B.

    1999-01-01

    In Panama large quantities of pesticides are used in agriculture and livestock farming and there is increasing concern about their impact on public health and the environment. Chiriqui is the Province that registers the largest number of producers whose activities have impact on the environment, especially on surface and groundwater. Systematic monitoring programmes are non-existent due, in part, to the high cost of laboratory determination of environmental residues of pesticides. Within the framework of the FAO/IAEA/SIDA Coordinated Research Programme, efforts were focused on evaluating and optimising the use of solid phase extraction C 18 membrane disks in the analysis of surface and groundwater samples to determine pesticide residues. Factors studied were the effect of pre-washing and conditioning of the disks, flow rates, concentration level and matrix effects of field samples. Four pesticides, carbofuran, chlorothalonil, ametryn and chlorpyrifos were selected for these tests because preliminary analysis showed their presence in surface and groundwater. The technique significantly reduces the amount of organic solvents used as compared with the liquid-liquid extraction method. Quantifiable detection limits (Q L ) for the method were found to be 0.003 μg/L carbofuran, 0.016 μg/L chlorothalonil, 0.007 μg/L ametryn and 0.003 μg/L chlorpyrifos, when using standard spiked solutions. Recovery (%) was high when standard mixtures were used for the test runs but low when real surface water samples were tested, especially for chlorothalonil which was not recovered at all. (author)

  16. Validation of an efficient method for the determination of pesticide residues in fruits and vegetables using ethyl acetate for extraction.

    Science.gov (United States)

    Aysal, Perihan; Ambrus, Arpád; Lehotay, Steven J; Cannavan, Andrew

    2007-01-01

    In this study, a version of the "quick, easy, cheap, effective, rugged, and safe" (QuEChERS) method was modified to use ethyl acetate (EtOAc) rather than acetonitrile (MeCN) for extraction in the determination of multiple pesticide residues in fruits and vegetables. EtOAc is better suited than MeCN for gas chromatographic (GC) analysis with electron capture detection (ECD) and nitrogen-phosphorus detection (NPD). The method entailed extraction of 30 g chopped sample plus 5 g NaHCO(3) and 30 g anhydrous Na(2)SO(4) with 60 mL EtOAc using a probe blender. After a centrifugation step, removal of residual water and cleanup were performed using dispersive solid-phase extraction (dispersive-SPE) with MgSO(4) and primary secondary amine (PSA) sorbent. (14)C-labeled chlorpyrifos with liquid scintillation counting was used to assist in optimizing and characterizing the method, and GC-ECD and GC-NPD were used for analysis of 24 selected pesticides. The method was validated using tomato, apple and frozen green bean matrices spiked at 0.05, 0.5, and 5 mg/kg. For 22 of the analytes, recoveries averaged 93% for all three commodities over the validation range with a relative standard deviation of 10% (n = 1182). Lower recoveries of dichlorvos were obtained with the method and iprodione determination was compromised in the green beans by an interfering peak. Typical limits of detection were 0.005-0.01 mg/kg with the method.

  17. Study of Antioxidant Effectiveness of Kraft Lignin in HDPE

    Directory of Open Access Journals (Sweden)

    I. Piña

    2015-01-01

    Full Text Available Polymers are subject to oxidative degradation during all steps of their useful cycle. This degradative process is prevented using stabilizers like antioxidant of the type sterically hindered phenols or amines. Lignin, due to the presence of phenolic groups in their structure, can present characteristic as antioxidant agent, in a similar way to the additives used in polymers. Therefore, in this work, the antioxidant capacity of the lignin in a sample of polyethylene is studied. For this reason, in this paper, a method based on nonisothermal differential scanning calorimetry (DSC to evaluate this property is used. The samples studied were subjected to heat treatment at different scan rates and in presence of oxygen to promote thermooxidation of the material. The antioxidant capacity of different formulations of lignin and additives in the polymer resin was determined from the temperature of onset of oxidation (Ti at different heating rates and adjusting Arrhenius model prediction. The results indicate that the procedure can predict the antioxidant capacity of antioxidant additives in HDPE with good reproducibility and accuracy, according to the Arrhenius model prediction.

  18. Multifamily determination of pesticide residues in soya-based nutraceutical products by GC/MS-MS.

    Science.gov (United States)

    Páleníková, Agneša; Martínez-Domínguez, Gerardo; Arrebola, Francisco Javier; Romero-González, Roberto; Hrouzková, Svetlana; Frenich, Antonia Garrido

    2015-04-15

    An analytical method based on a modified QuEChERS extraction coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was evaluated for the determination of 177 pesticides in soya-based nutraceutical products. The QuEChERS method was optimised and different extraction solvents and clean-up approaches were tested, obtaining the most efficient conditions with a mixture of sorbents (PSA, C18, GBC and Zr-Sep(+)). Recoveries were evaluated at 10, 50 and 100 μg/kg and ranged between 70% and 120%. Precision was expressed as relative standard deviation (RSD), and it was evaluated for more than 160 pesticides as intra and inter-day precision, with values always below 20% and 25%, respectively. Limits of detection (LODs) ranged from 0.1 to 10 μg/kg, whereas limits of quantification (LOQs) from 0.5 to 20 μg/kg. The applicability of the method was proved by analysing soya-based nutraceuticals. Two pesticides were found in these samples, malathion and pyriproxyfen, at 11.1 and 1.5 μg/kg respectively. Copyright © 2014 Elsevier Ltd. All rights reserved.

  19. Determination of Sodium deoxycolate residues in vaccinal formulation by micellar electrokinetic chromatography

    International Nuclear Information System (INIS)

    Merchan, Yaima; Lucangioli, Silvia; Carducci, Clyde

    2011-01-01

    The sodium deoxycholate (DCNa) source is the surfactant used in the biopharmaceutical industry for the solubilization of outer membrane vesicles. It is well known the importance of control of this metabolite in biological materials due to its high toxicity for humans. To demonstrate significant small variations of this metabolite in vaccine formulations it is necessary to use a methodology highly selective, sensitive, specific and reproducible. In this report we used the micellar electrokinetic chromatography (MEKC) in a Capillary Ion Analyzer (Water corp. Milford MA) detection at 185 nm mercury lamp. It employed a fused silica capillary uncoated (Waters Corp. Milford MA). We assessed the purity of 2 lots of sodium deoxycholate and analyzed 15 samples of purified vesicles active pharmaceutical ingredient vaccine formulations. Data were recorded and processed with software Millennium TM (Waters Corp. Milford MA). It was found that lots of sodium deoxycholate containing 1.19 and 0.44% cholic acid and contaminate that 93% of the purified vesicles samples were from 0 to 2.44 mg protein DCNa/100 μg. MECK's results were compared with a kinetic test used to determine bile acids in blood (Merckotest). MECK system showed better results regarding the Merkotest

  20. Application of laser interferometry for assessment of surface residual stress by determination of stress-free state

    International Nuclear Information System (INIS)

    Kim, Dong Won; Kwon, Dong Il; Lee, Nak Kyu; Choi, Tae Hoon; Na, Kyoung Hoan

    2003-01-01

    The total relaxed stress in annealing and the thermal strain/stress were obtained from the identification of the residual stress-free state using Electronic Speckle Pattern Interferometry (ESPI). The residual stress fields in case of both single and film/substrate systems were modeled using the thermo-elastic theory and the relationship between relaxed stresses and displacements. We mapped the surface residual stress fields on the indented bulk Cu and the 0.5 μm Au film by ESPI. In indented Cu, the normal and shear residual stress are distributed over -1.7 GPa to 700 MPa and -800 GPa to 600 MPa respectively around the indented point and in deposited Au film on Si wafer, the tensile residual stress is uniformly distributed on the Au film from 500 MPa to 800 MPa. Also we measured the residual stress by the X-Ray Diffractometer (XRD) for the verification of above residual stress results by ESPI

  1. Nondestructive Determination of Cu Residue in Orange Peel by Laser Induced Breakdown Spectroscopy

    International Nuclear Information System (INIS)

    Hu Huiqin; Huang Lin; Liu Muhua; Chen Tianbing; Yang Ping; Yao Mingyin

    2015-01-01

    Laser induced breakdown spectroscopy (LIBS) is an emerging tool with rapid, nondestructive, green characteristics in qualitative or quantitative analyses of composition in materials. But LIBS has its shortcomings in detect limit and sensitivity. In this work, heavy metal Cu in Gannan Navel Orange, which is one of famous fruits from Jiangxi of China, was analyzed. In view of LIBS's limit, it is difficult to determinate heavy metals in natural fruits. In this work, nine orange samples were pretreated in 50-500 μg/mL Cu solution, respectively. Another one orange sample was chosen as a control group without any pollution treatment. Previous researchers observed that the content of heavy metals is much higher in peel than in pulp. So, the content in pulp can be reflected by detecting peel. The real concentrations of Cu in peels were acquired by atomic absorption spectrophotometer (AAS). A calibration model of Cu I 324.7 and Cu I 327.4 was constructed between LIBS intensity and AAS concentration by six samples. The correlation coefficient of the two models is also 0.95. All of the samples were used to verify the accuracy of the model. The results show that the relative error (RE) between predicted and real concentration is less than 6.5%, and Cu I 324.7 line has smaller RE than Cu I 327.4. The analysis demonstrated that different characteristic lines decided different accuracy. The results prove the feasibility of detecting heavy metals in fruits by LIBS. But the results are limited in treated samples. The next work will focus on direct analysis of heavy metals in natural fruits without any pretreatment. This work is helpful to explore the distribution of heavy metals between pulp and peel. (paper)

  2. Chapter 1: A Brief Introduction to Lignin Structure

    Energy Technology Data Exchange (ETDEWEB)

    Katahira, Rui [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Beckham, Gregg T [National Renewable Energy Laboratory (NREL), Golden, CO (United States); Elder, Thomas J. [USDA-Forest Service

    2018-04-03

    Lignin is an alkyl-aromatic polymer found in the cell walls of terrestrial plants. Lignin provides structure and rigidity to plants, is a natural, highly effective barrier against microbial attack, and enables water and nutrient transport through plant tissues. Depending on the plant species, the constituents of lignin can vary considerably, leading to substantial diversity in lignin chemistry and structure. Despite nearly a century of research and development attempting to convert lignin into valuable products, lignin in most current and planned biorefinery contexts remains underutilized, most often being burned to generate heat and power. However, the drive towards effective lignin valorization processes has witnessed a significant resurgence in the past decade, catalyzed by advances in improved understanding of lignin chemistry, structure, and plasticity in parallel with new catalytic and biological approaches to valorize this important, prevalent biopolymer. As a preface to the subsequent chapters in this book, this chapter briefly highlights the known aspects of lignin structure.

  3. Multiphase materials with lignin. VI. Effect of cellulose derivative structure on blend morphology with lignin

    Science.gov (United States)

    Timothy G. Rials; Wolfgang G. Glasser

    1989-01-01

    Polymeric blends of lignin with ethyl cellulose (EC) and cellulose acetate/butyrate (CAB) prepared by solution casting from dioxane. Fracture surface analysis by scanning electron microscopy revealed phase separation when the lignin content exceeded 10% for blends with EC and 5% in the CAB system. While this phase behavior is as predicted for the EC blends, a greater...

  4. Chemical modifiers for direct determination of cobalt in coal combustion residues by ultrasonic slurry-sampling-ETAAS

    Energy Technology Data Exchange (ETDEWEB)

    Felipe-Sotelo, M.; Carlosena, A.; Fernandez, E.; Lopez-Mahia, P.; Muniategui, S.; Prada, D. [Dept. of Analytical Chemistry, Univ. of La Coruna (Spain)

    2001-12-01

    Five modifiers were tested for the direct determination of cobalt in coal fly ash and slag by ultrasonic slurry-sampling electrothermal atomic absorption spectrometry (USS-ETAAS).The furnace temperature programs and the appropriate amount for each modifier were optimized to get the highest signal and the best separation between the atomic and background signals. Nitric acid (0.5% v/v) was the most adequate chemical modifier for cobalt determination, selecting 1450 C and 2100 C as pyrolysis and atomization temperatures, respectively. This modifier also acts as liquid medium for the slurry simplifying the procedure. The remaining modifiers enhanced the background signal, totally overlapped with cobalt peak. The method optimized gave a limit of detection of 0.36 {mu}g g{sup -1}, a characteristic mass of 13{+-}1 pg and an overall-method precision which is highly satisfactory (<7%, RSD). The method was validated by analyzing two certified coal fly ash materials, and satisfactory recoveries were obtained (83-90%) and no statistical differences were observed between the experimental and the certified cobalt concentrations. Additionally, certified sediment, soil and urban particulate matter were assayed; again good results were obtained. The developed methodology was used to determine cobalt in several coal combustion residues from five Spanish power plants. (orig.)

  5. Systematic Parameterization of Lignin for the CHARMM Force Field

    Energy Technology Data Exchange (ETDEWEB)

    Vermaas, Joshua; Petridis, Loukas; Beckham, Gregg; Crowley, Michael

    2017-07-06

    Plant cell walls have three primary components, cellulose, hemicellulose, and lignin, the latter of which is a recalcitrant, aromatic heteropolymer that provides structure to plants, water and nutrient transport through plant tissues, and a highly effective defense against pathogens. Overcoming the recalcitrance of lignin is key to effective biomass deconstruction, which would in turn enable the use of biomass as a feedstock for industrial processes. Our understanding of lignin structure in the plant cell wall is hampered by the limitations of the available lignin forcefields, which currently only account for a single linkage between lignins and lack explicit parameterization for emerging lignin structures both from natural variants and engineered lignin structures. Since polymerization of lignin occurs via radical intermediates, multiple C-O and C-C linkages have been isolated , and the current force field only represents a small subset of lignin the diverse lignin structures found in plants. In order to take into account the wide range of lignin polymerization chemistries, monomers and dimer combinations of C-, H-, G-, and S-lignins as well as with hydroxycinnamic acid linkages were subjected to extensive quantum mechanical calculations to establish target data from which to build a complete molecular mechanics force field tuned specifically for diverse lignins. This was carried out in a GPU-accelerated global optimization process, whereby all molecules were parameterized simultaneously using the same internal parameter set. By parameterizing lignin specifically, we are able to more accurately represent the interactions and conformations of lignin monomers and dimers relative to a general force field. This new force field will enables computational researchers to study the effects of different linkages on the structure of lignin, as well as construct more accurate plant cell wall models based on observed statistical distributions of lignin that differ between

  6. Biological treatment of crop residues for ruminant feeding: A review ...

    African Journals Online (AJOL)

    Crop residues are often referred to as 'lignocellulosics' as they are rich in cellulose which is bound with a biopolymer lignin. Rumen microbiota (bacteria, protozoa and fungi), even with their hydrolytic enzymes, are not very competent enough to break these bonds efficiently. Biological treatment of such crop residues using ...

  7. Studies on polyphenols and lignin of Astronium urundeuva wood

    Directory of Open Access Journals (Sweden)

    Morais Sérgio A.L.

    1999-01-01

    Full Text Available An Astronium urundeuva ball-milled wood sample was successively extracted with benzene, benzene-ethanol (2:1, v/v-1, chloroform, and water in a soxhlet apparatus. The extracted wood was air-dried giving the residue A that was then treated with ketone-water (9:1, in a soxhlet apparatus. From the ketone-water extract was precipitated the milled wood lignin (MWL. With exception of MWL, the extract contents summed up 18.19% (o.d.w.. The Klason lignin content of A and the methoxyl content of the MWL were 23.84% and 19.00%, respectively. Another sample of A gave hardly and easily hydrolysable polysaccharide contents of 34.86% and 18.81%, respectively. A second sample of ball-milled wood was submitted to a single extraction with methanol, at room temperature, affording the methanol extract B (23.85% o.d.w.. Liquid and solid state 13C-NMR spectroscopies indicated that B is mainly constituted by proanthocyanidins of profisetinidin and prorobinetidin types.

  8. Molecular Determinants Underlying Binding Specificities of the ABL Kinase Inhibitors: Combining Alanine Scanning of Binding Hot Spots with Network Analysis of Residue Interactions and Coevolution

    Science.gov (United States)

    Tse, Amanda; Verkhivker, Gennady M.

    2015-01-01

    Quantifying binding specificity and drug resistance of protein kinase inhibitors is of fundamental importance and remains highly challenging due to complex interplay of structural and thermodynamic factors. In this work, molecular simulations and computational alanine scanning are combined with the network-based approaches to characterize molecular determinants underlying binding specificities of the ABL kinase inhibitors. The proposed theoretical framework unveiled a relationship between ligand binding and inhibitor-mediated changes in the residue interaction networks. By using topological parameters, we have described the organization of the residue interaction networks and networks of coevolving residues in the ABL kinase structures. This analysis has shown that functionally critical regulatory residues can simultaneously embody strong coevolutionary signal and high network centrality with a propensity to be energetic hot spots for drug binding. We have found that selective (Nilotinib) and promiscuous (Bosutinib, Dasatinib) kinase inhibitors can use their energetic hot spots to differentially modulate stability of the residue interaction networks, thus inhibiting or promoting conformational equilibrium between inactive and active states. According to our results, Nilotinib binding may induce a significant network-bridging effect and enhance centrality of the hot spot residues that stabilize structural environment favored by the specific kinase form. In contrast, Bosutinib and Dasatinib can incur modest changes in the residue interaction network in which ligand binding is primarily coupled only with the identity of the gate-keeper residue. These factors may promote structural adaptability of the active kinase states in binding with these promiscuous inhibitors. Our results have related ligand-induced changes in the residue interaction networks with drug resistance effects, showing that network robustness may be compromised by targeted mutations of key mediating

  9. pH-Induced Lignin Surface Modification to Reduce Nonspecific Cellulase Binding and Enhance Enzymatic Saccharification of Lignocelluloses

    Science.gov (United States)

    Hongming Lou; J.Y. Zhu; Tian Qing Lan; Huranran Lai; Xueqing Qiu

    2013-01-01

    We studied the mechanism of the significant enhancement in the enzymatic saccharification of lignocelluloses at an elevated pH of 5.5–6.0. Four lignin residues with different sulfonic acid contents were isolated from enzymatic hydrolysis of lodgepole pine pretreated by either dilute acid (DA) or sulfite pretreatment to overcome recalcitrance of lignocelluloses (SPORL...

  10. Effect of lignin derivatives in the bio-polyols from microwave liquefied bamboo on the properties of polyurethane foams

    Science.gov (United States)

    Jiulong Xie; Jinqiu Qi; Chung-Yun Hse; Todd F. Shupe

    2014-01-01

    Bamboo residues were subjected to a microwave-assisted liquefaction process for the production of crude bio-polyols (CBP). The fractionated bio-polyols (FBP) were obtained by the removal of lignin derivatives from the crude bio-polyols (CBP) using a simple method. Polyurethane (PU) foams were successfully prepared from both CBP and FBP. The object of this study was to...

  11. Use of mass spectrometry methods as a strategy for detection and determination of residual solvents in pharmaceutical products.

    Science.gov (United States)

    Pérez Pavón, José Luis; del Nogal Sanchez, Miguel; García Pinto, Carmelo; Fernandez Laespada, M Esther; Moreno Cordero, Bernardo

    2006-07-15

    In the present work a strategy for the qualitative and quantitative analysis of residual solvents in pharmaceutical products is reported. First, a low-resolution chromatogram is generated for the identification of the solvents present in the samples by means of headspace generation-fast gas chromatography-mass spectrometry (HS-fast GC/MS). From the plotting of this information by means of contour plots with time and mass/charge axes, it is decided whether quantification of such compounds can be accomplished without chromatographic separation or whether it should be done by fast gas chromatography. The nonseparative method is based on direct coupling of a headspace sampler with a mass spectrometer (HS-MS) and requires a signal recording time of only 3 min, while with fast gas chromatography the time required to obtain a chromatogram is 7.16 min. The use of headspace generation for introducing the sample and standard addition as a quantification technique provided satisfactory results and minimized the matrix effect. An important advantage of the methodologies used here is related to the fact that no prior treatment of the sample is required, thus minimizing the creation of analytical artifacts and the errors associated with this step of the analytical process. The methods were applied to the determination of residual solvents in 27 different pharmaceutical products. Detection and quantitation limits were sufficiently low to enable the estimation of organic volatile impurities according to the International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use.

  12. Thermal desorption extraction proton transfer reaction mass spectrometer (TDE-PTR-MS) for rapid determination of residual solvent and sterilant in disposable medical devices.

    Science.gov (United States)

    Wang, Yujie; Shen, Chengyin; Li, Jianquan; Wang, Hongmei; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2011-07-15

    Thermal desorption extraction proton transfer reaction mass spectrometer (TDE-PTR-MS) has been exploited to provide rapid determination of residual solvent and sterilant like cyclohexanone (CHX) and ethylene oxide (EO) in disposable medical devices. Two novel methods are proposed for the quantification of residual chemicals in the polyvinyl chloride infusion sets with our homemade PTR-MS. In the first method, EO residue in the solid infusion sets (y, mgset(-1)) is derived through the determination of EO gas concentration within its packaging bag (x, ppm) according to the correlative equation of y=0.00262x. In the second one, residual EO and CHX in the solid infusion sets are determined through a time integral of their respective mass emission rates. The validity of the proposed methods is demonstrated by comparison with the experimental results from the exhaustive extraction method. Due to fast response, absolute concentration determination and high sensitivity, the TDE-PTR-MS is suggested to be a powerful tool for the quality inspection of disposable medical devices including the quantitative determination of residual solvent and sterilant like CHX and EO. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Residue-specific pK(a) determination of lysine and arginine side chains by indirect N-15 and C-13 NMR spectroscopy : Application to apo calmodulin

    NARCIS (Netherlands)

    Andre, Ingemar; Linse, Sara; Mulder, Frans A. A.

    2007-01-01

    Electrostatic interactions in proteins can be probed experimentally through determination of residue-specific acidity constants, We describe here triple-resonance NMR techniques for direct determination of lysine and arginine side-chain protonation states in proteins. The experiments are based on

  14. Determination of quinolone residues in tilapias (Orechromis niloticus) by HPLC-FLD and LC-MS/MS QToF.

    Science.gov (United States)

    Paschoal, J A R; Reyes, F G R; Rath, S

    2009-10-01

    A method for the simultaneous determination of flumequine, oxolinic acid, sarafloxacin, danofloxacin, enrofloxacin, and ciprofloxacin in tilapia (Orechromis niloticus) fillet, using high-performance liquid chromatography with fluorescence detection (HPLC-FLD) is presented. The quinolones were extracted from the food matrix with a solution of 10% trichloroacetic acid and methanol (80:20 v/v). Clean-up of the extract was performed using polymeric solid-phase extraction cartridges. Identification of the quinolones was confirmed by liquid chromatography-tandem mass spectrometry. The HPLC-FLD method was validated in-house and the following analytical parameters were obtained: linearity higher than 0.99 for all the quinolones; intra- and interassay precisions were lower than 3.5% and 10.9%, respectively; and recoveries ranged from 73% to 110%. The limit of quantification was below the maximum residue limit established by the Joint Expert Committee on Food Additives (JECFA), which indicates that the method is appropriate for the determination of quinolones in fish fillet.

  15. Validation of LED spectrofluorimeter for determination of both biodiesel and nontransesterified residual cooking oil in diesel samples

    Science.gov (United States)

    Meira, Marilena; Quintella, Cristina M.; Costa Neto, Pedro Ramos; Pepe, Iuri M.; Ribeiro, Erika M. de O.; Silva, Weidson Leal; Cid, Alexandre Lopes Del; Guimarães, Alexandre Kamei

    2015-02-01

    This paper presents the results of the validation of a LED spectrofluorimeter patented for the analysis of biodiesel in diesel and non-transesterified residual cooking oil (RCO) in diesel. Detection limit, quantification limit and sensitivity were determined from the regression lines. The spectrofluorimeter validated in this study was adequate for quantifying the amount of biodiesel in diesel in the range from 2% to 45% (B02-B45) with an R-squared value of 0.9962 and a detection limit of 3%. For the analysis of non-transesterified RCO in diesel, the linear range was from 2% to 20% with an R-squared value of 0.9872 and a detection limit of 2%. The accuracy of the equipment for the analysis of biodiesel in diesel and non-transesterified RCO in diesel was evaluated using Student's t-test for paired data. With 95% confidence level there was no significant difference between the actual values and those determined by the equipment.

  16. Optimization of a method by liquid chromatography of high resolution to determine residues of ethilenthiourea in samples of tomato

    International Nuclear Information System (INIS)

    Mora, D.; Rodriguez, O.M.

    2002-01-01

    A method was optimized to determine the present residues of ethilenthiourea in samples of tomatoes. The method consisted of three stages: a extraction of ultrasonic bath with methanol; a cleaning of the extract through a glass column of 11 mm of diameter stuffed with 2,5 g of neutral aluminium's mixture and activated coal (97,5:2,5) and 2,5 g of pure-neutral aluminium, it is dissolved with 250 ml of methanol. The third stage was of quantification by HPLC in a C 18 ' column with a methanol and water mixture (90:10) like a mobile phase to an flow of 2,0 ml/min. and with UV detection to 232 nm. The retention's time under theses conditions was of 2,15 minutes. The merit's parameters of the method were determined, proving and lineal sphere between 1,0 and 28,0 (g/ml of ETU; some quantification and detection limits have been calculated by the method of Hubaux and Vos (22) of 0,153 and 0,306 mg/ml respectively and a recuperation of 84%. (Author) [es

  17. The essential role of the sialic acid residues for IFN-β1a activity determined in vivo

    DEFF Research Database (Denmark)

    Olesen, Lasse Dissing; Andersen, Morten Thaysen

    the function of the rhIFN-β1a glycan moiety and its individual carbohydrate residues using the myxovirus resistance (Mx) mRNA as a biomarker in Mx-congenic mice. We showed that the Mx mRNA level in blood leukocytes peaked three hours after subcutaneous administration of rhIFN-β1a. In addition, a clear dose......-response relationship was confirmed and the Mx response was shown to be receptor mediated. Using specific glycosidases, different glycosylation analogs of rhIFN-β1a were obtained and their activities determined. The glycosylated rhIFN-β1a showed significantly higher activity than its deglycosylated counterpart, due...... to a protein stabilization/solubilization effect of the glycan. Interestingly, the terminating sialic acids were essential for these effects. Conclusively, the structure/bioactivity relationship of rhIFN-β1a was determined in vivo and provided a novel insight into the role of the rhIFN-β1a glycan and its...

  18. Determination of organophosphorus pesticides and their major degradation product residues in food samples by HPLC-UV.

    Science.gov (United States)

    Peng, Guilong; He, Qiang; Lu, Ying; Mmereki, Daniel; Zhong, Zhihui

    2016-10-01

    A simple method based on dispersive solid-phase extraction (DSPE) and dispersive liquid-liquid microextraction method based on solidification of floating organic droplets (DLLME-SFO) was developed for the extraction of chlorpyrifos (CP), chlorpyrifos-methyl (CPM), and their main degradation product 3,5,6-trichloro-2-pyridinol (TCP) in tomato and cucumber samples. The determination was carried out by high performance liquid chromatography with ultraviolet detection (HPLC-UV). In the DSPE-DLLME-SFO, the analytes were first extracted with acetone. The clean-up of the extract by DSPE was carried out by directly adding activated carbon sorbent into the extract solution, followed by shaking and filtration. Under the optimum conditions, the proposed method was sensitive and showed a good linearity within a range of 2-500 ng/g, with the correlation coefficients (r) varying from 0.9991 to 0.9996. The enrichment factors ranged from 127 to 138. The limit of detections (LODs) were in the range of 0.12-0.68 ng/g, and the relative standard deviations (RSDs) for 50 ng/g of each analytes in tomato samples were in the range of 3.25-6.26 % (n = 5). The proposed method was successfully applied for the extraction and determination of the mentioned analytes residues in tomato and cucumber samples, and satisfactory results were obtained.

  19. Development of direct competitive biomimetic immunosorbent assay based on quantum dot label for determination of trichlorfon residues in vegetables.

    Science.gov (United States)

    Liu, Qiurui; Jiang, Mingdi; Ju, Zeliang; Qiao, Xuguang; Xu, Zhixiang

    2018-06-01

    A direct competitive biomimetic immunosorbent assay method based on molecularly imprinted polymer was developed for the determination of trichlorfon. A CdSe/ZnS quantum dot label was used as the marker. The hydrophilic imprinted film was synthesized directly on the surface of a 96-well plate, and characterized by Fourier-transform infrared spectroscopy and thermo-gravimetric analyses. The method exhibited high stability, selectivity, and sensitivity. Under optimal conditions, the limits of detection and sensitivity of the biomimetic immunosorbent assay method were 9.0 μg L -1 and 5.0 mg L -1 (0.1 mg kg -1 and 62.5 mg kg -1 for vegetable sample), respectively. Low cross-reactivity values of 19.2% and 15.6% were obtained for the structural analogues. Spinach and rape samples spiked with trichlorfon were extracted and determined by this method with recoveries ranging from 83.6% to 91.1%. The method was applied for the detection of trichlorfon residues in leek and cucumber samples, and results correlated well with those obtained using GC. Copyright © 2018 Elsevier Ltd. All rights reserved.

  20. Determination of alkylphenol residues in baby-food purees by steam distillation extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Li, Chia-Tien; Cheng, Chin-Yuan; Ding, Wang-Hsien

    2008-02-01

    This paper describes a simple and sensitive method for determining alkylphenols namely 4-tert-octylphenol (4-t-OP) and the isomers of 4-nonylphenol (4-NPs) present in various types of baby-food purees. The method involves extracting a sample with n-hexane for 1h using a modified Nielson-Kryger steam distillation extraction system and then identifying and quantitating the alkylphenols using a gas chromatography-mass spectrometry (GC-MS) operated in the selected ion monitoring (SIM) mode. The extraction conditions were evaluated at various values of pH of the sample solution. The limits of quantitation for this method were 0.2 ng/g from 1.0 g (wet weight) samples of 4-t-OP and the 4-NPs. The intra- and interbatch precisions and accuracies were also determined. The precision, in terms of the relative standard deviation (RSD), were less than 8%. Most of the recoveries of the alkylphenols from various spiked samples exceeded 60%, while the values of RSD ranged from 1% to 10%. Alkylphenol residues were detected in baby-food purees at concentrations of up to 19 ng/g (wet weight) for 4-t-OP and up to 21 ng/g (wet weight) for the 4-NPs.

  1. Rapid gas chromatographic method for the determination of famoxadone, trifloxystrobin and fenhexamid residues in tomato, grape and wine samples.

    Science.gov (United States)

    Likas, D T; Tsiropoulos, N G; Miliadis, G E

    2007-05-25

    Trifloxystrobin, fenhexamid and famoxadone belong to the generation of fungicides acting against a broad spectrum of fungi and widely used in Integrated Pest Management strategies in different agricultural crops but mainly in viticulture. In the present work, a gas chromatographic (GC) method for their determination was developed and validated on tomato, grape and wine matrices. The method was based on a simple one step liquid-liquid microextraction with cyclohexane/dichloromethane (9+1, v/v) and determination of fungicides by gas chromatography with nitrogen phosphorous (NP-) and electron capture (EC-) detection, and ion trap mass spectrometry (ITMS) for confirmation. The method was validated by recovery experiments, assessment of matrix effect and calculation of the associated uncertainty. Recoveries for GC-NPD and GC-ECD were found in the range of 81-102% with RSD NPD, respectively, depending on the sensitivity of each compound with trifloxystrobin being the most sensitive. The expanded uncertainty, calculated for a sample concentration of 0.10 mg/kg, ranged from 4.8 to 13% for the GC-ECD and from 5.4 to 29% for the GC-NPD. The concentration levels for famoxadone residues found in tomato and grape samples from field experiments were clearly below the EU established MRL values, thus causing no problems in terms of food safety.

  2. Fast pyrolysis of lignin, macroalgae and sewage sludge

    DEFF Research Database (Denmark)

    Trinh, Ngoc Trung

    is available in the literature. Nonconventional biomass feedstock may also be applicable for fast pyrolysis processes. Among the forms of nonconventional biomasses: macroalgae, lignin (industrial residue) and sewage sludge may be attractive materials due to their low price, non-competitiveness with food crops......In the last twenty years, the fast pyrolysis process has been explored to produce bio-oil from biomass. Fast pyrolysis is a thermal conversion technology that is performed at a temperatures of 450 - 600 ºC, high biomass heating ratess (100 - 2000 K/s), a short gas residence time (less than 2 s......) with no presence of oxygen. Fast pyrolysis can convert a large fraction of the biomass to bio-oil, and smaller fractions of char and gas. The pyrolysis centrifuge reactor (PCR) has been developed at the CHEC center at DTU Department of Chemical Engineering. The reactor is a compact design that uses a low flow rate...

  3. Lignin Films from Spruce, Eucalyptus, and Wheat Straw Studied with Electroacoustic and Optical Sensors: Effect of Composition and Electrostatic Screening on Enzyme Binding.

    Science.gov (United States)

    Pereira, Antonio; Hoeger, Ingrid C; Ferrer, Ana; Rencoret, Jorge; Del Rio, José C; Kruus, Kristiina; Rahikainen, Jenni; Kellock, Miriam; Gutiérrez, Ana; Rojas, Orlando J

    2017-04-10

    Lignins were isolated from spruce, wheat straw, and eucalyptus by using the milled wood lignin (MWL) method. Functional groups and compositional analyses were assessed via 2D NMR and 31 P NMR to realize their effect on enzyme binding. Films of the lignins were fabricated and ellipsometry, atomic force microscopy, and water contact angle measurements were used for their characterization and to reveal the changes upon enzyme adsorption. Moreover, lignin thin films were deposited on quartz crystal microgravimetry (QCM) and surface plasmon (SPR) resonance sensors and used to gain further insights into the lignin-cellulase interactions. For this purpose, a commercial multicomponent enzyme system and a monocomponent Trichoderma reesei exoglucanase (CBH-I) were considered. Strong enzyme adsorption was observed on the various lignins but compared to the multicomponent cellulases, CBH-I displayed lower surface affinity and higher binding reversibility. This resolved prevalent questions related to the affinity of this enzyme with lignin. Remarkably, a strong correlation between enzyme binding and the syringyl/guaiacyl (S/G) ratio was found for the lignins, which presented a similar hydroxyl group content ( 31 P NMR): higher protein affinity was determined on isolated spruce lignin (99% G units), while the lowest adsorption occurred on isolated eucalyptus lignin (70% S units). The effect of electrostatic interactions in enzyme adsorption was investigated by SPR, which clearly indicated that the screening of charges allowed more extensive protein adsorption. Overall, this work furthers our understanding of lignin-cellulase interactions relevant to biomass that has been subjected to no or little pretreatment and highlights the widely contrasting effects of the nature of lignin, which gives guidance to improve lignocellulosic saccharification and related processes.

  4. Esterification and characterization of lignin aiming the synthesis of polymeric composite; Esterificacao e caracterizacao da lignina visando a sintese de compositos polimericos

    Energy Technology Data Exchange (ETDEWEB)

    Victor, Priscilla A.; Machado, Fabricio, E-mail: fmachado@unb.br [Universidade de Brasilia (UnB), DF (Brazil). Instituto de Quimica; Goncalves, Silvia B., E-mail: silvia.belem@embrapa.br [Embrapa Agroenergia, Parque Estacao Biologica (PqEB), Brasilia, DF (Brazil)

    2015-07-01

    Lignin is a natural polymer derived from lignocellulosic materials with high availability, presenting a huge potential for production of new materials. Due to its complex macromolecular structure, and its low compatibility with styrene, eucalyptus wood-extracted lignin method was esterified with methacrylic anhydride - exhibiting a yield of 64% - in order to ensure homogeneity in the organic phase into the reaction medium. The evaluation of both the natural and esterified lignin through infrared (IR) spectroscopy showed a decrease of the hydroxyl band, characteristic of natural lignin (3200-3400 cm{sup -1}) and an increase of the characteristic ester band (1720 to 1740 cm{sup -1}). According to nuclear magnetic resonance ({sup 1}H NMR) analysis on esterified lignin, intense peaks were observed in the range from 1.7 to 2.05 ppm (-CH{sub 3}) and 5.4 ppm to 6.2 ppm (=CH{sub 2}), related to methacrylic anhydride. According to the thermogravimetric analysis (TGA), the esterified lignin showed a decrease in its thermal stability when compared to natural lignin, exhibiting two main weight losses between 200 °C and 300 °C and in the interval from 550 °C to 800 °C. Comparatively, the esterified lignin also displayed an increase in its glass transition temperature (Tg = 98 °C) for, when compared to natural lignin, whose Tg value was determined to be equal to 91 °C. (author)

  5. A Novel Enterovirus 71 (EV71) Virulence Determinant: The 69th Residue of 3C Protease Modulates Pathogenicity.

    Science.gov (United States)

    Li, Bingqing; Yue, Yingying; Zhang, Yajie; Yuan, Zenglin; Li, Peng; Song, Nannan; Lin, Wei; Liu, Yan; Gu, Lichuan; Meng, Hong

    2017-01-01

    Human enterovirus type 71 (EV71), the major causative agent of hand-foot-and-mouth disease, has been known to cause fatal neurological complications. Unfortunately, the reason for neurological complications that have been seen in fatal cases of the disease and the relationship between EV71 virulence and viral genetic sequences remains largely undefined. The 3C protease (3C pro ) of EV71 plays an irreplaceable role in segmenting the precursor polyprotein during viral replication, and intervening with host life activity during viral infection. In this study, for the first time, the 69th residue of 3C protease has been identified as a novel virulence determinant of EV71. The recombinant virus with single point variation, in the 69th of 3C pro , exhibited obvious decline in replication, and virulence. We further determined the crystal structure of 3C N69D at 1.39 Ǻ resolution and found that conformation of 3C N69D demonstrated significant changes compared with a normal 3C protein, in the substrate-binding site and catalytic active site. Strikingly, one of the switch loops, essential in fixing substrates, adopts an open conformation in the 3C N69D-rupintrivir complex. Consistent with this apparent structural disruption, the catalytic activity of 3C N69D decreased sharply for host derived and viral derived substrates, detected for both in vitro and in vivo . Interestingly, in addition to EV71, Asp69 was also found in 3C proteases of other virus strains, such as CAV16, and was conserved in nearly all C type human rhinovirus. Overall, we identified a natural virulence determinant of 3C protease and revealed the mechanism of attenuated virulence is mediated by N69D substitution. Our data provides new insight into the enzymatic mechanism of a subdued 3C protease and suggests a theoretical basis for virulence determinantion of picornaviridae.

  6. [Determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes by gas chromatography-tandem mass spectrometry].

    Science.gov (United States)

    Zhang, Qun; Liu, Chunhua; Wu, Nancun; Wu, Xiaofang; Li, Shuhuai

    2014-08-01

    An analytical method was established for the determination of propargite, tebuconazole and bromopropylate in Taiwan green jujubes (Zizyphus mauritiana Lam) by gas chromatography-tandem mass spectrometry (GC-MS/MS). The sample was extracted with acetonitrile from the Taiwan green jujubes after treated with a homogenizer. The organic phase was then separated from water phase by adding NaCl. The extract was further purified on a carbon/ NH2 cartridge with elution solvents of acetonitrile/toluene (3:1, v/v). Finally, the target analytes were separated by a capillary gas chromatographic column SLB-5MS (30 m x 0. 25 mm x 0. 25 μm). A tandem quadrupole mass spectrometer operated in either full scan mode or in MS/MS mode for multiple reaction monitoring (MRM) was used for the qualitative and quantitative analysis of the constituents, respectively. The results showed that the average recoveries of the three pesticides ranged from 75. 8% to 103. 6% with the RSDs of 1. 7%-9. 3% at the spiking levels from 0.01 mg/kg to 0. 50 mg/kg (n= 5). The calibration curves showed good linearity in the range of 0.01-0.50 mg/kg, with the determination coefficients over 0.99 (R2>0.99). The limits of quantification (LOQs) were 0.01 mg/kg for propargite, tebuconazole and bromopropylate in Taiwan green jujubes. The method is available for the determination of propargite, tebuconazole and bromopropylate pesticide residues in Taiwan green jujubes.

  7. New techniques for the characterization of lignins

    International Nuclear Information System (INIS)

    Javor, T.

    2001-09-01

    In the present work new techniques for the characterization of lignins, ligninsulfonates as well as lignin degradation products with capillary electrophoresis (CE), size exclusion chromatography (SEC) and mass spectrometry (ESI-MS, APCI-MS and MALDI-MS) are described. After an overview on wood and wood pulping the development of microemulsion electrokinetic chromatography (MEEKC) for the investigation of low-molecular-mass lignin degradation compounds is described. This method is suited for the analysis of phenolic compounds as well as for non-phenolic compounds in this kind of samples. Using a carrier electrolyte system consisting of 1-butanol/n-heptane/sodiumdodeylsulfate (SDS)/20 mM borate (6.61/0.81/1.66/90,29 % (w/w)) pH 9.2 it was possible to separate 14 lignin degradation compounds (2-methoxyphenol, 3,4,5-trimethoxyphenol, 2,6-dimethoxyphenol, 3,4-dimethoxybenzaldehyde, 3,4-dimethoxyacetophenone, 3,4,5-trimethoxybenzaldehyde, 3,4,5-trimethoxyacetophenone, 3-(3,4-dimethoxyphenyl)-2-propen-1-ol, 4-methoxyacetophenone, 3,5-Dimethoxy-4-hydroxyacetophenone, acetovanillone, syringaldehyde, vanillin, 4-hydroxybenzaldehyde and 1-(3-methoxy-4-hydroxyphenyl)-2-(2-methoxyphenoxy)-ethanol). In addition the advantages and disadvantages of microemulsions are discussed in comparison with carrier electrolytes containing micelles. Subsequently, the results from size exclusion chromatographic measurements are presented. SEC using modern high-performance poly(styrene-divinylbenzene) gels as stationary phase and 0.1 M NaOH as mobile phase allows efficient separations and good characterization of lignins and ligninsulfonates. Adsorption effects are practical negligible. SEC yields results which are independent of the charge of lignins or ligninsulfonates, so that this technique looks complementary to capillary electrophoresis. For the characterization of intact lignins and ligninsulfonates by capillary zone electrophoretic techniques, carrier electrolytes in the the pH range 10

  8. Mechanochemical Lignin-Mediated Strecker Reaction

    Directory of Open Access Journals (Sweden)

    Saumya Dabral

    2017-01-01

    Full Text Available A mechanochemical Strecker reaction involving a wide range of aldehydes (aromatic, heteroaromatic and aliphatic, amines, and KCN afforded a library of α-aminonitriles upon mechanical activation. This multicomponent process was efficiently activated by lignocellulosic biomass as additives. Particularly, commercially available Kraft lignin was found to be the best activator for the addition of cyanide to the in situ formed imines. A comparative study of the 31P-NMR (Nuclear Magnetic Resonance along with IR (Infrared data analysis for the Kraft lignin and methylated Kraft lignin samples ascertained the importance of the free hydroxyl groups in the activation of the mechanochemical reaction. The solvent-free mechanochemical Strecker reaction was then coupled with a lactamization process leading to the formation of the N-benzylphthalimide (5a and the isoindolinone derivative 6a.

  9. Incorporation of Epicatechin Esters into Lignin Enhances Cell Wall Fermentability

    Science.gov (United States)

    Polyphenolic catechin esters are potentially attractive targets for lignin bioengineering because their copolymerization with monolignols could reduce lignin hydrophobicity and cross-linking to polysaccharides, or facilitate delignification by biomass pretreatments. To test this hypothesis, we biomi...

  10. Fiber and lignin analysis in concentrate, forage, and feces

    DEFF Research Database (Denmark)

    Hindrichsen, I.K.; Kreuzer, M.; Madsen, Jørgen

    2006-01-01

    Hemicelluloses, cellulose, and lignin contents of contrasting feeds, with emphasis on concentrate ingredients and complete concentrates, were analyzed using the Van Soest detergent procedure (analyzing neutral detergent fiber, acid detergent fiber, and acid detergent lignin) and the enzymatic...

  11. Fiber and lignin analysis in concentrate, forage, and feces

    DEFF Research Database (Denmark)

    Hindrichsen, I.K.; Kreuzer, M.; Madsen, Jørgen

    2006-01-01

    Hemicelluloses, cellulose, and lignin contents of contrasting feeds, with emphasis on concentrate ingredients and complete concentrates, were analyzed using the Van Soest detergent procedure (analyzing neutral detergent fiber, acid detergent fiber, and acid detergent lignin) and the enzymatic-che...

  12. Anaerobic biodegradation of the lignin and polysaccharide components of lignocellulose and synthetic lignin by sediment microflora

    Energy Technology Data Exchange (ETDEWEB)

    Benner, R.; Maccubbin, A.E.; Hodson, R.E.

    1984-05-01

    Specifically radiolabeled (/sup 14/C-lignin)lignocelluloses and (/sup 14/C-polysaccharide)lignocelluloses were prepared from a variety of marine and freshwater wetland plants including a grass, a sedge, a rush, and a hardwood. These (/sup 14/C)lignocellulose preparations and synthetic (/sup 14/C)lignin were incubated anaerobically with anoxic sediments collected from a salt marsh, a freshwater marsh, and a mangrove swamp. During long-term incubations lasting up to 300 days, the lignin and polysaccharide components of the lignocelluloses were slowly degraded anaerobically to /sup 14/CO/sub 2/ and /sup 14/CH/sub 4/. Lignocelluloses derived from herbaceous plants were degraded more rapidly than lignocellulose derived from the hardwood. After 294 days, 16.9% of the lignin component and 30.0% of the polysaccharide component of lignocellulose derived from the grass used (Spartina alterniflora) were degraded to gaseous end products. In contrast, after 246 days, only 1.5% of the lignin component and 4.1% of the polysaccharide component of lignocellulose derived from the hardwood used (Rhizophora mangle) were degraded to gaseous end products. Synthetic (/sup 14/C) lignin was degraded anaerobically faster than the lignin component of the hardwood lignocellulose; after 276 days 3.7% of the synthetic lignin was degraded to gaseous end products. Contrary to previous reports, these results demonstrate that lignin and lignified plant tissues are biodegradable in the absence of oxygen. Although lignocelluloses are recalcitrant to anaerobic biodegradation, rates of degradation measured in aquatic sediments are significant and have important implications for the biospheric cycling of carbon from these abundant biopolymers. 31 references.

  13. Determination of the residues of 18 carbamate pesticides in chestnut and pine nut by GPC cleanup and UPLC-MS-MS.

    Science.gov (United States)

    Lin, Qin-Bao; Xue, Yuan-Yuan; Song, Huan

    2010-01-01

    A new method using gel permeation chromatography (GPC) cleanup followed by ultra-performance liquid chromatography combined with tandem mass spectrometry (UPLC-MS-MS) has been established for simultaneous determination of 18 carbamate pesticides in nuts (chestnut and pine nut). Recoveries obtained by fortifying nut (spiking at 0.02 mg/kg) range from 70.21% to 89.56%. The proposed method features good sensitivity. Its limits of quantification are low enough to allow pesticide residues to be determined at concentrations below the maximum residue levels legally accepted. The precision, expressed as relative standard deviation, ranges from 2.26% to 4.07%.

  14. Residual deposits (residual soil)

    International Nuclear Information System (INIS)

    Khasanov, A.Kh.

    1988-01-01

    Residual soil deposits is accumulation of new formate ore minerals on the earth surface, arise as a result of chemical decomposition of rocks. As is well known, at the hyper genes zone under the influence of different factors (water, carbonic acid, organic acids, oxygen, microorganism activity) passes chemical weathering of rocks. Residual soil deposits forming depends from complex of geologic and climatic factors and also from composition and physical and chemical properties of initial rocks

  15. Effect of lignin linkages with other plant cell wall components on in vitro and in vivo neutral detergent fiber digestibility and rate of digestion of grass forages.

    Science.gov (United States)

    Raffrenato, E; Fievisohn, R; Cotanch, K W; Grant, R J; Chase, L E; Van Amburgh, M E

    2017-10-01

    The objective of this study was to correlate in vitro and in vivo neutral detergent fiber (NDF) digestibility (NDFD) with the chemical composition of forages and specific chemical linkages, primarily ester- and ether-linked para-coumaric (pCA) and ferulic acids (FA) in forages fed to dairy cattle. The content of acid detergent lignin (ADL) and its relationship with NDF does not fully explain the observed variability in NDFD. The ferulic and p-coumaric acid linkages between ADL and cell wall polysaccharides, rather than the amount of ADL, might be a better predictor of NDFD. Twenty-three forages, including conventional and brown midrib corn silages and grasses at various stages of maturity were incubated in vitro for measurement of 24-h and 96-h NDFD. Undigested and digested residues were analyzed for NDF, acid detergent fiber (ADF), ADL, and Klason lignin (KL); ester- and ether-linked pCA and FA were determined in these fractions. To determine whether in vitro observations of ester- and ether-linked pCA and FA and digestibility were similar to in vivo observations, 3 corn silages selected for digestibility were fed to 6 ruminally fistulated cows for 3 wk in 3 iso-NDF diets. Intact samples and NDF and ADF residues of diet, rumen, and feces were analyzed for ester- and ether-linked pCA and FA. From the in vitro study, the phenolic acid content (total pCA and FA) was highest for corn silages, and overall the content of ester- and ether-linked pCA and FA in both NDF and ADF residues were correlated with NDF digestibility parameters, reflecting the competitive effect of these linkages on digestibility. Also, Klason lignin and ADL were negatively correlated with ether-linked ferulic acid on an NDF basis. Overall, esterified FA and esterified pCA were negatively correlated with all of the measured fiber fractions on both a dry matter and an NDF basis. The lignin content of the plant residues and chemical linkages explained most of the variation in both rate and extent of

  16. Decomposition behavior of hemicellulose and lignin in the step-change flow rate liquid hot water.

    Science.gov (United States)

    Zhuang, Xinshu; Yu, Qiang; Wang, Wen; Qi, Wei; Wang, Qiong; Tan, Xuesong; Yuan, Zhenhong

    2012-09-01

    Hemicellulose and lignin are the main factors limiting accessibility of hydrolytic enzymes besides the crystallinity of cellulose. The decomposition behavior of hemicellulose and lignin in the step-change flow rate hot water system was investigated. Xylan removal increased from 64.53% for batch system (solid concentration 4.25% w/v, 18 min, 184°C) to 83.78% at high flow rates of 30 ml/min for 8 min, and then 10 ml/min for 10 min. Most of them (80-90%) were recovered as oligosaccharide. It was hypothesized that the flowing water could enhance the mass transfer to improve the sugars recovery. In addition, the solubilization mechanism of lignin in the liquid hot water was proposed according to the results of Fourier transform-infrared spectroscopy and scanning electron microscopy of the water-insoluble fraction and gas chromatography-mass spectrometry of the water-soluble fraction. It was proposed that lignin in the liquid hot water first migrated out of the cell wall in the form of molten bodies, and then flushed out of the reactor. A small quantity of them was further degraded into monomeric products such as vanillin, syringe aldehyde, coniferyl aldehyde, ferulic acid, and p-hydroxy-cinnamic acid. All of these observations would provide important information for the downstream processing, such as purification and concentration of sugars and the enzymatic digestion of residual solid.

  17. Cellulose and lignin colocalization at the plant cell wall surface limits microbial hydrolysis of Populus biomass

    Energy Technology Data Exchange (ETDEWEB)

    Dumitrache, Alexandru [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Tolbert, Allison [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Georgia Inst. of Technology, Atlanta, GA (United States); Natzke, Jace [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Brown, Steven D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Davison, Brian H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ragauskas, Arthur J. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)

    2017-04-20

    Biorefining of plant feedstocks into fuels and specialty chemicals, using biological conversion, requires the solubilization of lignocellulosics into simpler oligomeric compounds. However, non-pretreated woody biomass has shown high resistance to hydrolysis by cellulolytic microbes or purified cellulases. We investigate the limited solubilization of Populus deltoides by the cellulolytic thermophile Clostridium thermocellum in the absence of solute inhibitors. Compared to control samples, fermented poplar revealed that the hydrolysis of carbohydrates in secondary cell walls ceased prematurely as lignin presence increased at the surface. In quantitative fluorescence colocalization analysis by confocal laser scanning microscopy, the Manders’ coefficient of fractional overlap between lignin and cellulose signals increased from an average of 0.67 to a near-maximum 0.92 in fermented tissue. Chemical imaging by time-of-flight secondary ion mass spectrometry revealed a 49% decline in surface cellulose and a compensatory 30% and 11% increase in surface S- and G- lignin, respectively. Although 72% of the initial glucan was still present in the lignocellulose matrix of this feedstock, subsequent treatments with cell-free purified cellulases did not significantly restore hydrolysis. This confirmed that biomass surfaces had become non-productive for the C. thermocellum hydrolytic exoproteome. This study provides direct evidence for an explicit definition of feedstock recalcitrance, whereby depletion of surface carbohydrate increases lignin exposure which leads to inhibition of enzyme activity, while the bulk residual biomass retains significant undigested carbohydrate content. The analysis presented here establishes a novel method for the quantitation of lignocellulose recalcitrance.

  18. Low-Energy Catalytic Electrolysis for Simultaneous Hydrogen Evolution and Lignin Depolymerization.

    Science.gov (United States)

    Du, Xu; Liu, Wei; Zhang, Zhe; Mulyadi, Arie; Brittain, Alex; Gong, Jian; Deng, Yulin

    2017-03-09

    Here, a new proton-exchange-membrane electrolysis is presented, in which lignin was used as the hydrogen source at the anode for hydrogen production. Either polyoxometalate (POM) or FeCl 3 was used as the catalyst and charge-transfer agent at the anode. Over 90 % Faraday efficiency was achieved. In a thermal-insulation reactor, the heat energy could be maintained at a very low level for continuous operation. Compared to the best alkaline-water electrolysis reported in literature, the electrical-energy consumption could be 40 % lower with lignin electrolysis. At the anode, the Kraft lignin (KL) was oxidized to aromatic chemicals by POM or FeCl 3 , and reduced POM or Fe ions were regenerated during the electrolysis. Structure analysis of the residual KL indicated a reduction of the amount of hydroxyl groups and the cleavage of ether bonds. The results suggest that POM- or FeCl 3 -mediated electrolysis can significantly reduce the electrolysis energy consumption in hydrogen production and, simultaneously, depolymerize lignin to low-molecular-weight value-added aromatic chemicals. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Lignin- and Hemicellulose-derived Biomass Recalcitrance

    DEFF Research Database (Denmark)

    Deralia, Parveen Kumar

    and their associations at the molecular level are primary obstacles when cellulose is saccharified enzymatically to monomeric sugars, limiting the extent of saccharification. In this thesis, the main objective is to understand how the structure and composition of lignin and hemicellulose interact with pretreatment...... composition techniques are applied to reveal the structural and compositional modifications in lignin and hemicellulose. The scission of β-aryl ethers and concomitant generation of repolymerized structures (β-5 and β-β) and removal of different subsets of hemicellulose (in terms of different groups, e...

  20. Liquid chromatography – tandem mass spectrometry method for the determination of ten tetracycline residues in muscle samples

    Directory of Open Access Journals (Sweden)

    Gajda Anna

    2015-09-01

    Full Text Available A liquid chromatography – tandem mass spectrometry (LC-MS/MS method for the determination of oxytetracycline (OTC, 4-epi oxytetracycline (4-epi OTC, tetracycline (TC, 4-epi tetracycline (4-epi TC, chlortetracycline (CTC, 4-epi chlortetracycline (4-epi CTC, doxycycline (DC, minocycline (MINO, methacycline (META and rolitetracycline (ROLI residues in muscles was developed. The procedure consisted of an oxalic acid extraction followed by protein removal with trichloroacetic acid. Further solid phase clean-up on polymeric (Strata X reversed phase columns was performed to obtain an extract suitable for LC-MS/MS analysis. The tetracyclines were separated on a C 18 analytical column with mobile phase consisting of 0.01% formic acid in acetonitrile and 0.01% formic acid in water in gradient mode. The method was validated according to the Commission Decision 2002/657/EC. The recoveries of all target compounds were 91.8% – 103.6%. The decision limits were from 109.0 to 119.8 μg/kg and detection capability varied within the range of 122.2 to 137.6 μg/kg, depending on the analyte.